JP2020524225A - Method, process, and apparatus for making dyed and deposited substrates - Google Patents

Abstract

The fusing process may be configured to convert a substrate having short staple fibers into a fusing substrate having a significantly increased strength as compared to a raw substrate. When applied to one-dimensional substrates such as yarns, the welding process can also reduce the diameter of the welded substrate as compared to the raw substrate. In addition, the fusing process may be configured to impart superior color properties to the fusing substrate as compared to the color properties of the raw substrate, and the raw substrate having colored and/or dyed recycled fibers. Excellent color properties are very noticeable when the welding process is performed on the material. [Selection diagram] Fig. 22

Description

Cross-reference of related applications

Applicant claims priority to US Patent Application No. 62/520,056, filed June 15, 2017, the disclosure of which is incorporated herein by reference in its entirety. ..

The present disclosure relates to a method for producing a fiber composite material, a product that can be produced from the fiber composite material, and a method for producing a colored welded substrate.

Synthetic polymers such as polystyrene are typically deposited using a solvent such as dichloromethane. Ionic liquids (eg 1-ethyl-3-methylimidazolium acetate) can dissolve natural fiber biopolymers (eg cellulose and silk) without derivatization. Natural fiber welding is a process in which biopolymer fibers are fused in a manner generally similar to conventional plastic welding.

Partial dissolution of natural fibers for structural and chemical modification, as disclosed in US Pat. No. 8,202,379, which is incorporated herein by reference in its entirety. One of the process solvents that can be used for is an ionic liquid-based (IL-based) solvent. This patent discloses the basic principles developed using tabletop equipment and materials. However, this patent does not specifically disclose the process and equipment for producing the composite material on a commercial scale.

There are examples of natural fiber biopolymer solutions that are poured into a mold to create the desired two-dimensional shape. In this case, the biopolymer is completely dissolved, resulting in the destruction of the original structure and modification of the biopolymer. In contrast, fiber welding deliberately leaves the interior of the fiber (the core of each individual fiber) unmodified. It is tough from biopolymers such as silk, cellulose, chitin, chitosan, other polysaccharides and combinations thereof, because the final structure composed of biopolymer retains some of the properties of the original material. Advantageous in producing the material.

The conventional method of using a biopolymer solution is also disadvantageous in that there is a physical limit to the amount of polymer that can be dissolved in the solution. For example, a solution of 10% by weight cotton (cellulose) and 90% by weight of an ionic liquid solvent is viscous and difficult to handle even at high temperatures.

US Patent No. 8,202,379

Provided is a fiber welding process that allows the fiber bundle to be manipulated into the desired shape prior to performing the welding.

The fiber welding process can manipulate the fiber bundle into the desired shape prior to performing the welding. The use and handling of natural fibers often allows for control over the engineering of the final product, which is not possible with solution-based technology.

The accompanying drawings, which are incorporated in and constitute a part of this specification, serve to illustrate embodiments and, together with the description, serve to explain the principles of methods and systems.

FIG. 3 is a schematic view of various aspects of a process for producing a welded substrate (fused substrate). 3 is a schematic view of various aspects of another process for making a welded substrate. FIG. FIG. 3 is a schematic view of one of the process solvent recovery zones that can be used with the welding process. A process for the addition and physical entrapment of a solid material within a fiber-matrix composite is shown with the sub-process or components of FIG. 3 labeled FIGS. 3A-3E. The functional material is predispersed in the fiber matrix before welding. The process for the addition and physical entrapment of the solid material within the fiber-matrix composite was performed using the material (pre)dispersed in the IL-based solvent, sub-section of FIG. 4, labeled as FIGS. 4A-4D. Shown with processes or components. The process for the addition and physical entrapment of a solid material within a fiber-matrix composite is illustrated in Figures 5A-5D using a material (pre-)dispersed in an IL-based solvent with additional solubilized polymer. 5 with the sub-process or components of FIG. FIG. 6 is a side cross-sectional view of one configuration of the process solvent application zone. FIG. 6 is a perspective view of another configuration of the process solvent application zone. FIG. 6 is a perspective view of another configuration of the process solvent application zone. FIG. 6 is a side view of an apparatus that can be used with various welding processes. FIG. 6D is a side view of the device of FIG. 6D with the plates in different positions relative to each other. FIG. 6 is a side view of an apparatus that can be used with various welding processes, the apparatus being configurable for use with multiple 1D substrates positioned adjacent to each other. FIG. 8 is a schematic view of a welding process that can be used to manufacture the welding substrate shown in FIG. 7C. FIG. 3 is a scanning electron microscope image of a raw 1D substrate with 30/1 ring-spun cotton yarn. 7B is a scanning electron microscope image of the base material shown in FIG. 7B after being processed by another welding process using a process solvent containing an ionic liquid to produce a welded base material. FIG. 7 is a graph showing the relationship between stress (g) and elongation for both the representative raw yarn base material sample and the representative welded yarn base material sample of FIG. 7C, where the upper curve is the welded yarn base material. Material, the lower curve is the yarn. FIG. 9 is a schematic view of a welding process that can be used to manufacture the welding base material shown in FIG. 8C. 3 is a scanning electron microscope image of a raw 1D substrate with 30/1 ring spun cotton yarn. 8B is a scanning electron microscope image of the substrate after the raw substrate shown in FIG. 8B is processed by another welding process using a process solvent containing an ionic liquid to produce the substrate. FIG. 8 is a graph showing the relationship between stress (g) and elongation for both the representative raw yarn base material sample and the representative welded yarn base material sample of FIG. 8C, with the upper curve being the welded yarn base material and the lower side. The curve is the raw yarn. FIG. 9C is a perspective view of a welding process that can be configured to produce the welding substrate shown in FIGS. 9C-9E. 3 is a scanning electron microscope image of a raw 1D substrate with 30/1 ring spun cotton yarn. 9B is a scanning electron microscope image of the unprocessed substrate shown in FIG. 9B after being processed by a welding process using a process solvent containing an ionic liquid, in which the substrate is lightly welded. 9B is a scanning electron microscope image of the unprocessed substrate shown in FIG. 9B after being processed by a welding process using a process solvent containing an ionic liquid, the substrate being welded to a moderate extent. 9B is a scanning electron microscope image of the substrate shown in FIG. 9B after being processed by a welding process using a process solvent containing an ionic liquid, the substrate being firmly welded. 9D is an image of a fabric made from the welded substrate shown in FIG. 9D. FIG. 9 is a graph showing the relationship between stress (g) and elongation for both the representative raw yarn base material sample and the representative welded yarn base material samples of FIGS. 9C and 9K, where the upper curve is the welded yarn base material. The lower curve is the raw yarn. The left side is an image of a fabric made from the green substrate shown in Figure 9B, and the right side is an image of a fabric made from the welded substrate shown in Figure 9D. It is an image of the welding base material which can be regarded as a shell welding base material. It is an image of the welding base material which can be regarded as a shell welding base material. 9B is a scanning electron microscope image of the raw substrate shown in FIG. 9B after being processed by a welding process using a process solvent containing an ionic liquid, in which the welded substrate is lightly welded. FIG. 9B is a scanning electron microscope image of the raw substrate shown in FIG. 9B after being processed by a welding process using a process solvent containing an ionic liquid, the substrate being welded to a moderate extent. 9B is a scanning electron microscope image of the raw substrate shown in FIG. 9B after being processed by a welding process using a process solvent containing an ionic liquid, and the substrate is firmly welded. FIG. 11 is a perspective view of a welding process that can be configured to produce the welding substrate shown in FIGS. 10C-10F. 3 is a scanning electron microscope image of a raw 1D substrate with 30/1 ring spun cotton yarn. FIG. 10B is a scanning electron microscope image of the raw substrate shown in FIG. 10B after being processed by a welding process using a process solvent containing a hydroxide, in which the substrate is lightly welded. FIG. 10B is a scanning electron microscope image of the unprocessed substrate shown in FIG. 10B after it has been processed by a welding process using a process solvent containing hydroxide, the welded substrate being moderately welded. .. FIG. 10B is a scanning electron microscope image of the raw substrate shown in FIG. 10B after being processed by a welding process using a process solvent containing hydroxide, showing that the substrate has been firmly welded. FIG. 10E is an enlarged image of a part of the welding base material in the center of FIG. 10E. FIG. 11 is a graph showing the relationship between stress (g) and elongation for both the representative raw yarn base material sample and the representative welded yarn base material sample of FIG. 10C, where the upper curve is the welded yarn base material, and the lower side is The curve is the raw yarn. FIG. 6 is a schematic diagram illustrating various aspects of a modulated fiber welding process. FIG. 6 is a schematic view showing another aspect of the modulation fiber welding process. FIG. 6 is a schematic view showing another aspect of the modulation fiber welding process. FIG. 6 is a schematic view showing another aspect of the modulation fiber welding process. Figure 5 is an image of a welded substrate produced by a modulation welding process, where the right part of the figure is lightly welded and the right part of the figure is firmly welded. In another image of a fabric made from a modulation welded substrate, the fabric shows a heather effect. 3 is a scanning electron microscope image of a raw 2D substrate containing denim. FIG. 12B is a scanning electron microscope image of the substrate shown in FIG. 12A after being processed into a firmly welded substrate. 3 is a scanning electron microscope image of a raw 2D substrate with knitted fabric. 12C is a scanning electron microscope image of the substrate after processing the green substrate shown in FIG. 12C into a medium welded substrate. 3 is a scanning electron microscope image of a raw 2D substrate with a jersey knit cotton fabric. 12E is a scanning electron microscope image of the substrate after processing the raw substrate shown in FIG. 12E into a lightly welded substrate. 3 is an enlarged scanning electron microscope image of a raw 2D substrate with a jersey knit cotton fabric. 12E is a scanning electron microscope image of the substrate after processing the raw substrate shown in FIG. 12E into a lightly welded substrate. 3 is a scanning electron microscope image of a welded yarn substrate produced using a welding process with a reconstituted solvent at about 20° C. 3 is a scanning electron microscope image of a welded yarn substrate produced using a welding process with a reconstituted solvent at about 22° C. 3 is a scanning electron microscope image of another welded yarn substrate produced using the welding process with a reconstituted solvent at about 40° C. 2 is an X-ray diffraction data of a cotton yarn (Plot A) and a cotton yarn reconstituted from a raw cotton yarn base material completely dissolved in an ionic liquid. 15B is an X-ray diffraction data of three different types of welded yarn base materials manufactured from the same raw cotton yarn base material as in the plot A of FIG. 15A. FIG. 4 is a cross-sectional view of a raw cotton yarn substrate showing various individual cotton fibers. FIG. 3 is a cross-sectional view of a raw cotton yarn base material ring-dyed using a conventional technique. FIG. 3 is a diagram of a welded yarn substrate that can be manufactured by one dyeing and welding process. It is sectional drawing of the single welding fiber of the welding thread base material shown to FIG. 17A. FIG. 4 is a cross-sectional view of a welded yarn base material that can be manufactured by another dyeing and welding process. It is sectional drawing of the single welding fiber of the welding thread base material shown to FIG. 18A. FIG. 3 is a cross-sectional view of a welded yarn base material that can be manufactured by a welding process. FIG. 6 is a cross-sectional view of a welded yarn base material that can be manufactured by another welding process. FIG. 6 is a cross-sectional view of a welded yarn base material that can be manufactured by another welding process. FIG. 1 is a diagram of a roll of raw yarn made from denim. FIG. 20B is a diagram of a welded yarn made from the yarn shown in FIG. 20A by a welding process configured to use a process solvent containing hydroxide. FIG. 20B is a diagram of a weld yarn made from the yarn shown in FIG. 20A by a weld process configured to use a process solvent containing an ionic liquid. 3 is a scanning electron microscope image of a composite raw 1D substrate with anti-wool yarns. 20B is a scanning electron microscope image of the welded yarn shown in FIG. 20B. 20C is a scanning electron microscope image of the welded yarn shown in FIG. 20C. Raw wool substrate samples (FIGS. 20A and 21A), fused yarn made from raw wool substrate using hydroxide-containing process solvent (FIGS. 20B and 21B) and process solvent with ionic liquid 20C is a graph showing the relationship between the tensile strength (cN/dtex) and the elongation of the welded yarn (FIGS. 20C and 21C) produced from the raw wool yarn base material. It is a visible image of a plurality of raw yarns produced from a part of the fluff fibers after the clocking test. It is a visible drawing image of a plurality of welding threads produced from a part of fluff fiber after a clocking test. 3 is a graph showing the proportion of short staple fibers in the yarn as a function of yarn weight. 3 is a graph showing the increase in strength and the increase in strength per cross-sectional area that occur when processing three different yarns in the welding process according to the present invention. 3 is a graph showing the increase in strength and the increase in strength per cross-sectional area that occurs when processing three different yarns in another welding process according to the present invention. 3 is a graph showing the increase in strength and the increase in strength per cross-sectional area that occur when processing three different yarns in yet another welding process according to the present invention. It is a photograph showing a dyed fabric containing a raw yarn. It is a photograph showing a dyed woven fabric including a fused yarn. FIG. 26B is a photograph showing the dyed fabric of FIG. 26A after performing a pilling test. FIG. 26B is a photograph showing the dyed fabric of FIG. 26A after performing a pilling test. It is a scanning electron microscope image of an original short staple fiber yarn. 28B is a scanning electron microscope image of a welded yarn produced by using the raw short staple fiber yarn shown in FIG. 28A.

Before disclosing the method and apparatus of the present invention, it should be understood that the method and apparatus are not limited to a particular method, a particular component, or a particular implementation. It should also be understood that the terminology used herein is for the purpose of describing particular embodiments/aspects only and is not intended to be limiting.

As used in this specification and the appended claims, the singular forms "a" ("a", "an" and "the") refer to plural references unless the context clearly dictates otherwise. Includes. Ranges may be expressed herein as from "approximately" one particular value, and/or to "approximately" another particular value. When such a range is expressed, another embodiment includes from the one particular value and/or to the other particular value. Similarly, where a value is expressed as an approximate number, it will be understood that the use of "about" in front of that particular value forms another embodiment. It will be further understood that the endpoints of each of the ranges are significant both in relation to the other endpoint, and independently of the other endpoint.

“Optional” or “optionally” means that the events or circumstances described thereafter may or may not occur, and that such statements may or may not occur. Means inclusion.

"Aspect" does not mean that the limitation, function, component, etc. referred to as an aspect is required when referring to a method, apparatus, and/or these components, but rather as a specific example. It is not intended to limit the scope of methods, devices, and/or components thereof, unless specifically set forth in the following claims as such.

Throughout the description and claims of this specification, the word “comprise” and variations thereof are meant to include “including but not limited to” and “comprises.” Is not meant to be exclusive, and is not intended to exclude other components, integers, or steps, for example. “Exemplary” means “an example of” and is not intended to convey the instructions of the preferred or ideal embodiments. “Such as” is used for descriptive purposes rather than in a limiting sense.

Disclosed are components that can be used to implement the disclosed methods and apparatus. These and other components are disclosed herein, and when combinations, subsets, interactions, groups, etc. of these components are disclosed, each of the various separate and collective combinations and Although no specific reference to the permutation of the above may be explicitly disclosed, it is understood that all methods and apparatus are each explicitly conceived and described herein. This applies to all aspects herein, including but not limited to steps of the disclosed method. Thus, where there are various additional steps that can be performed, it is understood that each of these additional steps can be performed in any particular embodiment or combination of embodiments of the disclosed method.

The method and apparatus of the present invention may be more readily understood by reference to the following detailed description of the preferred embodiments and the examples contained therein, as well as the figures and the description before and after it. When referring to general constructions and/or corresponding components, aspects, features, functions, methods, and/or structural materials, terms equivalent to these terms can be used interchangeably.

It is to be understood that this disclosure is not limited in its application to the detailed structure and construction of the components described in the following description or illustrated in the drawings. The disclosure is capable of other embodiments and of being practiced or being carried out in various ways. The nomenclature and terms used herein with reference to the orientation of the device or element (eg, "anterior," "rearward," "top," "bottom," "top," "bottom," etc.) are simplified in description. It is also to be understood that it is only used to do so and does not, by itself, indicate or imply that the referenced device or element must be in a particular orientation. Furthermore, terms such as "first," "second," and "third" are used herein for purposes of illustration and in the appended claims, to indicate their relative importance or significance. Nor is it intended to be implied.

1. Definition

Throughout this disclosure, various terms may be used to describe particular components of a process, apparatus, and/or other components that may be used with this disclosure. For clarity, some definitions of these terms appear below. However, when used to describe such components, these terms and their definitions are not meant to limit the scope unless so indicated in the following claims, and to the present disclosure. Is meant to exemplify one or more aspects of Furthermore, the inclusion of any term and/or definition thereof requires explicit mention of components in any particular process or apparatus disclosed herein, unless so indicated in the following claims. It does not mean.

A. Base material

“Substrate” as used herein means one pure biomaterial (eg, cotton thread, etc.), multiple biomaterials (eg, lignocellulosic fibers mixed with silk fibers), or a known amount of biomaterial. It may include any of the materials containing materials. In one aspect, the substrate may contain a natural material containing at least one biopolymer component (eg, cellulose) bound by hydrogen bonds. In some embodiments, the term "substrate" may refer to synthetic materials such as polyester, nylon, etc., however, when the term "substrate" refers to synthetic materials, it is typically explicitly noted throughout. Will. The fusing or welding process may be performed in a manner that limits the modification of at least one component of the substrate. For example, a limited amount of process solvent may be added at moderate temperatures and pressures for a controlled period of time to limit modification of the lignocellulosic fibers.

"Cellulose-based substrates" include cotton, pulp, and/or other purified cellulosic fibers and/or particles and the like.

Examples of the "lignocellulose-based base material" include wood, hemp, corn stover, soybean straw, grass and the like.

Examples of the "other sugar-based biopolymer base material" include chitin, chitosan and the like.

Examples of the “protein-based substrate” include keratin (eg, wool, hoof, horn, nail), silk, collagen, elastin, tissue and the like.

"Raw substrate", as used herein, includes any substrate that has not been subjected to any welding process.

B. Substrate format types

The substrate format can be various commercial or customized products. "Loose" one-dimensional (1D), two-dimensional (2D), and/or three-dimensional (3D) substrates can all be used in various processes according to the present disclosure. The finished welded substrate or composite may be molded in 1D, 2D, and/or 3D, respectively. The following definitions apply to both substrates and weld substrates (as defined further below).

"Loose" means any natural fiber and/or particle or mixture of natural fibers and/or particles supplied to the welding process in a loose (loose) and/or relatively entangled format (eg, A mixture of loose cotton and wood fibers and/or particles).

"1D" includes both untwisted single and twisted yarns and threads.

Examples of “2D” include a paper base material (eg, cardboard substitute, wrapping paper, etc.) and a board base (eg, hard board substitute, plywood, OSB, MDF, standard material, etc.).

“3D” includes automobile parts, structural building components (eg, extruded beams, joists, walls, etc.), furniture parts, toys, electronic device cases and/or components.

In general, the resulting welded substrate or composite material may contain significant amounts of natural materials (eg, materials produced from living organisms and/or enzymes), which natural materials include glues, resins, And/or may be joined by fusing or welding biopolymers of natural materials rather than other adhesives.

C. Process solvent system

A “process solvent” includes a material capable of breaking intermolecular forces (eg, hydrogen bonds) on a substrate and swelling, mobilizing, and/or swelling at least one biopolymer component in the substrate. Or materials that can be dissolved and/or otherwise disrupt the force that may bind the biopolymer components together.

“Pure process solvent” includes process solvents without additional additives, including ionic liquids, 3-ethyl-1-methylimidizolium acetate, 3-butyl-1-methylimidizolium chloride, And other currently known or later developed similar salts that serve to disrupt the intermolecular forces of the substrate.

"Deep eutectic process solvent" includes an ionic solvent that incorporates one or more compounds into a mixture form to give a eutectic having a melting point lower than one or more of the constituent components of the mixture. And further include pure ionic liquid process solvents mixed with other ionic liquids and/or molecular species.

"Mixed organic process solvent" refers to an ionic liquid (eg, 3-ethyl-1-methylimidizolium) mixed with a polar protic solvent (eg, methanol) and/or a polar aprotic solvent (eg, acetonitrile). Acetate), and 4-methylmorpholine 4-oxide, also known as N-methylmorpholine N-oxide (NMMO).

The “mixed inorganic process solvent” is an aqueous salt solution (for example, an aqueous solution of LiOH and/or NAOH, mixed with urea or other molecular additive, aqueous guanidine chloride, a solution of LiCl in N,N-dimethylacetamide (DMAc)) It may be).

In one aspect, the process solvent may contain a relatively small amount (eg, less than 10% by weight) of additional functional material such as a fully solubilized natural polymer (eg, cellulose), but is selected. Synthetic polymers (eg meta-aramid) as well as other functional materials may be included.

D. Functional material

“Functional materials” include natural or synthetic inorganic materials (eg, magnetic or conductive materials, magnetic fine particles, catalysts, etc.), natural or synthetic organic materials (eg, carbon, dyes (including fluorescent and phosphorescent, but (Without limitation), enzymes, catalysts, polymers, etc.) and/or devices (eg, RFID tags, MEMS devices, integrated circuits) that can add features, functions, and/or benefits to the substrate. Further, the functional material may be placed in the substrate and/or process solvent.

E. Process wet base material

"Process wet substrate" can refer to substrates of any combination of formats and types that have been wet with process solvent applied to all or part of the substrate. Thus, the process wet substrate may contain some partially dissolved and mobilized natural polymer.

F. Reconstituted solvent system

"Reconstituted solvents" include liquids that have a non-zero vapor pressure (non-zero vapor pressure) and are capable of forming a mixture with ions from the process solvent system. In one aspect, one feature of the reconstituted solvent system is that it cannot dissolve the natural substrate as it is. Generally, the reconstitution solvent can be used to separate and remove process solvent ions from the substrate. That is, in one aspect, the reconstitution solvent removes the process solvent from the process wet substrate. In doing so, the process wet substrate can be converted to a reconstituted wet substrate as described below.

Examples of the reconstitution solvent include a polar protic solvent (eg water, alcohol etc.) and/or a polar aprotic solvent (eg acetone, acetonitrile, ethyl acetate etc.). The reconstitution solvent may be a mixture of molecular components or may include ionic components. In one aspect, the reconstitution solvent can be useful in controlling the distribution of the functional material within the substrate. The reconstitution solvent may be configured to be chemically similar or substantially chemically identical to the molecular additive in the process solvent system.

In one aspect, the (pure) reconstitution solvent may be mixed with the ionic component to form the process solvent. The reconstitution solvent may be configured to be chemically similar or substantially chemically identical to the molecular additive in the process solvent system. For example, acetonitrile is a polar aprotic molecular liquid with a non-zero vapor pressure that is incapable of dissolving cellulose when pure. Acetonitrile may be mixed with a sufficient amount of 3-ethyl-1-methylimidizolium acetate to form a solution capable of breaking hydrogen bonds, and acetonitrile may be used as the reconstitution solvent. Therefore, a mixture containing appropriate ions in sufficient concentration (ionic strength) can function as a process solvent. Within this disclosure, any mixture of 3-ethyl-1-methylimidizolium acetate in acetonitrile that does not contain sufficient ionic strength to dissolve or mobilize the natural matrix polymer is considered a reconstitution solvent. Be done.

G. Reconstituted wet base material

"Reconstituted wet substrate" can refer to any combination of format and type of process wet substrate that has been wetted with a reconstituted solvent applied to all or a portion of the process wet substrate. Generally, the reconstituted wet substrate does not contain the partially dissolved, mobilized natural polymer, which is believed to be due to the application of the reconstitution solvent to remove the process solvent.

H. Dry gas system

A "dry gas" may include materials that are gases at room temperature and atmospheric pressure, but may also be supercritical fluids. In one aspect, the dry gas can be mixed with and carry a non-zero vapor pressure component (eg, all or part of the reconstituted solvent) originating from both the process wet substrate and/or the reconstituted wet substrate. .. The dry gas may be a pure gas (eg nitrogen, argon etc.) or a mixture of gases (eg air).

I. Welding base material

"Welded substrate" (fused substrate) means that one or more individual fibers and/or particles act on a process polymer that acts on a biopolymer derived from any of the fibers and/or particles, and/or Alternatively, it may be used to refer to a finished composite that includes at least one natural substrate that has been fused or welded by action on another natural material within the substrate. In general, the weld substrate may include "finished composite" and/or "fiber-matrix composite". Specifically, "fiber-matrix composite" can be used to refer to a welded substrate having a natural substrate that acts as both the fiber and matrix of the welded substrate.

J. Welding

"Welding" as used herein may be used to refer to the binding and/or fusing of materials by the close intermolecular association of polymers.

2. General welding process

The present disclosure provides various processes and/or apparatus for converting a biopolymer containing a fibrous and/or particulate substrate into a welded substrate, an example of which is a composite material, and Also disclosed are various products that can be made from the welded substrate. Generally, the process steps and/or combination of process steps for converting a biopolymer containing a fibrous and/or particulate substrate into a welded substrate may be referred to herein as a "welding process", There is no limitation unless so indicated in the following claims. In one aspect of the process, the process solvent may be applied to one or more substrates containing natural materials. In one aspect, the process solvent disrupts one or more intermolecular forces within the at least one component of the substrate containing the natural material, the intermolecular forces can include, but are not limited to, hydrogen bonds. obtain.

Removal of a portion of the process solvent (which may be performed with a reconstitution solvent, which is described in further detail below) causes the fibers and/or particles in the substrate to fuse or weld together, leaving the welded substrate untouched. May be obtained. Testing revealed that the deposited substrate may have enhanced physical properties (eg, enhanced tensile strength) compared to the original substrate (prior to being processed). The welded substrate has enhanced chemistry due to the parameters selected for the welding process itself, or by including a functional material in the substrate before or during the welding process that transforms the substrate into the welded substrate. It may also have specific properties (eg, hydrophobicity) or other features/functions.

The various processes and/or apparatus disclosed herein are such that the processes and/or apparatus are capable of completely removing a biopolymer of a natural material, in any number of process solvents and/or substrates (academic or patent literature). In some cases, it is known that it can be dissolved or it has been generalized so that it can be configured to use process solvents and/or substrates that were developed later). In one aspect of the present disclosure, the fusing process may be configured such that the biopolymer-containing substrate is not completely dissolved in the treatment process. In another aspect, tough composites of various compositions and shapes can be made without the use of glues and/or resins (even processes configured to completely dissolve the biopolymer-containing substrate).

In general, the deposition process and/or equipment may be configured to carefully and intentionally control the amount of process solvent, temperature, pressure, time of exposing the natural material to the process solvent, and/or other parameters. There is no limitation, unless so indicated in the following claims. In addition, the means by which the process solvent, reconstituted solvent, and/or dry gas can be efficiently recycled for reuse can be optimized for commercialization. Accordingly, disclosed herein is a collection of novel concepts and features that are not obvious from the prior art. Given that natural materials are generally plentiful, inexpensive, and sustainable to manufacture, the processes and devices disclosed herein produce deformable and sustainable materials that produce trillions of dollars of value per year. It can be a prototype of various means. This technology allows mankind to move forward without being limited by limited resources such as petroleum and petroleum-containing materials. In one aspect, the present disclosure provides a novel and non-obvious process and/or apparatus configured to use this result with a substrate, process solvent, and/or reconstitution not disclosed in the prior art. Can be achieved using, which can result in various new and non-trivial end products.

A. Substrate supply zone

Referring now to the drawings, FIG. 1 illustrates various aspects of one welding process configured to produce a weld substrate, such that like reference numerals refer to like or corresponding parts throughout the several views. A schematic diagram is provided. This general deposition process may be modified and/or optimized based on at least the particular substrate, the particular process solvent system, the particular deposition substrate to be manufactured, the functional material utilized, and/or combinations thereof. It may be embodied. The welding process schematically illustrated in FIG. 1 is not meant to be limiting and is for illustrative purposes only, unless so indicated in the following claims. Further details of certain aspects of the welding process for producing the welded substrate (eg, specific equipment, process parameters, process solvent system, etc.) are provided further below, with examples of the welding process immediately below. It highlights one aspect of the disclosure that may be applied to a wide range of substrates, process solvent systems, reconstitution solvent systems, welded substrates, functional materials, substrate formats, welded substrate formats, and/or combinations thereof. It is intended to provide a comprehensive framework.

Generally, the welding process is configured such that the substrate feed zone 1 comprises a welding process portion at which the substrate format can be controllably fed (introduced) to the welding process and/or associated equipment. May be done. Substrate supply zone 1 may include an apparatus for making a particular substrate format from a particular substrate material or combination of substrate materials. Alternatively, the substrate supply may be configured to deliver a roll of pre-made substrate format. The substrate may be pushed or pulled through the substrate feed zone 1. The substrate may be mounted on a powered conveyor system. The substrate may be fed through the substrate feeding zone 1 by an extrusion type screw. Therefore, the scope of the present disclosure is whether and/or how the substrate moves in the substrate feed zone 1 and/or when the substrate is not otherwise indicated in the following claims. It is not limited by whether the equipment and/or other components of the welding process, when stationary, move relative to the substrate.

The substrate may contain a functional material that can be added to the substrate in the substrate supply zone 1. The equipment and instrumentation may be used to monitor and control at least the temperature, pressure, composition, and/or feed rate of the material in the substrate feed zone 1. Generally, the substrate or substrates may be moved from the substrate feed zone 1 to the process solvent application zone 2.

In one aspect of the welding process according to the present disclosure configured for use with certain 1D substrates (eg, textile yarns and/or similar substrates), the substrate is stressed before it enters the welding process. It may be advantageous to include a device that applies By applying a predetermined stress to the substrate prior to entering the fiber welding process, weak areas of the substrate may be damaged and exposed. The device may be configured to have a mechanism to tie a knot and reconstruct a continuous substrate. Finally, the welding process so configured can locate and repair weak areas of the substrate so as to limit downtime. The device may be a stand-alone machine that improves a particular substrate long before performing the welding process. Alternatively, the device can be incorporated directly into the substrate feed zone 1.

B. Process solvent application

In the process solvent application zone 2, as the substrate passes through the process solvent application zone 2, one or more process solvents are dipped, wicked, painted, inkjet printed, sprayed, etc., or by any combination thereof. , May be applied to the substrate. The process solvent may include functional materials and/or molecular additives, any of which are described in further detail below.

In one aspect, the process solvent application zone 2 may be configured with an additional device that adds the functional material to the substrate separately from the process solvent. The apparatus and instrumentation may be used to monitor and control at least the temperature and/or pressure of the process solvent, substrate, and/or atmosphere during process solvent application. Devices and instruments that monitor and control the composition, amount, and/or rate of applied process solvent may be used. The process solvent may be applied at a specific location or over the substrate, depending on the process solvent application method.

In aspects of the welding process for producing a weld substrate using extrusion, a die may be used at the end of process solvent application zone 2. The welding process so configured may also include apparatus for forming a 1D, 2D, or 3D shape from the loose substrate to which the process solvent has been applied as the substrate passes through the process solvent application zone 2. .. In general, the optimum configuration of the solvent application zone 2 may vary depending at least on the substrate format, the choice of process solvent and/or process solvent system, and the equipment used to apply the process solvent. These parameters may be configured to achieve the desired amount of viscous drag. "Viscosity resistance," as used herein, refers to the viscosity of a process solvent and/or process solvent system and the mechanical force (eg, pressure, friction, etc.) that applies the process solvent and/or process solvent system to a substrate. (Shear etc.). As will be discussed in more detail below, in some cases the optimum viscous drag is configured to result in a weld substrate with consistent consistent properties, while in other cases the optimum viscous drag is modulated. It is configured so as to obtain a welded base material.

In one aspect of the welding process according to the present disclosure configured for use with certain 1D substrates (eg, textile yarns and/or similar substrates), the process solvent is suitably applied to the substrate (whereby It may be advantageous to use an appropriately sized needle-like orifice that can be designed to exert a viscous drag) and produce the desired properties of the weld substrate. The process solvent may be controllably metered into the device while the substrate is moving within the orifice. At least the temperature, flow rate and flow characteristics of the process solvent, and/or substrate feed rate may be monitored and/or controlled to impart desired properties to the finished welded substrate. As described in more detail below with respect to FIGS. 6A-6C, the size, shape and configuration of the orifice (eg, diameter, length, gradient, etc.) will depend on the substrate when the process solvent is applied to the substrate. It may be designed to limit or add stress. This design consideration can be particularly important for knitted or woven yarns that have not undergone fines or short fiber removal by combing.

The specific configuration of process solvent application zone 2 may vary depending at least on the specific chemistry used for the process solvent and/or process solvent system. For example, some process solvents and/or process solvent systems are effective at swelling and mobilizing biopolymers at relatively low temperatures (ie, LiOH-urea below about -5°C), and others. (Ie, ionic liquids, NMMOs, etc.) are effective at relatively high temperatures. While NMMOs may require temperatures above 90°C, some ionic liquids are effective above 50°C. Further, many process solvents and/or process solvent systems may be correlated with temperature, so the optimal configuration of various aspects of process solvent application zone 2 (or other aspects of the deposition process) is It may depend on the temperature of the application zone 2, the process solvent itself, and/or the process solvent system. That is, an apparatus used to apply a process solvent and/or process solvent system to a substrate when the particular process solvent and/or process solvent system is effective at low temperatures and is also relatively viscous at such low temperatures. Must be designed to accommodate the above temperatures and viscosities. Within the effective temperature range of a given process solvent and/or process solvent system, temperatures within that range, chemistry of the process solvent and/or process solvent system (eg, cosolvent addition and/or ratios, etc.), process solvent Appropriate amount of process solvent is applied to the substrate so as to obtain a wet substrate with desirable properties for the rest of the deposition process by making further improvements such as the configuration of the equipment associated with application zone 2. Viscosity resistance of However, the specific operating temperatures within the process solvent application zone 2 do not limit the scope of the present disclosure in any way, unless so indicated in the following claims.

C. Process temperature/pressure zone

Upon application of the process solvent to the substrate, the wet substrate can enter the deposition process zone at least at a controlled temperature, pressure, and/or atmosphere (composition) for a controlled amount of time. The apparatus and instrumentation may be used to monitor, modulate, and/or control at least the temperature, pressure, composition, and/or feed rate of the process wet substrate within the substrate feed zone 1. Specifically, the temperature may be controlled and/or modulated by using a chiller, convection oven, microwave, infrared, or any number of other suitable methods or devices.

In one aspect, the process solvent application zone 2 is separate from the process temperature/pressure zone 2. However, in another aspect of the present disclosure, the welding process may be configured such that the two zones 2, 3 above are one adjacent segment. For example, a deposition process in which a substrate is immersed in and passed through a process solvent bath under controlled temperature and pressure for a specified time combines process solvent application zone 2 and process temperature/pressure zone 3. It will be. In general, the process solvent application zone 2 and the process temperature/pressure zone 3 together can be considered a welding zone.

In aspects of the welding process according to the present disclosure in which extrusion is performed, a die may be included in or at the end of the process temperature/pressure zone 3. Other aspects of the welding process according to the present disclosure may also include an apparatus for forming a 1D, 2D, or 3D shape from a loose substrate to which a process solvent has been applied and passed through a process temperature/pressure zone 3.

D. Process solvent recovery zone

The process solvent may be separated from the substrate within the process solvent recovery zone 4. In one aspect, the process solvent may contain salts with little or no vapor pressure. A reconstitution solvent may be introduced to remove the process solvent (at least some of which may include ions) from the substrate. When the reconstituted solvent is applied to the process wetting substrate, the process solvent may exit the substrate and migrate into the reconstituted solvent. Although not required, in some embodiments, the reconstituted solvent may flow in a direction opposite to the movement of the substrate, so that the reconstituted solvent required to recover the process solvent is very small and very small. Use time, space, and energy (if applicable).

In one aspect of the deposition process constructed in accordance with the present disclosure, the process solvent recovery zone 4 may be a bath, a series of baths, or a series of segments in which the reconstituted solvent flows in a direction opposite or across the process wet substrate. Good. Equipment and instrumentation may be used to monitor and control at least the temperature, pressure, composition, and/or flow rate of the reconstituted solvent in the process solvent recovery zone 4. Upon exiting this zone 4, the substrate may be wetted with the reconstitution solvent.

In one aspect, a process solvent system having an ionic liquid process solvent is configured in combination with a molecular additive, and the reconstitution solvent is configured to be chemically similar or chemically identical to the molecular additive. It may be optimal. For process solvents that include ionic liquids, it may be useful to select a molecular additive that has a relatively low boiling point but a relatively high vapor pressure. Furthermore, it may be useful for such molecular additives to be generally polar aprotic (polar protic solvents are generally more difficult to separate from ionic liquids and Examples thereof include, but are not limited to, acetonitrile, acetone, ethyl acetate, and the like, because they also tend to reduce the efficacy of the solvent-containing system). For process solvents that include an aqueous hydroxide (eg, LiOH) solution, it may be advantageous to choose a reconstitution solvent that includes water that is polar protic. Constructing the deposition process using a molecular additive that is chemically similar or chemically identical to the reconstituted solvent is necessary for at least the process solvent recovery zone 4, solvent collection zone 7, and solvent recycle 8 equipment and It may be beneficial to the economics of the welding process because it may simplify energy and/or time. Further, increasing the temperature of the reconstitution solvent and/or process solvent recovery zone 4 can significantly reduce the time required for reconstitution, which results in a reduction in the overall length of the welding process and associated equipment. Potential, which in turn leads to reduced substrate tension complexity and/or variability and volume consolidation control capabilities (discussed in more detail below).

Alternatively, the deposition process may consist of a composition of reconstituted solvent and a temperature that produces a deposited substrate having certain characteristics. For example, as described in more detail below, in one deposition process using a process solvent that includes a reconstitution solvent that includes EMIm OAc and water, the temperature of the water can affect the properties of the welded yarn substrate.

E. Drying zone

The reconstituted solvent may be separated from the substrate in the drying zone 5. That is, the reconstituted wet substrate may be converted to the completed (dry) welded substrate in the drying zone 5. Although not required, in one aspect, the dry gas may flow in a direction opposite the movement of the reconstituted wet substrate, resulting in negligible time, space, and/or energy (if applicable). Removal of the reconstitution solvent used may require very little dry gas to dry the reconstituted wet substrate. Equipment and instrumentation may be used to monitor and control at least the temperature, pressure, composition, and/or flow rate of gas in the drying zone 5.

The drying zone 5 may also be configured such that "controlled volume consolidation" is observed in the substrate, process wet substrate, reconstituted substrate, and/or welded substrate during the drying process. Good. "Controlled volume consolidation", as used herein, means a particular manner in which the finished welded substrate undergoes volume shrinkage during drying and/or reconstitution and/or conforms to a particular shape. To do. For example, for one-dimensional substrates such as knitting yarns, controlled volume consolidation can occur either when the knitting yarn diameter is reduced and/or when the knitting yarn length is shortened.

Controlled volume consolidation can be limited to one or more directions/dimensions by appropriately constraining at least the reconstituted wet substrate during the drying process. Further, the amount and type of process and/or reconstitution solvent used, the method of application of the process and/or reconstitution solvent (including the degree and type of viscous drag, etc.) should be such that the reconstituted wet substrate will shrink when dried. It can affect how much you do. For example, in 1D substrates (eg, knitting yarns, sutures), controlled volumetric compaction is one of the deposition processes (particularly process solvent recovery zone 4, drying zone 5, and/or deposition substrate collection zone 6). By configuring the drying zone 5 such that the substrate is subjected to the proper amount of tension during one or more steps, it is limited to only a reduction in diameter. Similarly, in the example of a two-dimensional sheet-type substrate, the substrate in one or more steps of the fusing process (particularly process solvent recovery zone 4, drying zone 5, and/or fusing substrate collection zone 6). Appropriate tensioning and pinning of the can constrain the controlled volume consolidation such that it affects only the substrate thickness and does not change the substrate area (length and/or width). Alternatively, the sheet-type substrate may allow controlled volume reduction in one or more dimension directions.

Controlled volume consolidation is a reconstitution wet substrate in the drying zone 5 to control the direction in which the substrate shrinks or to physically match the finished welded substrate to a particular shape or morphology. Can be promoted and/or limited by a dedicated device that holds the substrate as it dries. For example, there are a series of rollers that prevent the cardboard substitute product from shrinking in the length or width of the roll, but allow the material to shrink in the thickness direction. Another example is a mold on which a reconstituted wet substrate can be pressed to take a specific 3D shape and retain that shape when dried.

In one aspect of the welding process according to the present disclosure, the drying zone 5 may be configured such that the reconstituted wet substrate can be subjected to a pressure below atmospheric pressure and exposed to a relatively small amount of dry gas. In such a configuration, the reconstituted wet substrate may be lyophilized. This type of drying can be advantageous in preventing or minimizing the amount of shrinkage that occurs when the reconstituted solvent sublimes.

In one aspect of the deposition process according to the present disclosure, where the reconstitution solvent used is harmless (eg, water), the drying zone 5 may be omitted and the reconstitution wet substrate proceeds directly to collection. For example, the reconstituted wet substrate configured as a knitted yarn may be wound onto a collection reel and air dried after collection and/or collection.

F. Welding base material collection zone

The welding base material collecting zone 6 may be a portion of the welding process where the welding base material (for example, the finished composite material) is collected. In some aspects of the present disclosure, the weld substrate collection zone 6 may be configured as a roll of material (eg, a coil of weaving yarn, a cardboard substitute, etc.). The welding base material collecting zone 6 may use, for example, a saw or a stamp for cutting and/or forming a sheet from the welding base material configured as a composite material extruded product. In one aspect, an automatic stacking device may be used to package the bundle of finished composites. Further, in the example of a rolled and wrapped 1D welded substrate, the method of winding and wrapping may be configured to act on one or more variables that affect the viscous drag of the welding process.

In one aspect of the welding process according to the present disclosure configured for use with certain 1D substrates (eg, textile yarns and/or similar substrates), immediately after process solvent application zone 2 or process temperature/pressure zone. Either immediately following, it may be advantageous to use a device for coiling the welded substrate onto a cylindrical or tube-like structure. The apparatus can be used to produce a three-dimensional tube-like structure from a one-dimensional substrate before the substrate enters the process solvent recovery zone 4. The substrate may then conform to the new tube-like shape. Such apparatus is intended to produce a functional composite material from a textile yarn substrate containing a functional material (eg, a catalyst embedded in a textile yarn), without limitation unless so indicated in the following claims. It is envisioned that it may be particularly useful when using a welding process that is at least partially configured in.

In another aspect of the welding process according to the present disclosure configured for use with certain 1D substrates (eg, textile yarns and/or similar substrates), immediately after process solvent application zone 2 or at process temperature/pressure. It may be advantageous to use a device capable of knitting or weaving the substrate, either immediately after zone 3. The apparatus may be configured to produce a fabric structure from the substrate before it enters the process solvent recovery zone 4. Such a device may be configured such that the welding process can produce 2D fabrics with unique properties that cannot be achieved by other manufacturing means.

In yet another aspect of the welding process according to the present disclosure configured for use with certain specific 1D substrates (eg, textile yarns and/or similar substrates), an apparatus capable of producing a coiled package of textile yarns ( For example, it may be advantageous to use traverse cams. Such a device may be configured to wind the welded substrate into a coil-like package that can be subsequently unwound without entanglement.

G. Solvent collection zone

As mentioned above, the process solvent may be washed from the process wet substrate by the reconstituted solvent in the process solvent recovery zone 4. Thus, the reconstituted solvent may be mixed with various portions of the process solvent (eg, ions and/or any molecular components, etc.). This mixture (or relatively pure process solvent or reconstituted solvent) may be collected at any suitable point within the solvent collection zone 7. In one aspect, the collection point may be located near the point of introduction of the process wet substrate. Since the lowest concentration of process solvent component in the process-wet substrate is the lowest concentration of process solvent component in the reconstitution solvent, such a configuration is suitable for process-wet substrates. It can be particularly useful for configurations that utilize a stream of reconstituted solvent. This configuration not only facilitates separation and recycling of the process and reconstituted solvent, but may reduce the amount of reconstituted solvent used.

In the solvent collection zone 7, various devices and instrumentation are used to monitor and control at least the temperature, pressure, composition, and flow rate of the reconstituted solvent, process wet substrate, and/or reconstituted wet substrate. May be.

H. Solvent recycling

In one aspect, the deposition process according to the present disclosure may be configured to recover mixed solvents (eg, partially reconstituted solvent and partially processed solvent), a relatively pure process solvent, and/or a relatively pure process solvent. The pure reconstituted solvent may be recovered and recycled. A variety of equipment and/or methods may be used to separate, purify, and/or recycle the reconstituted solvent and process solvent. Any known or later-developed method and/or device may be used to separate the reconstituted solvent and the process solvent, the optimum device for such separation is at least the chemical composition of the two solvents. Will depend. Accordingly, the scope of the present disclosure is in no way limited by the particular apparatus and/or method used to separate the reconstituted solvent and the process solvent, as such apparatus and/or method may include cosolvents and/or Simple distillation of ionic liquids (eg, the method described in US Pat. No. 8,382,926), fractional distillation, membrane-based separations (eg, pervaporation and electrochemical crossflow separations). ), supercritical CO ₂ phase, and the like, but are not limited thereto. After sufficient separation of reconstituted solvent and process solvent, each solvent may be recycled to the appropriate zone within the process.

I. Mixed gas collection

As mentioned above, reconstituted solvent entangled in the reconstituted wet substrate may be removed from the substrate in drying zone 5. In one aspect, either the mixed gas containing the carrier dry gas having a portion of the reconstituted solvent gas therein or the reconstituted solvent gas may be recovered from the drying zone 5. Devices and/or instrumentation may be used to monitor and control at least the temperature, pressure, composition, and/or flow rate of the recovered gas.

J. Mixed gas recycling

Once recovered, the gas may be sent to a device that separates and recycles the carrier dry gas, the reconstituted solvent, or both. In one aspect, the apparatus may be single or multi-stage condenser technology. Separation and recycling may also include gas permeable membranes and other technologies and is not limited unless so indicated in the following claims. The carrier gas may be discharged into the atmosphere or returned to the drying zone 5, depending on the choice. The reconstituted solvent may be discarded or recycled to the process solvent recovery zone 4, depending on the choice.

In general, a welding process configured according to the above aspects comprises the step of converting natural fibers and/or particles containing a substrate into a substrate feed zone 1, a process solvent application zone 2, a process temperature/pressure zone 3, a process solvent. It may be configured to convert to a finished weld substrate in a continuous and/or batch welding process using a recovery zone 4, a drying zone 5 and a weld substrate collecting zone 6. In some embodiments, monitoring and controlling the amount, composition, time, temperature, and pressure of process solvent based on the substrate can be extremely important.

3. Example of welding process (Figs. 1 and 2)

Referring to FIG. 1, the substrate may be moved at a controlled rate by any suitable method and/or apparatus (eg, pushing, drawing, conveying system, screw extrusion system, etc.). In one aspect, the substrate continuously comprises a substrate feed zone 1, a process solvent application zone 2, a process temperature/pressure zone 3, a process solvent recovery zone 4, a drying zone 5, and/or a welded substrate collection zone 6. You may pass to. However, the specific order in which the substrate progresses from one zone 1, 2, 3, 4, 5, 6 to another may vary from welding process to welding process, and in some welding processes according to the present disclosure. The substrate may pass through the welded substrate collection zone 6 prior to moving to the drying zone 5, as described above for aspects. Additionally, in some aspects, the substrate may remain relatively stationary while the solvent and/or other deposition process components and/or equipment are in transit. At any point in a welding process constructed in accordance with the present disclosure, automation, instrumentation, and/or equipment may be used to monitor, control, report, operate, or process the welding process and/or one or more components of the equipment. And/or otherwise interact. Such automation, instrumentation, and/or equipment may monitor and control the force (eg, tension) exerted on the substrate, process wet substrate, reconstituted substrate, and/or finished welded substrate. These include, but are not limited to (unless indicated in the following claims). In general, the various process parameters and equipment used in the deposition process may be configured to control the amount of viscous drag to a desired process solvent application. The various process parameters and equipment used in the deposition process may be configured to perform controlled volume consolidation to obtain a deposited substrate with desired properties, form factors, and the like.

With further reference to FIG. 1, in the embodiment of the deposition process depicted, the process solvent loop comprises a process solvent application zone 2, a process temperature/pressure zone 3, a process solvent recovery zone 4, a solvent collection zone 7, and It can be defined as solvent recycle 8, after which the process solvent may be transferred to the process solvent application zone 2 again.

In another aspect of the deposition process shown in FIG. 1, the reconstituted solvent loop is two separate reconstituted solvent loops, one in the liquid state and one in the gas state. It may be defined as a loop. The liquid reconstituted solvent loop may include a recovery zone 4, a solvent collection zone 7, and a solvent recycle 8, after which the reconstituted solvent may be transferred back to the process solvent recovery zone 4. The gaseous reconstituted solvent loop may include a process solvent recovery zone 4, a drying zone 5, a mixed gas collection 9, and a mixed gas recycle 10, after which the reconstituted solvent moves back to the process solvent recovery zone 4. May be. In the gaseous gas reconstitution solvent loop embodiment, some of the reconstitution solvent may be carried to the drying zone 5 by the reconstitution wet substrate.

In a welding process according to the present disclosure in which a carrier gas is used, the carrier gas may be recycled in a loop that includes a drying zone 5, a mixed gas collection 9, and a mixed gas recycle 10, after which the dried gas is dried again. You may move to zone 5.

For commercialization, recycling of process solvent, reconstitution solvent, carrier gas, and/or other deposition process components can be very important. Further, any loop of process solvent, reconstitution solvent, carrier gas, and/or other deposition process components may include buffer tanks, storage vessels, etc., without limitation unless otherwise indicated in the following claims. As will be discussed in further detail below, the specific choice of substrate, process solvent, reconstitution solvent, dry gas, and/or desired finished weld substrate will be at least the optimum weld process steps, sequence thereof, weld deposition. It can significantly affect the process parameters and/or the equipment used for them.

In view of the above description, it will be apparent that the welding process according to the present disclosure may be separated into separate processing steps. For example, one deposition process consists of a substrate feed zone 1, a process solvent application zone 2, a process temperature/pressure zone 3, and a deposited substrate collection zone 6, followed by a process wet substrate for some time. It may be stored or aged and then serve as the process solvent recovery zone 4 and/or the drying zone 5. Again, in some embodiments one or more treatment steps may be omitted (eg, drying zone 5 when water is used as the reconstitution solvent). Further, in some aspects of the welding process according to the present disclosure, several process steps may occur simultaneously, or, as will be detailed below, the end of the process will naturally start another process step. You may flow to the section.

Referring now to FIG. 2, a schematic diagram illustrating various aspects of another deposition process that can be configured to produce a deposited substrate is provided. The illustrated deposition process is similar to that shown in FIG. 1, but in FIG. 2 the process temperature/pressure zone 3 and process solvent recovery zone 4 constitute separate deposition process steps. Instead, they may be combined into one continuous welding process step. Therefore, the deposition process shown in FIG. 2 may use two mixed gas recovery zones 9, the solvent collection zone 7 mainly collecting the process solvent and the solvent recycling mainly adapted to the process solvent. (As opposed to a mixture of process solvent and reconstitution solvent). It is envisioned that such an arrangement may provide some advantages associated with device simplification and/or consolidation. In various deposition processes according to the present disclosure, the process solvent recovery zone 4 may be configured such that the reconstituted solvent and the process wetting substrate move in opposite directions, as shown schematically in FIG. 2A.

In an aspect of the deposition process configured according to FIG. 2, the deposition process is such that the reconstituted solvent comprises a component of the process solvent (eg, a mixture of 3-ethyl-1-methylimidizolium acetate and acetonitrile). , And a reconstitution solvent of acetonitrile) may be applied. In such a configuration, some of its advantages are detailed below, but some of the volatile acetonitrile can be captured and separated from the process solvent at any point in the deposition process, and the process solvent is controlled. Exist via any suitable method and/or device including, but not limited to, a low pressure environment, a carrier gas, and/or combinations thereof, without limitation unless the following claims indicate otherwise. In general, a sufficient concentration of 3-ethyl-1-methylimidizolium acetate can disrupt intermolecular forces in some substrates (eg hydrogen bonds in cellulose). Therefore, the combination of process temperature/pressure zone 3 and process solvent recovery zone 4 provides the desired property that the molar ratio of 3-ethyl-1-methylimidizolium acetate to acetonitrile destroys the intermolecular force in the substrate. The general welding process zone may be configured anywhere suitable to cause This general welding process zone may also constitute all or part of the reconstitution and recycling zone, provided that the proper flow rates, temperatures, pressures and other welding process parameters are properly designed and/or controlled. ..

With further reference to FIG. 2, the substrate is again, without limitation, unless otherwise indicated in the following claims, any suitable method and/or apparatus (eg, pushing, drawing, conveying system, screw extrusion system, etc.). May be used to move through the deposition process at a controlled rate. In one aspect, the substrate comprises a substrate feed zone 1, a process solvent application zone 2, a combination of a process temperature/pressure zone 3 and a process solvent recovery zone 4, a drying zone 5, and/or a deposited substrate collection zone 6. You may pass continuously. However, the specific order in which the substrate progresses from one zone 1, 2, 3, 4, 5, 6 to another may vary from welding process to welding process, and in some welding processes according to the present disclosure. The substrate may pass through the welded substrate collection zone 6 prior to moving to the drying zone 5, as described above for aspects. Additionally, in some aspects, the substrate may remain relatively stationary while the solvent and/or other deposition process components and/or equipment are in transit. At any point in a welding process constructed in accordance with the present disclosure, automation, instrumentation, and/or equipment may be used to monitor, control, report, operate, or process the welding process and/or one or more components of the equipment. And/or otherwise interact. Such automation, instrumentation, and/or equipment may monitor and control the force (eg, tension) exerted on the substrate, process wet substrate, reconstituted substrate, and/or finished welded substrate. These include, but are not limited to (unless indicated in the following claims).

With further reference to FIG. 2, in the embodiment of the deposition process depicted, the process solvent loop comprises a process solvent application zone 2, a combination of process temperature/pressure zone 3 and process solvent recovery zone 4, a (process) solvent. It can be defined as the collection zone 7, after which the process solvent may again be transferred to the process solvent application zone 2.

In another aspect of the deposition process shown in FIG. 2, the reconstituted solvent loop is as two separate loops, one for the reconstituted solvent in the liquid state and one for the process solvent in the gas state. May be defined. The liquid reconstituted solvent loop may include a combination of process temperature/pressure zone 3 and process solvent recovery zone 4, and one or more mixed gas collection zones, after which the reconstituted solvent is again processed in the process temperature/pressure zone. 3 may be moved to the combination of the process solvent recovery zone 4 and the process solvent recovery zone 4. The gaseous reconstituted solvent loop may include a drying zone 5, at least one mixed gas collection 9, and a mixed gas recycle 10, after which the reconstituted solvent is once again process temperature/pressure zone 3 and process solvent recovery zone 4. You may move to the combination with. In the gaseous gas reconstitution solvent loop embodiment, some of the reconstitution solvent may be carried to the drying zone 5 by the reconstitution wet substrate.

In a welding process according to the present disclosure using a carrier gas, the carrier gas may be recycled in a loop that includes a drying zone 5, at least one mixed gas collection 8, and a mixed gas recycle 10, after which the dry gas is You may move to the drying zone 5 again.

In the embodiment of the deposition process shown in FIG. 2, the deposition process may also include a carrier volatiles capture loop, which loop comprises a combination of process temperature/pressure zone 3 and process solvent recovery zone 4, at least one mixed gas trap. Collection 8 and mixed gas recycle 10 may be included. In aspects of the welding process according to the present disclosure in which the reconstituted solvent may be present in the process solvent, the welding process may include more than one carrier gas loop. For example, if the process solvent was configured as a mixture of 3-ethyl-1-methylimidizolium acetate and acetonitrile, acetonitrile can act as a reconstitution solvent.

Some welding processes include one or more electrically controlled valves, drive wheels, and/or substrate guides (eg, new loose ends or broken yarn ends, with little or no human intervention). It is envisaged that it may be advantageous to include a (re)threading thread guide in the apparatus of the welding process. It is envisioned that a welding process so configured may reduce both the amount of downtime of the welding process and the amount of human contact required for the welding process as compared to a welding process not so configured. To be done.

In one aspect, the process solvent recovery zone 4 may be configured such that the process wet substrate can be collected while the reconstituted solvent is introduced to the process wet substrate. For example, in a welding process configured to use knitting and/or sewing threads as the substrate, the winding mechanism can be located at the end of the process temperature/pressure zone 3. In one aspect, a winding mechanism may be included so that the reconstitution solvent is introduced into the process wetting substrate (eg, by spraying), and the process wetting substrate is continuously washed to reconstitute the wetting group. It may be converted into wood. Such a configuration may lead to a significant simplification of the overall welding process in that the substrate need not continuously flow from the process solvent recovery zone 4 to the drying zone 5. Instead, the reconstitution is more likely to occur as a batch process, causing certain parts of the substrate (eg, a cylinder or ball of yarn to be wound into a continuous, untangled entity). Manufacturable and reconfigurable. At some point, the reconstituted wetted package can be transferred to a secondary reconstitution process and/or sent to a drying zone to remove reconstitution solvent.

In another aspect, the deposition process is configured as a continuous process in which the substrate can move continuously through the process temperature/pressure zone 3-process solvent recovery zone 4-drying zone 5. In such a configuration, the substrate may be under tension and sometimes cause breakage, which can be very problematic for the efficiency of the welding process. Accordingly, the welding process may be configured with rollers, pulleys, and/or other suitable methods and/or devices that assist movement of the substrate through the welding process and reduce and/or eliminate damage. ..

Additionally and/or alternatively, the welding process may be configured to reduce the amount of tension the substrate experiences during all or part of the welding process. In such a configuration, the reconstitution solvent can be applied to the process-wet substrate, rather than the substrate passing through a separate tube, which is expensive and can also be more difficult to rethread. It may be moved within a particular space (eg, via an applicator, which is described in more detail below). Such a configuration may be used with any substrate format, such a configuration may be any 1D substrate (e.g., in a sheet-like configuration that includes a plurality of separate substrates disposed alone or adjacent to each other (eg, , Knitting and/or sewing threads), and/or 2D substrates (eg, fabrics and/or fabrics) may be particularly useful. The process solvent recovery zone 4 so configured reduces and/or eliminates friction and/or unwanted tension buildup on the substrate, which can increase substrate throughput of the deposition process.

4. Solvent Application Zone: Equipment/Method

Various aspects of the viscous drag concept associated with process solvent application are shown in FIG. 6A. This figure provides a cross-sectional view of an apparatus that may be used in process solvent application zone 2. Natural fiber substrates may differ in fiber density per unit cross section and/or unit area. The process solvent application to the substrate can be modulated such that the mass ratio of process solvent applied to the substrate per unit mass of substrate is well controlled. This involves actively monitoring substrate differences with appropriate sensors, and using this data to determine the speed of the process solvent pump and/or the speed of the substrate through the process solvent application zone and/or the process solvent composition. It can be realized by controlling. Alternatively, it is possible to create a point of viscous drag that applies appropriate squeezing force and/or shear to the process wet substrate to control the process solvent application. The viscous drag design may include a small volume that allows the process solvent to be properly pooled. The process solvent can then be applied such that the mass ratio of process solvent to substrate either remains stable or is modulated within the desired tolerance. (The modulated fiber welding process is described in more detail below).

In one aspect of the deposition process (either modulated or unmodulated unless otherwise indicated in the claims below), the deposition process is configured to apply the process solvent via an injector. May be. In one configuration of injector, the injector may comprise a capillary having two inlets and one outlet. Substrates, including textile yarns (or other 1D substrates) may enter through one inlet and process solvent may flow through the other inlet. The process-wet substrate (textile yarn to which the process solvent has been applied) may exit from the outlet. The injector may include additional inlets for adding functional material, additional process solvent, and/or other components. As described hereinabove, process wet substrates (eg, process solvent applied textile yarns, sutures, fabrics, and/or fabrics) are processed solvent application zone 2 followed by process temperature/pressure zone 3. You may proceed to.

As shown in FIG. 6A, injector 60 may be configured for use with either 1D or 2D substrates (eg, knitting yarn or fabric, respectively). The injector may include a substrate inlet 61 and an opposite substrate outlet 64. Injector 60 may be configured to deliver a controlled amount of process solvent to one or more substrates, which may include fabrics, fabrics, knitting yarns, sutures, etc., generally In particular, it may be further configured to properly distribute the process solvent around and within the substrate. For example, in a non-modulation deposition process, it may be desirable to have the process solvent evenly distributed throughout a given substrate, whereas in a modulated deposition process, the process solvent distribution in a given substrate may vary. It may be desirable to make a change.

One example of an injector 60 so configured may include a shell having a T-shaped cross section, with the 1D or 2D substrate entering the injector and exiting through a relatively straight path. .. The process solvent may be pumped through the secondary inlet, which may be in a path that is generally perpendicular to the substrate inlet. An injector 60 having such a structure is shown in FIG. 6A.

As shown in FIG. 6A, the injector 60 may include a base material inlet 61 to which a raw base material (knitting yarn, sewing thread, cloth, fabric, etc.) may be supplied. The injector 60 may also include a process solvent inlet 62 in fluid communication with a portion of the substrate inlet 61. As such, process solvent may flow into the injector 60 through the process solvent inlet 62 and entangle the substrate adjacent the application interface 63. This part of the injector 60 may constitute the process solvent application zone 2 as described above.

When configured for use with a 1D substrate, the portion of injector 60 from substrate inlet 61 to substrate outlet 64 may be configured like a tube. When configured for use with a 2D substrate, the portion of injector 60 may be configured as two spaced plates (similar to the device shown in FIG. 6C, which is described in further detail below). Exist). The substrate and/or the process wet substrate may be disposed in the space between the two plates 82, 84, at least one plate 82, 84 being formed with at least one process solvent inlet 63. May be.

The substrate outlet 64 may engage a portion of the injector 60 that is generally opposite the substrate inlet 61. In one configuration of injector 60, substrate outlet 64 may be non-linear, as shown in Figure 6A. The non-linear substrate outlet 64 may be configured to physically contact the outer surface of the process wet substrate to direct the process solvent to the desired portion of the substrate, which physical contact comprises: It may be achieved at at least one or more inflection points, which may impart shear and/or compression forces to the substrate. Additionally, the non-linear substrate outlet 64 may be configured to make physical contact with the outer surface of the process wet substrate. This physical contact can be one way of achieving the desired viscous drag of a given welding process. Physical contact may be configured to add further smoothness to the outer surface of the process wet substrate, eliminating and/or reducing short hairs/fibers of the resulting welded substrate. Physical contact with the process-wet substrate may also improve heat transfer from the process solvent to the substrate and/or the process-wet substrate, which heat transfer reduces the required processing time (eg, welding time). Shortening, which may result in shortening the length of the welding chamber and reducing the space required for the equipment associated with a given welding process. Physical contact with the substrate and/or the process-wet substrate may be achieved by considering a number of designs (for making inflection points in one, two, and/or three dimensions), Examples include, but are not limited to, varying the dimensions (eg, diameter, width, etc.) and/or curvature of the substrate inlet 61, application interface 63, and/or substrate outlet 64, and/or these. , Placing another structure adjacent to the substrate and/or the process-wet substrate (eg, wiper, baffle, roller, flexible orifice, etc.), and the like in the claims below. There is no limitation unless otherwise indicated.

Alternatively, the injector may be configured to be Y-shaped and/or the one or more injectors may add process solvent, functional material, and/or other components to a particular location, at a particular location. Under conditions, it may be configured in multiple stages for addition at one or more points in the welding process.

In one aspect, the injector may be used with a knitting yarn receiver, wherein both the injector and the knitting yarn receiver selectively move the rail system and/or the injector and knitting yarn receiver along one direction. It may be configured to slide over any other suitable method and/or device that can be placed. A welding process configured to selectively manipulate one or more injectors and/or knitting yarn receivers in at least one direction (eg, by allowing sliding along the length of the rail system). Is the time and/or resources required to re-pass the weaving thread and/or the sewing thread to any point in the welding process (especially in the process temperature/pressure zone 3) as compared to the welding process without such selective manipulation. Can be reduced, while at the same time allowing a (more) dense welding process to be multiplexed in a relatively small space.

For example, in a fusing process consisting of "n" knitting yarns processed simultaneously, only the outer yarns are easily accessible. For this reason, when the individual knitting yarns are broken, it may be difficult to carry out rethreading. By having a removable, orbital injector at the beginning of the substrate feed zone 1, the process solvent application zone 2, and/or the process temperature/pressure zone 3, (human or automated equipment) facilitates the injector. It can be removed and moved to the end of a group of substrates that have been placed in the welding process and rethreaded. For some applications it may be advantageous to configure the injector in a clamshell type, but it is also possible to be an assembly of tubes, without limitation unless so indicated in the following claims. Inspired. That is, the injector can be designed in a "clamshell" shape in which at least two materials surround the yarn or group of yarns. This also lends itself to the design of a system that facilitates the loading of the yarn into the fusing process machine initially and simultaneously provides suitable viscous drag to multiple ends of the yarn. When any particular injector is removed, the other injector slides down to a position that closes the existing void, creating a new void located at one edge of the equipment for the welding process. A series of receiving units located at or near the end of any given process zone may operate in concert and move accordingly, so that the individual yarns are each renewed. Move to position.

The optimum configuration of the receiving unit may vary depending on the aspect of the welding process and may depend at least on the size of the substrate, the process solvent used, and/or the type of substrate used. In one aspect, the receiving unit may include a simple pulley or yarn guide to direct the yarn to the process solvent recovery zone 4 and/or the drying zone 5. In another aspect, the receiving unit is dependent on how the deposition process is configured, such as the configuration of process solvent application zone 2, process temperature/pressure zone 3, process solvent recovery zone 4, and/or drying zone 5. Can be quite complex (ie, the winding mechanism).

Another device illustrating the concept of viscous drag related to process solvent application is shown in FIG. 6B. The device may be configured as a tray 70 and may be configured to use both 1D and 2D substrates as shown in Figure 6B. As shown, the tray 70 may be configured with one or more substrate grooves 72 formed in the surface of the tray 70. The tray 70 may have multiple grooves 72 such that the process solvent can be applied to multiple substrates simultaneously (1D substrate shown in FIG. 6B).

The groove 72 shown in FIG. 6B may be linear, but in other aspects of the tray 70, the groove may be non-linear relative to the injector 60 shown in FIG. 6A and the plate shown in FIG. 6C. That is, the tray 70 and its groove 72 may be configured such that a portion of the tray 70 and/or groove is in physical contact with a portion of the substrate (physical contact optimizes viscous drag. Can be a consideration for). Physical contact may be achieved through a number of design considerations (to produce inflection points, shear forces, compression, etc. in one, two, and/or three dimensions), examples of which include, but are not limited to, Although not by varying the depth of the groove 72, the cross-sectional shape of the groove 72, the width of the groove 72, the curvature of the groove 72 and/or a combination thereof, and/or another structure for substrate and/or process wetting. Placement adjacent to the substrate (eg, wipers, baffles, rollers, flexible orifices, etc.) and the like, without limitation, unless otherwise indicated in the following claims.

In one configuration, the spacing of 1D substrates can be reduced to the point where multiple substrates essentially move together in a two-dimensional plane or "sheet", as further illustrated in Figure 6C. In another configuration, the width of the groove 72 may be selected to allow a generally two-dimensional sheet of fabric and/or fabric to move through the groove 72 relative to the tray 70.

Generally, the process solvent is continuous in each groove 72 and/or a portion thereof such that as the substrate moves along the grooves 72, the process solvent is applied to the substrate to form a process wet substrate. May be supplied in a positive manner. The groove 72 may be flooded with process solvent (in this configuration, the groove 72 may function similar to a process solvent bath) and/or the process solvent is applied to the substrate adjacent the tip of the groove 72. , May then be suitably wiped along the outer surface portion of the substrate as it moves toward the trailing edge of the groove. In one configuration of the deposition process, the tray 70 may be angled with respect to the horizontal to use gravity to the process solvent, the optimal angle being at least the speed and direction of movement of the substrate relative to the tray 70. May depend on.

The optimum configuration of each groove 72 is expected to vary from application to application of the welding process, and therefore does not limit the scope of the present disclosure in any way, unless so indicated in the following claims. When configuring a plurality of 1D substrates laterally spaced at a distance equal to or greater than the average diameter of each substrate, the width of the groove 72 may be approximately the same as its depth, and each dimension is a substrate. It is envisioned that the average diameter may be about 10% larger.

The optimum cross-sectional shape of each groove 72 may also vary from welding process to welding process. For example, in some applications it may be optimal for the cross-sectional shape of the groove 72 (or at least its bottom portion) to be approximately the same and/or to match the cross-sectional shape of the substrate (or at least a portion thereof). For example, the groove 72 may be configured with a U-shaped cross section when configured for use with a substrate that includes 1D knitting or sewing threads. When configured for use with substrates including 2D fabrics or fabrics, the grooves 72 may be configured with a width much larger than their depth (eg, 10 times, 20 times, etc.). However, the particular cross-sectional shape, depth, width, configuration, etc. of groove 72 does not limit the scope of the present disclosure in any way, unless so indicated in the following claims.

The configuration of process solvent application zone 2 configured for use with multiple 1D substrates (which may include sutures and/or weaving yarns) close to a 2D sheet is shown in FIG. 6C. The process solvent application zone 2 uses a first plate 82 and a second plate 84 having corresponding bends to create at least three points of physical contact (ie, inflection points) in at least one dimension. Good. In other configurations, the plates 82, 84 may be configured differently to create more or less inflection points in one or more dimensions, where the inflection points are the substrate and/or process. It may be configured to add more or less resistance to the wet substrate. Physical contact may be achieved by a number of design considerations (to create inflection points in one, two, and/or three dimensions), including, but not limited to, plates. Changing the distance between 82, 84, the curvature of one of the plates 82, 84, whether the concave portion of the curved surface of one plate 82, 84 corresponds to the convex portion of the curved surface of the other plate 82, 84, and And/or combinations thereof, and/or disposing another structure adjacent to the substrate and/or the process wet substrate (eg, wiper, baffle, roller, flexible orifice, etc.) and the like, including: There is no limitation unless so indicated in the claims of.

In another configuration, the viscous drag may vary based at least on the relative position of one or more structural components. For example, referring specifically to FIGS. 6D, 6E, and 6F, the plate may be configured such that its inner edges overlap by an adjustable amount. If the inner edge overlap is greater, as shown in FIG. 6E, the substrate placed between the corresponding plates may have greater physical resistance to movement relative to the plates. If the inner edge overlap is smaller, as shown in FIG. 6E, the substrate placed between the corresponding plates may have less physical resistance to movement relative to the plates. The figure shows an adjustable overlap applied to a welding process configured for use with a plurality of 1D substrates placed adjacent to each other. The adjustable relative position of the plates allows multiple process solvents for a given device and/or a given device for a welding process to be configured to produce a weld substrate having different attributes. can do.

As described above with respect to the viscous drag concept and FIGS. 6A and 6B, the plates 82, 84 in FIGS. 6C, 6D, and 6E may be configured to control process solvent application. The designs shown in FIGS. 6A-6E are not meant to be limiting in any way, unless so indicated in the following claims, as long as the process solvent is properly applied to the substrate and/or the substrate and Any suitable structure and/or method may be used to properly interact with the process wet substrate and/or achieve the desired attributes for the weld substrate. That is, a suitable amount of viscous drag can be achieved by any number of structures (which can be moved to preset tolerances to achieve the desired process solvent application effect) or method, Examples include rollers, shaped edges, smooth surfaces, number and/or orientation of inflection points, resistance to relative movement, temperature fluctuations, etc., but no other indications in the following claims. As long as it is not limited to these.

In another configuration of the deposition process (either modulated or unmodulated, without limitation unless so indicated in the following claims), the deposition process uses an applicator to apply the process solvent. It may be configured. In one configuration of the applicator, the application may be correlated with that used in inkjet printers, screen printing technology, spray guns, nozzles, dip tanks, or tilt trays, and/or combinations thereof ( There are no limitations, at least some of which are shown in Figures 6A-6F and detailed above), unless so indicated in the following claims. The welding process involves the applicator directing the process solvent to the substrate when the substrate (eg, weaving thread, suture, fabric, and/or fabric) is properly positioned relative to the applicator, thereby It is envisioned that it may be configured to make a process wet substrate. Such a deposition process may be configured such that the process solvent and/or the functional material can be applied to the multi-dimensional pattern, which uses the deposition process to emboss the pattern on the fabric and/or fabric. Can be useful to. Such a pattern may constitute a modulated deposition process (discussed further below), where the modulation is at least a result of application of the process solvent to the substrate. As described hereinabove, process wet substrates (eg, process solvent applied textile yarns, sutures, fabrics, and/or fabrics) are processed solvent application zone 2 followed by process temperature/pressure zone 3. You may proceed to.

Referring to FIGS. 11A-11D, in the configuration of a modulation deposition process using an injector or applicator, the modulation deposition process comprises at least controlling the at least pump flow rate of the individual process solvent components in real time for the process solvent. The composition can be varied. The modulated deposition process is at least controlled by controlling the pump flow rate of the process solvent components and/or at least by the variable speed of the substrate through the process solvent application zone 2 to a ratio of process solvent to substrate (volume or mass basis). May be changed). A schematic diagram of such a modulation welding process is shown in FIG. 11B for 2D substrates and in FIG. 11D for 1D substrates, all of which are described in further detail below.

Referring now to FIGS. 11A (2D substrate) and 11C (1D substrate), the modulation welding process may be configured to allow temperature modulation by any suitable method and/or apparatus, as an example. Includes, but is not limited to, microwave heating, convection, conduction, radiation, and/or combinations thereof, unless otherwise indicated in the claims below. The modulation deposition process may be configured to allow modulation of the pressure, tension, viscous drag, etc. experienced by the substrate and/or process wet substrate. Welding including weld yarns that exhibit a unique dye and/or coloring pattern and a unique feel and/or finish due to the combined action of the modulation of various parameters of the modulation welding process, including but not limited to the above conditions. The substrate can be manufactured.

Conversely, as noted above, the deposition process can be made very difficult without modulation of various process parameters (eg, process solvent composition, process solvent to substrate mass ratio, temperature, pressure, tension, etc.). By being configured to operate consistently, it may be configured to provide a weld substrate with consistent features (eg, color, size, shape, feel, finish, etc.) throughout.

In one aspect of a welding process configured for mass production of a weld substrate (eg, a sheet-like structure including a plurality of adjacent knitting yarns) from a plurality of 1D substrates disposed adjacent to each other , Multiple ends of a knitting yarn can be moved as a sheet, which can improve the economies of scale of some welding processes. The concepts and principles relating to the welding process configured for the same 2D substrates (eg, fabric, paper substrate, woven, and/or composite mat substrate) disclosed herein are adjacent to one another. It can be applied to multiple ID substrates arranged.

Illustrating by example, a welding process configured to weld a plurality of 1D substrates into a sheet-like configuration includes a welding process configured to weld a 2D substrate (eg, fabric and/or fabric). Although similar, it is envisioned that the welding process for 1D substrates may have some important differences. Such differences include, but are not limited to, adaptations to reduce and/or eliminate the likelihood that one substrate may become entangled with itself and/or another substrate (eg, a separate yarn). , Yarn guides), and process solvent applications can use injectors, either for individual yarns or for groups of yarns. Alternatively, the fusing process may be performed by spraying, impregnating, wicking, dipping, and/or otherwise introducing the process solvent into the sheet-like configuration at a controlled rate to form a sheet-like configuration of a 1D group. It may be configured so that it does not require an injector when applied directly to the material. Thus, according to the present disclosure, various devices and/or methods may be configured to provide mass production scale highly multiplexed deposition processes.

A. Low moisture base material

Cellulose (ie, cotton, linen cloth, regenerated cellulose, etc.) and lignocellulose (ie, industrial cannabis, agave, etc.) fibers are known to contain sufficient (5-10% by weight) water. Moisture levels, for example for cotton, can vary by approximately 6-9% depending on pick-up temperature and relative humidity. In addition, 1-ethyl-3-methylimidazolium acetate (“EMIm OAc”), 1-butyl-3-methylimidizolium chloride (“BMIm Cl”), and 1,5-diaza-bicyclo[4 .3.0] IL-5 solvents such as non-5-enium acetate (“DBNH OAc”) are often contaminated with water during synthesis and/or by absorption from the environment. Furthermore, molecular component additives such as acetonitrile (ACN) to the process solvent are also hydrous. In general, the presence of water adversely affects the effectiveness of IL-based solvents with pure ionic liquids and molecular component additives to dissolve biopolymer substrates. However, it can be difficult and/or resource intensive to remove a minimum of a few points (mass %) of water from these solutions. The cost of ionic liquids and IL-based solvents can be directly correlated with their purity, especially the water content. Accordingly, the welding process may be configured to utilize a low moisture substrate to improve the performance of the welding substrate as well as to improve the overall economics of such a welding process.

In addition to being useful for welding processes that use ionic liquids and IL-based process solvents, low moisture substrate materials are also useful for fiber welding processes that use N-methylmorpholine N-oxide (NMMO) as the process solvent. obtain. Generally, NMMO solutions with 4 to 17 wt% water have the ability to dissolve cellulose and can be used in lyocell-type processes. The use of sufficient dry biopolymer-containing substrate material may constitute the deposition process with a process solvent having a water content above the upper limit (about 17% by weight) and still be efficient and economically desirable. It means to produce a welding base material. Ionic liquids that are moisture sensitive (eg, 1-butyl-3-methylimidizolium chloride (“BMIm”) Cl, 1-ethyl-3-methylimidazolium acetate (“EMIm OAc”), 1,5- In a deposition process configured to use a process solvent that includes diaza-bicyclo[4.3.0]non-5-enium acetate ("DBNH OAc", etc.), the amount of water in the substrate is Can affect the rate at which they occur and, thus, the associated process parameters and equipment design. Welding processes configured to use process solvents that are less moisture sensitive than some of the ionic liquids disclosed above (eg, NMMO, LiOH-urea, etc.) reduce the benefits of relatively dry substrates. And/or eliminated.

Thus, the experiments show the surprising results of a welding process configured to use a biopolymer substrate that was artificially dried to a low moisture state (<5 wt%) before welding. The low moisture substrate speeds up the deposition process while at the same time improving the quality of the deposition substrate (ie, strength, lack of stray fiber, etc.). Even more surprisingly, water is removed from ionic liquids and IL-based process solvents due to the strong drying properties of low moisture biopolymer substrates. In one aspect, water may be removed from ionic liquids and IL-based process solvents reconstituted with a non-aqueous medium (eg, ACN). In fact, the low moisture substrate purifies both process solvent and reconstitution solvent water while it is continuously recycled within the fiber deposition process.

The low moisture substrate material is, for example, in a sufficiently dry (and optionally warm, e.g., about 40-80<0>C) atmosphere prior to introduction into a deposition process utilizing a process solvent containing a moisture sensitive ionic liquid. , May be obtained by preconditioning the material over a controlled period of time. It can be important to keep the biopolymer-containing substrate in a controlled environment before and during the welding process. In addition, the intentional introduction of water into certain areas of the space within the biopolymer substrate may have the effect of delaying the in-situ deposition, allowing another way of modulating the deposition process. May be. Several methods are described below.

Generally, an artificially dried substrate (eg, substrate dried prior to introduction into substrate feed zone 1 and/or substrate dried in all or part of substrate feed zone 1). Experiments have shown that a welding process configured to utilize H.sub.2 results in a surprising new synergistic effect that improves the economics of the welding process and/or the welding substrates produced thereby. For example, drying a cotton substrate to less than 5 wt% moisture can dramatically improve the consistency and/or control of deposition when using a BMImCl+ACN solution (or other moisture sensitive process solvent system). Furthermore, when the dry cotton substrate is used continuously and when the process solvent is recycled multiple times, as long as the device is properly sealed from external water (eg, atmospheric water), the process solvent (eg, BMIm). Experiments have shown that the water content of both Cl+ACN) and reconstitution solvent (eg ACN) can be lowered. The drying characteristics of dry cotton substrates increase as the water content decreases. In other words, cotton with a water content of 3% by weight has a greater drying action than cotton with a water content of 4% by weight.

5. Characteristics of welded substrates produced on a commercial scale

The above description discloses the properties of various novel materials that may be produced using the welding process according to the present disclosure, which materials are commonly referred to as 1D and 2D welded substrates. The following properties are novel and non-obvious in the light of the prior art, since the following materials are only present in the materials produced in large quantities (eg on a commercial scale): Such material properties may allow for reduced manufacturing costs for textiles as well as new uses for textiles containing natural substrates (eg, cotton).

It is well known that petroleum-based materials (eg, polyester, etc.) can be configured to produce both filament type and staple fiber yarns. As used herein, the term "staple fiber knitting yarn" means a knitting yarn spun from fibers having relatively short, discrete lengths (staple fibers). However, prior to the processes and devices disclosed herein, filament-type yarns derived from natural staple fibers, including natural staple fibers (and, consequently, filament-type yarns derived therefrom). ) Did not retain the original properties and structure of the staple fiber to some extent. The process and apparatus disclosed herein are capable of differentiating from all previous teachings regarding rayon, modal, TENCEL®, etc., where artificial staple fibers are used for complete dissolution and/or derivatization of cellulose. Manufactured by and then extruded (complete dissolution can be achieved using NMMO, ionic liquid based systems, etc.). In the case of rayon, modal, TENCEL (registered trademark), etc., the cellulosic precursor is completely dissolved and modified to remove the cellulose source (for example, beech wood pulp, bamboo pulp, cotton fiber, etc.) from which staple fibers are derived. It is virtually impossible to judge. In contrast, a welded substrate produced in accordance with the present disclosure retains some of the properties, characteristics, etc. of staple fibers in the substrate, as further detailed below. In maintaining these original characteristics, features, etc., the method and apparatus of the present invention uses a relatively small amount of process solvent per unit of the welding base material used, as compared with the prior art, and moreover, is conventionally synthesized. And/or enables new functions associated with petroleum-based filament-type knitting yarns (eg, lowering water content, increasing strength, etc.). These new welded substrates and their capabilities, in turn, enable new fabric-wide applications not possible with the prior art. To what extent the welding base material performs these functions depends on at least the configuration of the welding process used for manufacturing the welding base material.

Included in the 1D fusing substrates that may be produced using the fusing process of the present disclosure are untwisted "single yarns" and twisted yarns (woven and sewing yarns) and "fused yarn substrates." Although the above attributes and examples may be attributed to a welded yarn substrate, the scope of the present disclosure is not so limited unless indicated in the following claims, and the term "1D welded substrate" is so. Not limited.

Generally, a welded yarn base material is distinguished from a conventional raw yarn base material equivalent product in at least the following points: (1) Amount of empty space between individual fibers constituting a knitting yarn: welded yarn base material The material is much denser than conventional raw substrate equivalents and has an average diameter of about 20% to 200% less than conventional knitting yarns of equal weight of biopolymer substrate per unit length; and (2) The welded yarn substrate is generally not abundant, if any, on the surface of loose fibers and therefore does not delaminate (the amount and characteristics of loose fibers on the surface can be manipulated during the welding process. ). Specific empirical data for the welded substrates and corresponding natural fiber substrates are detailed below.

Generally, when the loose fibers are present on the surface of the welded yarn substrate, at least a portion of the loose fibers are welded to the welded yarn substrate. That is, the fibers are not so loose that they actually separate from the welding yarn base material, but are fixed to the core of the welding fiber at the central portion of the welding yarn base material. This can occur when the process solvent tends to migrate to the center of the base knitting yarn during the fusing process. However, the welding process is such that at least the composition of the process solvent is varied to limit or promote welding in either the core or the outer portion of the textile yarn substrate, and/or multiple process solvent compositions are added at different times. May be configured to do so.

The above two attributes, alone and/or in combination, can be desirable/advantageous for a number of reasons. For example, non-peelable knitted yarns are spandex (also known as Lycra or elastane) or other synthetic fibers because loose fiber (lint) content is reduced and/or eliminated and does not cause problems on the knitting machine. And it can be knitted more efficiently. Lint and delamination are known problems in the textile industry as they cause defects in the fabric and lint buildup results in downtime of equipment that needs cleaning and/or repair. Adhesion by static electricity is a problem because it causes loose fibers to naturally adhere to synthetic fibers. The welded yarn substrate eliminates and/or mitigates delamination, thus greatly reducing these problems. Fabrics and/or fabrics made from welded yarn substrates and spandex (or lycra, etc.) are useful as active wear (eg shirts, pants, shoes etc.) and/or underwear (eg underwear, bras etc.) In some cases, and without limitation, as set forth in the following claims.

The welded yarn substrate may be manufactured to be stronger than conventional raw substrate equivalents (having similar weight per unit length and per unit diameter). The welded yarn substrate may eliminate the need for "slashing" (or "sizing") (warp sizing) during the manufacture of textile materials (eg, denim). Weaving yarn sizing is a process in which a sizing agent, such as starch, is applied to the yarn (most often before weaving) in order to provide sufficient strength to be processed in the weaving process. The size must be washed out during manufacture of the fabric. The slashing of textile yarns is not only costly, but also resource (eg, water) intensive. Thrashing is also not permanent in that the sizing removes the knitting yarn to its original (lower) strength. In contrast, the welding process can be configured such that the resulting welded yarn substrate is reinforced compared to traditional knitting yarns and eliminates the need for slashing, resulting in cost and resource savings as well as more permanent Gives strength improvement.

Textile bowing (skew) is a condition in which the warp and weft threads are straight but not at the correct angles to each other. This is due to the fact that conventional knitted yarns are twisted during manufacture and therefore biased for untwisting. Conventionally, the welded yarn base material has the property that, since the individual fibers can be fused/welded together, the fabric produced from the welded yarn base material can not be untwisted after the welding process. It may have the property of being much less warped than fabrics made from its raw substrate equivalents.

The fusing yarn base material is a low-twist knitting yarn, a knitting yarn having a shorter fiber length, and/or a knitting yarn manufactured from low-quality fibers (for example, fibers having different denier), which are more valuable and stronger It can be converted into a substrate. For example, in conventional knitting yarns, the twist factor correlates well with the strength. The more twists per unit length, the more costly. The low-twist knitted yarn used as a substrate in the welding process of the present disclosure is much stronger than the conventional knitted yarn substrate because the welding process is configured to fuse individual fibers. May be obtained.

Fused yarn substrates can convert uncombed knitted yarns into more valuable, stronger fused yarn substrates. In conventional yarns, the combing process removes short fibers from the sliver, producing higher strength yarns further down the manufacturing chain. Combing is mechanical and energy intensive and adds cost to the production of knitted yarns. Because the welding process can be configured to fuse short fibers and long fibers together to enhance strength, a textile yarn substrate made from a substrate that includes uncombed sliver is better than a conventional textile yarn substrate. Can produce much stronger welded yarn substrates. The fusing process may be configured to produce stronger knit yarns at significant cost savings.

Woven fabrics made from fusible yarn substrates may have the property of retaining their shape and are not as prone to shrinkage and/or propensity as fabrics made from conventional knitting yarns. Since the fusing process may be configured to produce a fusing yarn substrate that has significantly less loose fibers (little to no) on its surface as compared to conventional braiding yarns, the fabric is a conventional knitting fabric. It can be produced from a welded yarn base material having a much lower packing factor than that made from the yarn, in a manner similar to that performed with single filament synthetic textile yarns (eg polyester).

12A and 12B, SEM images of a raw denim 2D substrate and the resulting welded 2D substrate (using the raw substrate of FIG. 12A as the starting material) are shown, respectively. It can be easily visually observed that engagement with adjacent fibers is greater in the welded substrate than in the unprocessed substrate. The increased engagement between adjacent fibers provides the weld substrate with various qualities that are not present in the green substrate, including higher stiffness, lower moisture absorption, and/or increased drying rate. Are not limited to these.

Referring now to FIGS. 12C and 12D, SEM images of the raw knit 2D substrate and the resulting welded 2D substrate (using the raw substrate of FIG. 12C as the starting material) are shown, respectively. It can be easily visually observed that engagement with adjacent fibers is greater in the welded substrate than in the unprocessed substrate. The increased engagement between adjacent fibers provides the weld substrate with various qualities that are not present in the green substrate, including higher stiffness, lower moisture absorption, and/or increased drying rate. Are not limited to these.

In a fusing process configured to act on a 2D substrate (eg, a fusing process configured to produce a fusing substrate similar to that shown in FIG. 12B or FIG. 12D), the solubilized polymer is ( Adding to the substrate and/or the process solvent) and/or increasing the pressure on the process wet substrate in the process temperature/pressure zone 3 increases interlaminar adhesion in the production of multiple layered and/or laminated composites. Can be promoted. In general, the degree to which the substrate is welded (eg, high, medium, low) can affect the flexibility of the resulting welded substrate.

In addition to increasing burst strength, fabrics such as those shown in Figures 12B and 12D can exhibit a significant increase in fabric score when tested using the Martindale Pilling test. For example, a fabric containing a yarn base material that has a score of 1.5 or 2 in this test may have a moderate amount of suitable adhesion to the base material when the fabric is subjected to a welding process. , The score goes up to 5.

The fusible yarn base material may have excellent moisture wicking and absorption properties as compared to conventional knitted fabric yarns, specifically conventional cotton yarns. Accordingly, the welded yarn substrate dries faster than conventional knitted yarns, thereby providing associated cost and resource savings. In combination with a lesser tendency and/or tendency to shrink, fabrics containing a welded yarn substrate have a combination of moisture management and non-shrinkage that is an important attribute for active wear (eg sportswear), underwear (eg , Lingerie) and the like can be quite useful.

Woven fabrics made from fusible yarn substrates can be constructed to be much stronger by weight than fabrics made from conventional knitting yarns. Since the average diameter of the welding yarn base material for a given weight of the textile yarn may be smaller than the average diameter of conventional knitting yarn yarns, the burst strength of a fabric produced using the welding yarn base material is A significant increase is observed.

In addition, fabrics made from the fused yarn substrate can be configured to allow a wide range of deformations and controllable results in the "hand" (eg, feel, texture) and finish of the fabric. This is because the deposition process can be configured to add a coating to the substrate and/or adjust the depth of process solvent penetration into the substrate. For example, in one aspect of the fusing process, the fusing process can be configured to coat the textile yarn substrate with solubilized cellulose as a film, which can improve the smoothness of the outer surface of the resulting fusing yarn substrate. , There is a possibility of significant changes compared with the conventional equivalent to the unprocessed base material.

Examples of 2D fusing substrates that can be produced using the fusing process of the present disclosure include fusing substrate cardboard, fusing substrate paper mold materials, and/or fusing substrate paper replacement materials. While the above attributes and examples may be attributed to fusing substrate paper alternatives, the scope of the present disclosure is not so limited, and the term "2D fusing substrate" is such unless otherwise indicated in the following claims. Not limited to. In general, the materials of 2D welded substrates and/or their qualities allow a reduction in the manufacturing costs of paper-type materials and building materials, as well as new applications of these materials compared to conventional materials. ..

In general, the welded substrate paper replacement material is at least as good as the conventional raw substrate equivalent due to the fact that it may contain a significant amount (eg, greater than 10 wt% or volume%) of lignocellulosic material. Can be distinguished. Conversely, conventional cardboard and other paper materials contain refined cellulosic pulp with little or no lignocellulosic material. The fusing process according to the present disclosure may be configured to produce a fusing substrate paper replacement material that contains a significant amount of lignocellulosic material. The lignocellulosic material can function as either a low cost filler and/or a reinforcing (reinforcing) agent. These fusing-based paper alternatives may enable differentiation within the paper and cardboard industry, which is not currently seen. For example, low cost thermal sleeves for coffee cups, pizza, and other food delivery/packing boxes, boxes for shipping applications, clothes hangers, and the like. These fusing-based paper alternatives can be revolutionary in that the cost of pulping (eg, kraft pulping) is eliminated. Two-dimensional and/or three-dimensional fused substrates are used in paper and/or cardboard applications by providing stronger and/or lighter materials such as diapers, cardboard substitutes, paper substitutes, etc. , And may be useful without limitation unless so indicated in the following claims.

As part of a standard woven/fabric test used to validate and quantify the superior properties of a welded substrate in comparison to its raw substrate equivalent, including but not limited to: , (1) AATCC 135 (Washing Test-Cloth); (2) AATCC 150 (Washing Test-Clothing); (3) ASTM D2256 (Single Yarn Test); (4) ASTM D3512 (Pilling). Test-random tumble method); and (5) ASTM D4970 (Martindale pilling test). This list is not exhaustive and other tests may be mentioned herein. Therefore, the scope of the present disclosure is not intended to be limited to particular testing and/or quantitative data relating to particular raw or welded substrates unless otherwise indicated in the following claims.

6. Specific aspects of various welding processes and properties of the resulting weld substrate

Presented below are data for welded substrates produced using various methods and apparatus in accordance with the present disclosure. However, any of the specific examples disclosed below (eg, process parameters used in the manufacture of various weld substrates, the characteristics, dimensions, configurations, etc. of the weld substrates) are set forth in the following claims. Unless otherwise stated, it is not meant to limit the scope of the present disclosure, but for purposes of illustration.

One process for making a welded substrate uses a process solvent containing EMIm OAc and ACN and uses a 30/1 ring spun cotton yarn (“30 single yarn”, tex=19.69 (weight) knitting yarn) of the original yarn. May be configured to be applied to a substrate including. A scanning electron microscope (SEM) image of such a substrate is shown in Figure 7B, and an SEM image of the resulting welded substrate is shown in Figure 7C. Table 1.1 shows some of the key process parameters used to make the weld substrate of FIG. 7C. In this configuration, process solvent application was accomplished by pulling the substrate through a 33 inch long tube, which tube was filled with process solvent. Therefore, such an arrangement does not result in a separate process solvent application zone 2. At the end of the tube, a flexible orifice (eg, a squeegee) is in physical contact with the process wetting substrate to remove a portion of the process solvent from the outer surface of the process wetting substrate, and the process solvent. Was designed to allow proper distribution to the substrate.

A schematic diagram of the welding process is shown in FIG. 7A. The welding process can be configured to produce the welding substrate shown in FIG. 7C. The deposition process shown in FIG. 7A follows various principles and concepts for viscous drag, process solvent application, physical contact with a process wet substrate described herein with respect to FIGS. 1, 2 and 6A-6E. It may be configured. For simplicity, aspects of this deposition process for process solvent recovery zone 4, solvent collection zone 7, solvent recycle 8, mixed gas collection 9, and mixed gas recycle zone 10 are omitted. Viscosity resistance was achieved by co-optimization of process solvent composition, temperature, flexibility and size of squeegee orifice. Volume controlled consolidation of the welded substrate is achieved by controlling the linear tension applied to the process welded substrate and/or the reconstituted wet substrate during drying in its drying zone, and under controlled tension conditions. Due to the collection method of winding the welded substrate, it was limited to the reduction of the diameter of the knitting yarn. However, in the case of 2D or 3D substrates, volume controlled consolidation of the welded substrate may limit the tension on the process wetted substrate, reconstituted wetted substrate, etc. in other dimensions, which It may be necessary to control at least the first linear tension, the second linear tension, and/or the third linear tension.

Table 1.1 shows some of the main process parameters used to make the weld substrate shown in FIG. 7C using the weld process shown in FIG. 7A. Note that in Table 1.1, "weld zone time" refers to the length of time that the substrate has been in process solvent application zone 2 and process temperature/pressure zone 3. This time represents that the welding time was shortened by almost one digit as compared with the conventional technique. Of course, there are many processes in which samples have been shown to be processed for minutes to hours. However, the prior art does not disclose a partial solubilization type process capable of achieving a desired effect in such a short time. This significant reduction in deposition time was only possible by co-optimizing the chemistry of the process solvent and the hardware and control system developed to achieve the desired effect. That is, by combining chemistry with hardware to achieve proper viscous drag and controlled volume consolidation, a surprising new effect is achieved on the finished welded yarn substrate. A graph plotting stress (g) against elongation is shown in FIG. 7D for both a representative raw yarn substrate sample and a representative welded yarn substrate. The upper curve is the welded yarn base material, and the lower curve is the raw yarn.

Still referring to Table 1.1, "pull rate" refers to the linear rate at which the substrate moves through the deposition process, which affects viscous drag, and "solvent ratio" is the ratio of process solvent to substrate. Refers to the mass ratio.

Table 1.2 gives various property values of the weld substrate shown in Figure 7C (performed on about 20 unique samples of the weld yarn substrate). The characteristic values were collected by using a mechanical characteristic tester manufactured by Instron Co., Ltd. by operating in a tensile test mode similar to ASTM D2256. As used in Table 1.2, breaking strength represents the average absolute force of the welded substrate in grams. The normalized breaking strength is a value obtained by converting grams to centinewton and normalizing by the weight of the raw yarn base material (19.69 tex in this sample). The elongation rate (%) is a value obtained by dividing the displacement at which the fracture has occurred by the gauge length and multiplying by 100.

Another process for making a welded substrate may be configured to apply to a substrate containing 30/1 ring spun cotton yarn of the raw yarn using a process solvent containing EMIm OAc and ACN. A schematic diagram of such a welding process is shown in FIG. 8A. The welding process shown in FIG. 8A is based on various principles and concepts relating to viscous drag, process solvent application, physical contact with a process wet substrate, etc., described herein with respect to FIGS. 1, 2 and 6A-6E. May be configured according to. For simplification, aspects of the present welding process relating to the process solvent recovery zone 4, the solvent collection zone 7, the solvent recycle 8, the mixed gas collection 9, and the mixed gas recycle zone 10 are omitted. In this example, aspects of the apparatus for use in the welding process were specifically configured to increase the speed at which the substrate, including the substrate knitting yarn, can move through the process. Specifically, by separating the process solvent application 2 from the process temperature/pressure zone 3 using an injector 60 device similar to the device described in FIG. 6A.

Table 2.1 shows some of the key process parameters used to make the weld substrate shown in FIG. 8C using the weld process shown in FIG. 8A. The process parameters for each column heading in Table 2.1 are the same as described above for Table 1.1. In this deposition process, the temperatures of process solvent application zone 2 and process temperature/pressure zone 3 were kept at different values in order to co-optimize the desired amount of viscous drag and promote increased process solvent effectiveness. Further, by limiting the frictional force (eg, shearing) on the textile yarn substrate by achieving process solvent application with a metering pump and applying viscous drag at key points of process solvent application zone 2, Greater tension control could be achieved. This had the effect of further facilitating a volume controlled reduction of the textile yarn substrate diameter. The overall design allowed a faster total processing speed than the previous example, which is clear from a comparison of Table 1.1 and Table 2.1.

A scanning electron microscopy (SEM) image of a substrate containing a 30/1 ring spun cotton yarn raw yarn that can be used in the welding process of FIG. 8A is shown in FIG. 8B. The SEM image of the obtained welding base material is shown in FIG. 8C. Table 2.1 shows some of the key process parameters used to make the weld substrate of FIG. 8C.

Table 2.2 shows various attributes of the welded substrate shown in Figure 8C, which was manufactured using the parameters set forth in Table 2.1. The characteristics are averages carried out on about 20 unique samples of the welded yarn substrate, this characteristic being operated in a tensile test mode approximating ASTM D2256 using an Instron mechanical property tester. Collected. The mechanical properties of each column heading in Table 2.2 are the same as described above for Table 1.2. A graph plotting stress (g) against elongation is shown in FIG. 8D for both a representative raw yarn substrate sample and a representative welded yarn substrate sample. The upper curve is the welded yarn base material, and the lower curve is the raw yarn.

Another process for making a welded substrate is to use a process solvent containing EMIm OAc and ACN for application to a substrate containing 30/1 ring spun cotton yarn or 10/1 open end spun cotton yarn of the raw yarn. It may be configured. Such a process may be similar to the process schematically shown in Figure 8A. Table 3.1 shows some of the key process parameters used to produce weld substrates from substrates containing 10/1 open-ended spun cotton yarn, and Table 3.2 describes the weld processes. 2 shows various characteristics of the welded base material and the raw base material used in the parameters shown in FIG. Of course, these data exemplify the characteristics of the welding substrate that can be achieved by the welding process, and unless otherwise indicated in the following claims, the type of textile yarn substrate that can be welded and/or the welding substrate. It is not meant to limit the quality of the substrate.

Another process for making a welded substrate may be configured to apply to a substrate containing raw yarn using a process solvent containing EMIm OAc and ACN. A perspective view of various devices that may be configured to perform such a welding process is shown in FIG. 9A. The welding process and apparatus shown in FIG. 9A can be used in various methods for viscous drag, process solvent application, physical contact with process wet substrates, etc., described herein with respect to FIGS. 1, 2 and 6A-6E. It may be constructed according to the principles and concepts. For simplification, aspects of the present welding process relating to the process solvent recovery zone 4, the solvent collection zone 7, the solvent recycle 8, the mixed gas collection 9, and the mixed gas recycle zone 10 are omitted.

A scanning electron microscope (SEM) image of a substrate that can be used in the welding process and apparatus of FIG. 9A is shown in FIG. 9B, and an SEM image of the resulting welded substrate is shown in FIG. 9C. Table 3.1 shows the welding substrate shown in FIG. 9K (similar to the welding substrate shown in FIG. 9C in that it is lightly welded) using the welding process and equipment shown in FIG. 9A. Some of the main process parameters used to produce the welded substrate are shown below. The process parameters for each column heading in Table 3.1 are the same as described above for Table 1.1.

This welding process may be configured to move multiple ends of the textile yarn substrate at the same time, and virtually all weights such as process solvent flow rates, temperatures, substrate feed rates, substrate tensions, etc. Note that the process parameters can be adjusted. Specifically, the welding process and apparatus may allow co-optimization of viscous drag and controlled volume consolidation for a particular weld substrate designed for a particular product. Some of the fusing yarn substrates are shown in Figures 9C-9E and 9I-9M.

Table 3.2 shows various characteristics of the weld substrate shown in FIG. 9K, which were manufactured using the parameters set forth in Table 3.1. The characteristics are averages carried out on about 20 unique samples of the welded yarn substrate, this characteristic being operated in a tensile test mode approximating ASTM D2256 using an Instron mechanical property tester. Collected. The mechanical properties of each column heading in Table 3.2 are the same as described above for Table 1.2. The stress (g) was measured against the elongation for both the representative raw yarn base material sample and the representative welded yarn base material sample (for example, the lightly welded welded base material shown in FIGS. 9C and 9K). The plotted graph is shown in FIG. 9G. The upper curve is the welded yarn base material, and the lower curve is the raw yarn.

Table 4.1 shows the weld substrate shown in FIG. 9L using the weld process and equipment shown in FIG. 9A (which is similar to the weld substrate shown in FIG. 9D in that it is moderately welded). Some of the main process parameters used in the production of the welding base material during the production of are shown below. The process parameters for each column heading in Table 4.1 are the same as described above for Table 1.1.

This welding process may be configured to move multiple ends of the textile yarn substrate at the same time, and virtually all weights such as process solvent flow rates, temperatures, substrate feed rates, substrate tensions, etc. Note that the process parameters can be adjusted. Specifically, the welding process and apparatus may allow co-optimization of viscous drag and controlled volume consolidation for a particular weld substrate designed for a particular product.

Table 4.2 shows various characteristics of the weld substrate shown in FIG. 9L, which was manufactured using the parameters set forth in Table 4.1. The characteristics are averages carried out on about 20 unique samples of the welded yarn substrate, this characteristic being operated in a tensile test mode approximating ASTM D2256 using an Instron mechanical property tester. Collected. The mechanical properties of each column heading in Table 4.2 are the same as described above for Table 1.2.

Table 5.1 shows the welding substrate shown in FIG. 9M using the welding process and equipment shown in FIG. 9A (which is similar to the welding substrate shown in FIG. 9E in that it is firmly welded). As produced, some of the main process parameters used to make the weld substrate are shown. The process parameters for each column heading in Table 5.1 are the same as described above for Table 1.1.

This welding process may be configured to move multiple ends of the textile yarn substrate at the same time, and virtually all weights such as process solvent flow rates, temperatures, substrate feed rates, substrate tensions, etc. Note that the process parameters can be adjusted. Specifically, the welding process and apparatus may allow co-optimization of viscous drag and controlled volume consolidation for a particular weld substrate designed for a particular product.

Table 5.2 shows various attributes of the weld substrate shown in Figure 9M, which was manufactured using the parameters set forth in Table 5.1. The characteristics are averages carried out on about 20 unique samples of the welded yarn substrate, this characteristic being operated in a tensile test mode approximating ASTM D2256 using an Instron mechanical property tester. Collected. The mechanical properties of each column heading in Table 5.2 are the same as described above for Table 1.2.

The progress of the degree to which the base material is welded is shown in FIGS. 9C to 9E. In all of this, the welded substrate can be manufactured using the process and apparatus shown in Figure 9A by varying the process parameters. Specifically, the SEM data show that loose bristles on the cotton yarn are gradually eliminated, and the lightly welded substrate of FIG. 9C, the medium welded substrate of FIG. 9D, and 9E shows different degrees of controlled volume consolidation for the firmly welded substrates of FIG. 9E. All of these welded substrates were made using a substrate containing 30/1 cotton yarn. The terms "lightly," "moderately," and "tightly" are not meant to be limiting in any way, unless stated otherwise in the specification or the claims below, and are relative, qualitative. It means an embodiment.

A test fabric made from a lightly welded substrate (which may be similar to the weld substrate shown in Figure 9C or 9K) is shown in Figure 9F. The absolute quality of the fabric knitted or woven from the welded substrate can vary and can be manipulated through at least the process parameters and the degree of welding performed on the welded substrate containing the fabric. Table 6.1 shows some of the main process parameters used for manufacturing the welding base material when the welding base material used for the fabric shown in FIG. 9F was manufactured using the welding process and apparatus shown in FIG. 9A. Show. The process parameters for each column heading in Table 6.1 are the same as described above for Table 1.1.

Table 6.2 shows the use of fabric and yarn substrates containing three separate samples of lightly welded substrates such as those of Figures 9C and 9K (30/1 ring spun knit woven substrate). 9 shows various attributes of the corresponding fabrics produced. Bursting strength was measured using ASTM D3786. The column heading "burst strength" refers to the absolute burst strength in pounds per square inch, and the column heading "improved burst strength" is the welded yarn when compared to the fabric containing the base yarn base (control). Refers to the rate of improvement of the fabric containing the substrate.

In addition to increasing burst strength, fabrics such as those shown in Figure 9F may show a significant increase in fabric score when tested using the Martindale Pilling test (ASTM D4970). For example, a fabric containing a yarn base material that has a score of 1.5 or 2 in this test will have a score of 5 when the same yarn base material is treated in the welding process, even if it is moderately welded. ..

Another progression in the degree to which the substrate is welded is shown in Figures 9K-9M. In all of this, the weld substrates can be manufactured using the process and apparatus shown in FIG. 9A by varying the process parameters as described above for the tables associated with the weld processes that make each weld substrate. Specifically, the SEM data show that loose bristles on the cotton yarn are gradually eliminated, as well as the lightly welded substrate of FIG. 9K, the medium welded substrate of FIG. 9L, and FIG. 9M. 3 shows different degrees of controlled volume consolidation for the firmly welded substrates of. All of these welded substrates were made using a substrate containing 30/1 cotton yarn. 9K-9M and some mechanical properties of the knitted yarns shown in FIGS. 9I and 9J are shown in Table 7.1 and give a comparison with a base yarn substrate of the same mechanical properties. In Table 7.1, "tensile strength" refers to a weight-normalized measure of strength and is commonly used in the textile and textile industries.

Generally, an increase in strength is observed with the welded substrate compared to its raw substrate equivalent. As noted above, the fabric shown in Figure 9F has a burst strength that is about 30% greater than the burst strength of a similar control knit fabric made from a raw yarn substrate. Other improvements are also observed, such as reduced dry time (after washing), increased abrasion resistance, and improved dye brilliance, as compared to the raw substrate equivalent. This will be described in more detail below. The absolute degree to which these attributes are observed can be controlled at least by the process parameters (eg, the degree and quality of the welding process). The degree and quality of the welding process may further be correlated with at least co-optimization of process solvent application and viscous drag and controlled volume consolidation that occurs at various stages of the welding process.

Referring again to FIG. 9G, there is shown a comparison of elongation versus linear tension (in g) applied to both raw and welded substrates, which shows excellent mechanical properties. The welded substrate shown in FIG. 9C can be considered a “core-deposited” substrate, where the term “core-deposited” means that process solvent application and penetration of the welding action into the substrate is the basis. Refers to a welded substrate that is relatively uniform across the material diameter.

The welded substrates shown in FIGS. 9I and 9J can be considered as "shell welded" substrates, where the term "shell welded" is preferentially welded to the outer surface of the substrate ( That is, a welded substrate that forms a welded shell). The welded shells are distinguished from the micro-welded/non-welded cores as can be clearly seen in the central portion of the central welded substrate in FIG. 9J.

This shell welded substrate can be manufactured from a substrate containing a raw yarn of 30/1 ring spun cotton yarn using the welding process and apparatus shown in FIG. 9A. Table 8.1 shows a part of the main process parameters used for manufacturing the shell welding base material when manufacturing the welding base material shown in FIGS. 9I and 9J using the welding process and apparatus shown in FIG. 9A. Show. The process parameters for each column heading in Table 8.1 are the same as described above for Table 1.1.

This welding process may be configured to move multiple ends of the textile yarn substrate at the same time, and virtually all weights such as process solvent flow rates, temperatures, substrate feed rates, substrate tensions, etc. Note that the process parameters can be adjusted. Specifically, the welding process and apparatus may allow co-optimization of viscous drag and controlled volume consolidation for a particular weld substrate designed for a particular product.

Table 8.2 shows various characteristic values of the welding base materials shown in FIGS. 9I and 9J manufactured using the parameters described in Table 8.1. Characteristic values are averages performed on about 20 unique samples of welded yarn substrate. The characteristic values were collected by using a mechanical characteristic tester manufactured by Instron Co., Ltd. by operating in a tensile test mode similar to ASTM D2256. The mechanical properties of each column heading in Table 8.2 are the same as described above for Table 1.2.

By optimizing various process parameters (eg process solvent to substrate ratio, temperature, pressure, etc., and effectiveness of the resulting process solvent) and viscous drag, in the dimension from the outer surface of the substrate to its inner surface. It is possible to control the depth to which the substrate is deposited. That is, the welding process may be configured such that the outer regions of the substrate are preferentially welded and the substrate core is not welded to the same extent as its outer surface. This often has the effect of increasing the strength compared to the raw substrate, while retaining the elongation properties of the raw substrate, thus increasing the toughness (increasing the energy to break). Occurs. Both core-deposited and shell-deposited substrates have good properties such as faster drying, greater abrasion resistance, greater pilling resistance, brighter colors, etc., as compared to raw substrate equivalents. Can be shown.

A photograph of a piece of fabric composed of about 50% raw (raw) cotton yarn substrate and 50% medium welded textile yarn substrate is shown in FIG. 9H. The left side of the figure shows the raw cotton yarn and the right side of the figure shows the welded cotton substrate. When this fabric piece was subjected to pot dyeing processing, a stronger, richer, deeper, brighter color was exhibited on the fabric side knitted from the welded yarn base material. At least due to the co-optimized process solvent application method, viscous drag, and solvent efficiency, the welded yarn substrate and resulting fabric are less hairy. In addition, the controlled volume reduction associated with the welding, reconstitution, and drying steps of the welding process may be configured to reduce surface area and open space within the weld yarn substrate. This reduces the number of interfaces that light can scatter. The net effect of these effects is that the dye colorant is more visible through the fused substrate, making the fused substrate more transparent than the raw substrate.

The relatively low bristles and the reduction of open space in the fiber-bonded substrate also serve to surprisingly and dramatically reduce the time required to dry the fiber-bonded substrate. Again, the lack of bristles on the substrate surface and the reduction of open space in the weld substrate due to controlled volume consolidation may be configured to limit the extent to which bulk water can be integrated within the weld substrate. Good. For this reason, welded substrates are often dried more than twice as fast (with half the energy required) as the raw substrates. Finally, it is observed that the same coating and surface modification chemistries that are useful in reducing the water retention of raw cotton are even more effective with fiber-bonded cotton substrates. Similar results are observed with silk, linen, and other natural substrates.

Another process for producing a welded substrate may be configured to apply to a substrate containing 30/1 ring spun cotton yarn using a process solvent containing lithium hydroxide and urea. A perspective view of various devices that may be configured to perform such a welding process is shown in FIG. 10A. The welding process and apparatus therefor shown in FIG. 10A are various with respect to viscous drag, process solvent application, physical contact with a process wetted substrate, etc. described herein with respect to FIGS. 1, 2 and 6A-6F. May be configured according to the principles and concepts of. In this configuration, the substrate (eg, the knitting or weaving yarn in the specific configuration shown in FIG. 10A) is drawn multiple times through the grooved tray, as shown in FIG. 6B. Additional process solvent is provided to the substrate as it passes through the tray. The entire substrate welding path may be included in a temperature controlled environment (one configuration operating at -17°C to -12°C). Weld yarn substrates can generally reach optimum strength after a low temperature fusing time of 14 minutes. After this time, the process wet substrate can move to the reconstitution zone. For simplicity, aspects of this deposition process for process solvent recovery zone 4, solvent collection zone 7, solvent recycle 8, mixed gas collection 9, and mixed gas recycle zone 10 are omitted.

A scanning electron microscope (SEM) image of a substrate that may be used in the welding process and apparatus of FIG. 10A is shown in FIG. 10B, and an SEM image of the resulting welded substrate is shown in FIG. 10E. Table 9.1 shows some of the key process parameters used to make the weld substrate shown in FIG. 10E using the weld process and equipment shown in FIG. 10A. The process parameters for each column heading in Table 8.1 are the same as described above for Table 1.1. The welding process may be configured to move multiple ends of the textile yarn substrate at the same time, including virtually all heavy process parameters such as process solvent flow rate, temperature, substrate feed rate, substrate tension, etc. Can be adjusted. Specifically, the welding process and apparatus may allow co-optimization of viscous drag and controlled volume consolidation for a particular weld substrate designed for a particular product. Some of the welded yarn substrates are shown in Figures 10B-10F.

In other deposition processes configured to use process solvents that include LiOH and urea, the weight ratio of process solvent to substrate may be less than the values shown in Table 9.1. For example, in one welding process this ratio may be 0.5:1, in another welding process 1:1 and in another welding process 2:1 and in yet another welding process 3:1. Often (the welding process and the welding substrate produced thereby are discussed in detail below with respect to at least Table 10.1), it may be 4:1 for another welding process and 5:1 for yet another welding process. Good. Further, this ratio may be a non-integer value, such as 4.5:1. Therefore, the scope of the present disclosure is not limited to the specific values of this ratio unless otherwise indicated in the following claims.

Table 9.2 shows various property values for the welding process and equipment of FIG. 10A, the raw substrate shown in FIG. 10B, and the welded substrates produced using the parameters listed in Table 9.1. Characteristic values are averages performed on about 20 unique samples of welded yarn substrate. The characteristic values were collected by using a mechanical characteristic tester manufactured by Instron Co., Ltd. by operating in a tensile test mode similar to ASTM D2256. The mechanical properties of each column heading in Table 9.2 are the same as described above for Table 1.2. A graph of stress (g) versus elongation is shown in FIG. 10G for both a representative raw yarn substrate sample and a representative welded yarn substrate. The upper curve is the welded yarn base material, and the lower curve is the raw yarn.

The progress of the degree to which the base material is welded is shown in FIGS. 10C to 10E. In all of this, the welded substrate can be manufactured using the process and equipment shown in FIG. 10A by varying the process parameters. The chemistry of the process solvent used in the process and apparatus shown in FIG. 10A may be fundamentally different compared to the process and apparatus shown in FIG. 9A, and various engineering considerations may be involved. That is, the entire welding process may be operated according to similar principles and design concepts as described above for the welding process and associated apparatus shown in FIGS. 7A, 8A, and 9A.

Further, the principles and concepts described with respect to FIGS. 1 and 2 are relevant to understanding a comprehensive process design. Similar to the method described above with respect to FIGS. 9C-9E, the welding process and associated apparatus shown in FIG. 10A may be configured to control the degree of welding. The improved bristling and controlled volume consolidation progression of cotton yarn substrates when using various deposition parameters is shown in 10C-10E. All of these welded substrates were made using a substrate containing 30/1 cotton yarn. SEM data show that loose bristles on the cotton thread are gradually eliminated, as well as the lightly welded substrate of FIG. 10C, the medium welded substrate of FIG. 10D, and the firmly welded substrate of FIG. 10E. It is shown that the controlled degree of volume consolidation is different for different substrates. Again, the absolute quality of the welded fabric knitted or woven from the welded substrate can vary and can be manipulated via at least process parameters.

By properly co-optimizing various process parameters (eg, process solvent composition for effectiveness and viscosity, proper viscous drag of the process zone, temperature and time adjustments, and the like, transit speed through the drying zone). It is clear that the welding process can be controlled to achieve a similar effect, as detailed in Figures 9C-9E. These data show some of the surprising effects that can be achieved by co-optimizing the process using the concept of viscous drag and controlled volume consolidation. Put another way, these data show that co-optimized hardware, software, and chemistry can achieve the desired results, and the powerful new evidence demonstrated in this original study. It shows that it is a simple teaching.

An SEM image of the raw 2D substrate with jersey knit cotton is shown in Figure 12E and its magnified image is shown in Figure 12G. An SEM image of the same fabric after light welding is shown in FIG. 12F and its magnified image is shown in FIG. 12H. Table 10.1 shows some of the key process parameters used to make the welded 2D substrates shown in Figures 12F and 12H. The deposition process may be configured such that virtually all heavy process parameters such as process solvent flow rate, temperature, substrate feed rate, substrate tension, etc. can be adjusted. In the specific example, the welding process was carried out as a batch process in which the process solvent was uniformly applied to the raw substrate and allowed to act on the substrate for 7 minutes. In the Examples, similar results were obtained with longer or shorter deposition zone times, with longer deposition zone times generally corresponding to higher degrees of deposition and shorter deposition zone times generally It corresponds to a lower degree of welding. Water was used as the reconstitution solvent. Between the process solvent application 2, the process pressure/temperature zone 3, and the process solvent recovery zone 4, and the drying zone 5, the substrate has a controlled volume consolidation constraint and the individual yarns strongly adhere to each other. There wasn't. As a result, the welded 2D substrate retains the relatively soft hand and flexibility of the raw substrate, but has superior burst strength (about 20% greater) and Martindale pilling test compared to the raw substrate. Scores (up from 1.5 or 2 to at least 4) are shown.

The multiple process solvent chemistries are important in adding functional materials and additives to the weld substrate, and in configuring the particular weld process to produce the weld substrate exhibiting the desired attributes. It is important to note that it gives flexibility. Ionic liquid-based solvents (eg, the deposition process and apparatus shown in FIG. 9A), for example, tend to be slightly acidic, especially when the cations used are imidazolium-based. On the other hand, alkali metal urea type process solvents (eg, the deposition process and apparatus shown in FIG. 10A) are basic. It should be noted that the choice of process solvent is often described based on the suitability of the process solvent with specific additives, and the functional material is captured by the fiber welding process, as further detailed below. It is an important new teaching to be made.

7. Functional material

As noted above, in one aspect of the welding process according to the present disclosure, the substrate may be exposed to a process solvent for subsequent physical or chemical manipulation of the substrate and/or its properties. The process solvent can at least partially break the intermolecular bonds of the substrate and can cleave and mobilize (solvate) the substrate for modification. While the above examples and descriptions of functional material incorporation by the welding process refer to substrates that include natural fibers, the scope of the present disclosure is so limited unless otherwise indicated by the following claims. is not.

As noted above, one or more functional materials, chemicals, and/or components may be integrated within a weld substrate for 1D, 2D, and 3D substrates and/or weld substrates. .. In general, the incorporation of functional materials does not lead to complete modification of the biopolymer, which would otherwise be detrimental to the performance properties (physical and chemical properties) of the substrate, which would lead to new functionality. It is envisioned that (eg, magnetism, conductivity) can be imparted.

In general, the optimal integration of functional materials into the weld substrate is the optimization of viscous drag (which may be primarily associated with process solvent application zone 2 and/or process temperature/pressure zone 3) and/or volume control. It is envisioned that there may be a need for controlled consolidation, both of which are detailed above. For example, if it is desired that the functional material be evenly distributed over the surface area of the welded substrate, the viscous drag promotes a uniform distribution of the process solvent having the functional material disposed therein over the substrate. May be configured to do so. If it is desired that the functional material be concentrated at specific locations on the weld substrate, the viscous drag may be configured to promote a non-uniform distribution of such process solvent. Accordingly, a deposition process configured to integrate a functional material into a deposition substrate may be optimized according to the concepts, examples, methods, and/or apparatus described above and/or further detailed below. Good.

One aspect of the welding process according to the present disclosure includes substrates (cellulose, chitin, chitosan, collagen, hemicellulose, lignin, silk, other biopolymer components retained by hydrogen bonding and/or combinations thereof. May be swollen by a suitable process solvent capable of destroying the intermolecular force of the substrate, and further includes chemicals such as carbon powder, magnetic fine particles, and dyes, or a combination thereof. Non-limiting functional materials may be introduced prior to, concurrently with, or after application of the process solvent. In one aspect of the welding process according to the present disclosure, the fibrous biopolymer substrate, the functional material, and the process solvent (which may be an ionic liquid or "organic electrolyte", unless otherwise indicated in the claims below, are May be allowed to interact under controlled temperature (such as laser use or other directed energy heating), as well as specific atmospheric and pressure conditions. The process solvent may be removed after a predetermined amount of time. Upon drying, the resulting functional material may be bonded to the substrate and may impart additional functional properties to the welded substrate as compared to the properties of the original substrate material.

Good and permanent integration of the functional material into the fibrous material can be enabled by the welding process according to the present disclosure. The functional material may be introduced with the process solvent and/or engaged with the substrate prior to welding. Generally, in one aspect of the welding process, the natural fibers are tethered to an envelope in which the functional material can be placed, and when all or part of the open space is removed during the welding process, the functional material is removed. Can be captured. For example, in one aspect of the fusing process, the fusing process may be configured to embed the device in the center of the yarn, such as a micro-RFID chip. In another process, the functional material is placed in a material that acts as a substrate binder. For example, the welding process may be configured such that the fibers of the substrate can be coated with the dissolved substrate binder during the welding process.

In one aspect of the welding process, the process solvent is active with respect to the biopolymer in the natural substrate and is also compatible with the functional material. In one aspect, the functional material may include another biomaterial integrated with the base material, an example of such a composition being dissolved as an antimicrobial material in cellulose or as a blood coagulant in a wound dressing. It uses chitin. From the above, unless otherwise indicated in the following claims, the scope of the present disclosure is to the particular substrate, process solvent, point at which the functional material is introduced in the deposition process, and/or the method and/or method of introducing the functional material. Or it should be clear that it is not limited by the vehicle, the manner in which the functional material is retained on the weld substrate, and/or the type of functional material.

The depth of penetration of the solvent and/or the functional material into the substrate and the degree to which the substrate fibers are welded to each other are at least the amount of solvent, temperature, pressure, fiber spacing, morphology and/or grain of the functional material. Can be controlled by diameter (eg, molecule, polymer, RFID chip, etc.), residence time, other deposition process steps, substrate property (eg, water content and/or gradient) reconstitution method, and/or combinations thereof. .. After a period of time, the process solvent is removed as described above (eg, with water, reconstituted solvent, etc.) to produce a welded substrate with incorporated (captured) functional material. May also be held by a covalent bond. In addition to polymer transfer, chemical derivatization may also be performed during this process.

In one aspect of the welding process according to the present disclosure, the welding process increases the material density (eg, removes all or some of the spaces between the fibers) and the bundle of fibers as compared to the material density and surface area of the substrate. It can be configured to reduce the surface area of the finished welded substrate including, and at the same time capture the functional material in the welded substrate. In general, the extent to which the deposition process affects the amount of open space in a given substrate is manipulated using at least the same variables described above for the depth of penetration of the solvent and/or functional material. The variables may include the amount of solvent, temperature, pressure, fiber spacing, morphology and/or particle size of functional material (eg, molecule, polymer, RFID chip, etc.), residence time, and other deposition. Examples include, but are not limited to, process steps, substrate property (eg, water content and/or gradient) reconstitution methods, and/or combinations thereof. In another aspect, the deposition process may be configured to control the specific areas where the open space of a given substrate is cleared, which is described in further detail below. Again, the functional material may be added directly to the substrate (prior to deposition) with the process solvent and/or at any time before the process solvent is removed.

In one aspect of the deposition process according to the present disclosure, the deposition process uses a concept similar to that of multidimensional printing technology to enable spatial control of changes in physical and chemical properties of a substrate. It may be configured. The process solution is added to the substrate, for example by heating in a device similar to an inkjet printer, or by heating a selected portion of the substrate with a directed energy beam (eg, an infrared laser or other means known in the art). By activating the welding of the selected portion. Such a welding process is described in further detail below with respect to FIGS. 11A-11E for modulation welding processes.

In one aspect of the deposition process, the amount of process solvent relative to the amount of substrate may be kept relatively low to limit the extent to which the substrate is modified during the deposition process. As noted above, the process solvent may be provided by a second solvent system (eg, a reconstitution solvent), by evaporation if the process solvent is sufficiently volatile, or any other suitable method and/or apparatus. May be removed by any of, and is not limited, unless so indicated in the following claims. The deposition process may be configured to increase the evaporation rate of the process solvent by placing the process wet substrate under vacuum and/or heat treating.

The deposition process exhibits functions (eg, physical and/or chemical properties) not observed in the individual substrates and/or components that make up the substrate when viewed separately prior to the deposition process. It may be configured to produce a welded substrate that may comprise a "natural fiber functional composite" or a "fiber-matrix composite."

The welding process is a welding substrate comprising a fiber-matrix composite containing a functional material by using a process solvent comprising an ionic liquid-based solvent (“IL-based solvent”), as described in further detail below. May be configured to manufacture. One or more molecular additives in the process solvent increase the effectiveness of the process solvent as a swelling agent and mobilizer, and/or enhance the interaction of the process solvent with one or more functional materials. , And/or may enhance the uptake of process solvents and/or functional materials into natural fiber substrates. The IL-based process solvent is generally removed from the welded substrate (which may make up the fiber-matrix composite) by the reconstitution solvent, which generally rinses/washes the process wet substrate with the reconstitution solvent. In addition, the reconstitution solvent may include an excess of molecular solvent. It may be achieved by drying (sublimation, evaporation, boiling evaporation, or other reconstituted solvent removal method, or by any other suitable method and/or apparatus, as such in the following claims. Unless otherwise indicated), the welded substrate may constitute a functional material fiber-matrix composite with finished and associated novel physical and chemical characteristics.

The substrate may include natural fibers, which may include cellulose, lignocellulose, proteins and/or combinations thereof. The cellulose may include cotton, purified cellulose (kraft pulp, etc.), microcrystalline cellulose, etc. In one aspect of the welding process, the welding process and associated apparatus may be configured for use with substrates that include cellulose in the form of cotton or a combination thereof. Lignocellulosic-containing substrates include bast fibers from flax, industrial cannabis, and combinations thereof. Examples of the protein-containing base material include silk and keratin. In general, the term "natural fiber" as used herein is meant to include any high aspect ratio fiber-containing natural material produced by living organisms and/or enzymes. In general, the use of the term "fiber" refers to the macroscopic (large-scale) aspect of the material. Other examples of natural fibers include, but are not limited to, flax, silk, wool and the like. In one aspect of the welded substrate that may be produced in accordance with the present disclosure, natural fibers may generally reinforce the fiber component of the fiber-matrix composite. Thus, natural fibers may be used in formats such as non-woven mats, yarns, and/or fabrics.

Natural fibers typically include predominantly biopolymers, and there are biopolymer-containing materials that are generally not considered natural fibers. For example, the crab shell is predominantly chitin, a biopolymer containing N-acetylglucosamine monomers (a derivative of glucose), but is not commonly referred to as fibrous. Similarly, collagen and elastin are examples of protein biopolymers that provide structural support within many tissues that are not generally considered fibrous.

Natural fibers produced by plants are generally a mixture of different biopolymers (cellulose, hemicellulose, and/or lignin). Cellulose and hemicellulose have monomer units that are sugars. Lignin has a crosslinked phenolic monomer. Due to crosslinking, lignin generally cannot be solubilized (eg, swelled or mobilized) by IL-based solvents. However, natural fibers containing significant amounts of lignin function as structural support fibers in the composite. Moreover, natural fiber substrates containing significant amounts of lignin may be swollen or mobilized using process solvents that are not IL-based.

Natural fiber produced by animals often contains protein biopolymers. The monomeric units of proteins are amino acids. For example, there are many unique silk fibroin proteins that form silk. Wool, horns, and feathers mainly contain structural proteins classified as keratin. Natural fibers include cellulose, lignolsulose, proteins and/or combinations thereof. Generally, "natural fibers" include, but are not limited to, cellulose, chitin, chitosan, collagen, hemicellulose, lignin, silk, and/or combinations thereof, unless so indicated in the following claims.

In one aspect of the welding process of the present disclosure, the welding process may be configured to combine a substrate comprising natural fibers and a functional material into a welding substrate that is a continuous fiber-matrix composite. .. One purpose of the welding process is to combine a substrate comprising natural fibers and a functional material to form a natural fiber functional composite (herein "continuous fiber-matrix composite" or simply (Also referred to as “fiber-matrix composite”). Typically, the functional material is entrapped within the matrix portion of the fiber-matrix composite. The welding process may be configured so that the natural fibers make up the majority of the fiber portion of the welded substrate fiber-matrix composite, and typically function as the essential reinforcing agent.

A. Ionic liquid process solvent welding process

As mentioned above, the deposition process may be configured to use a process solvent that includes an ionic liquid. As used herein, the term "ionic liquid" is used to refer to a relatively pure ionic liquid (eg, a "pure process solvent" as defined above), and refers to an "ionic liquid system". A “solvent” (“IL-based solvent”) generally refers to a liquid that contains both anions and cations, and may be a molecular (eg, water, alcohol, acetonitrile, etc.) species, etc. In some cases, the molecular substrate can be solubilized, mobilized, swelled, and/or stabilized. Ionic liquids are attractive solvents because they are non-volatile, non-flammable, have high thermal stability, are relatively inexpensive to produce, and are environmentally friendly, making them more controllable and flexible throughout the processing process. Can be used for

US Pat. No. 7,671,178 includes examples of suitable ionic liquid solvents that can be used in various deposition processes according to this disclosure. In one deposition process, the deposition process may be configured to use an ionic liquid solvent having a melting point of less than about 200°C, 150°C, or 100°C. In one deposition process, the deposition process may be configured to use an ionic liquid solvent that includes imidazolium-based cations with acetate and/or chloride anions. In another aspect of the deposition process, the anions may include chaotropic anions such as acetate, formate, chloride, bromide, alone or in combination.

In another aspect of the deposition process, the deposition process uses a polar aprotic solvent such as acetonitrile, tetrahydrofuran (THF), ethyl acetate (EtOAc), acetone, dimethylformamide (DMF), dimethylsulfoxide (DMSO) as a molecular additive. It may be configured to use an IL-based solvent that may be included. More generally, a molecular additive for an IL-based process solvent system is even a polar aprotic solvent having a relatively low boiling point (eg, below 80° C. at atmospheric pressure) and a relatively high vapor pressure. Good. In one aspect, the IL-based solvent may be about 0.25 mol to about 4 mol of polar aprotic solvent per mol of ionic liquid. In another aspect, the polar aprotic solvent may be added to the IL-based solvent in the range of about 0.25 mol to about 2 mol of total polar aprotic solvent per mol of ionic liquid. The polar protic solvent (eg, water, methanol, ethanol, isopropanol) is typically present in the range of less than 1 mol of all polar protic solvent to 1 mol of IL-based solvent. In another aspect, the IL-based solvent may include about 0.25 to about 2 mol of polar aprotic solvent per mol of ionic liquid.

In one aspect of the deposition process configured for use with an IL-based solvent as the process solvent, the amount of IL-based process solvent added is from about 0.25 to about 4 parts by weight per part by weight of substrate. May be

In one aspect, the deposition process may be configured to use an IL-based solvent that comprises one or more polar protic solvents, such as water, methanol, ethanol, isopropanol and/or these. However, the present invention is not limited to these. In one aspect, less than about 1 mol of polar protic solvent may be combined with up to about 1 mol of ionic liquid. The deposition process may be configured to use an IL-based solvent that includes one or more polar aprotic solvents, which may constitute molecular additives to the process solvent system, and polar aprotic solvents. Include, but are not limited to, acetonitrile, acetone, and ethyl acetate. The reason for adding the molecular additive to the IL-based process solvent is to control the effectiveness of the process solvent as a swelling and mobilizing agent, and/or to enhance the interaction between the process solvent and the potency material, and/or the process. Examples include enhanced introduction of solvents and functional materials into the substrate. Such molecular additives include, but are not limited to, low boiling solvents that can control both the effectiveness of the IL as well as the rheological properties of the process solvent. That is, the molecular additives and their relative amounts may be selected to provide at least the desired viscous drag and controlled volume consolidation.

In general, the molecular component alone is a non-solvent for most of the relevant biopolymer materials. In one aspect of the deposition process, partial dissolution of the biopolymer or synthetic polymeric material is only at the proper concentration of about 1 mol of ionic liquid (ion) for up to about 4 mol of molecular constituents. Can be done. Molecular components may reduce the overall ability of ionic liquid ions to solubilize, mobilize, and/or swell polymers in a substrate, or increase the overall effectiveness of IL-based process solvents, This depends at least on the hydrogen bond donating and accepting capacities of the molecular components.

The polymers present in biopolymer substrates as well as in many synthetic polymer substrates are generally organized by intermolecular forces and intramolecular hydrogen bonds and organized at the molecular level. If the molecular constituents reduce the effectiveness of the IL-based process solvent, these molecular constituents may slow down the deposition process and/or have special properties not possible with other methods using pure ionic liquids. It can be useful in enabling spatial and temporal control. In one aspect of the deposition process, if the molecular components increase the IL-based process solvent effectiveness, these molecular components increase the speed of the deposition process and/or when using pure ionic liquids. It can be useful in allowing special spatial and temporal controls that are not possible. In addition, in another aspect, the molecular components can significantly reduce the overall cost of the deposition process, especially the costs associated with process solvents. Acetonitrile is less expensive than, for example, 3-ethyl-1-methylimidazolium acetate. Thus, in addition to allowing operation of the deposition process for a given substrate, acetonitrile can also reduce the cost of process solvent per unit volume (or mass) used.

A relatively large amount of IL-based process solvent is a substrate that is primarily composed of natural fibers (for reference, "large amount" as used herein means about 10 parts by weight per 1 part by weight of substrate). Biopolymer in the substrate can be completely dissolved when it is introduced for a sufficient time and at a suitable temperature. In the context of the present invention, complete dissolution refers to the disruption of intermolecular forces that may be necessary to preserve the native structure, features, and/or properties within the substrate (eg, breaking of hydrogen bonds due to the action of solvents). And/or indicate destruction of intramolecular forces. Generally speaking, for many deposition processes according to the present disclosure, it is believed to be advantageous to configure the deposition process without complete dissolution of most biopolymers. Specifically, complete dissolution often degrades natural fiber reinforcement by irreversibly modifying the embodied natural biopolymer structure. However, in certain aspects of the welding process, such as when using a biopolymer as the functional material, it may be advantageous to completely dissolve the biopolymer material. In a welding process so configured, the amount of completely dissolved polymer (functional material) used may typically be less than 1% by weight, based on the weight of the IL-based process solvent used. .. Given the relatively small amount of IL-based process solvent added to natural fibers, any fully dissolved biopolymer material can be a minor component of the resulting welded substrate.

When the native structure is lost, the natural material can lose its physical and chemical properties in its native state. Accordingly, the deposition process may be configured to limit the amount of IL-based process solvent added to substrates containing natural fibers. Limiting the amount of process solvent introduced into the substrate, in turn, may limit the extent to which the biopolymer is modified from its native structure, and thus the substrate's native function and/or characteristics. (Eg strength) can be preserved.

Surprisingly, the welding process according to the present disclosure facilitates the production of a welded substrate with a functional structure, including fibrous sutures, woven materials, fibrous mats, and/or combinations thereof, to which functional materials have been added. It can be manufactured by controlled fusion/welding. The physical and chemical properties of the weld substrate are at least the amount of IL-based process solvent applied, the duration of exposure to the IL-based process solvent, the temperature, the temperature and pressure applied during processing, and/or these. It can be operated reproducibly by strict control of the combination of One or more substrates and/or functional materials may be deposited to form a laminated structure with appropriate control of process variables. The surface of these substrates and/or functional materials may be modified, preferably leaving some of the substrates and/or functional materials in their unmodified state. Surface modification includes, but is not limited to, direct manipulation of material surface chemistry or indirect manipulation by the incorporation of additional functional materials to impart desired physical or chemical properties. .. Functional materials include, but are not limited to, drugs and dye molecules that are compatible with one or more substrates, nanomaterials, magnetic particles, and the like.

The functional material may be suspended, dissolved in an IL-based solvent, or a combination thereof. Examples of the functional material include, but are not limited to, conductive carbon and activated carbon, and there is no limitation unless otherwise indicated in the following claims. Activated carbon includes, but is not limited to, charcoal, graphene, nanotubes and the like, without limitation unless otherwise indicated in the following claims. In one aspect, the deposition process may be configured for use with functional materials that may include magnetic materials such as NdFeB, SmCo, iron oxide, etc., without limitation unless so indicated in the following claims.

In one aspect of the deposition process disclosed herein, the deposition process may be configured for use with functional materials that may include quantum dots and/or other nanomaterials. In another configuration of the deposition process, the functional material may include a mineral precipitate such as, but not limited to, clay. In yet another configuration of the welding process, the functional material may include a dye, which includes, but is not limited to, UV-visible light absorbing dyes, fluorescent dyes, phosphorescent dyes, and the like. There is no limitation unless so stated in the claims. In yet another configuration of the deposition process according to the present disclosure, the deposition process comprises a drug, a selected synthetic polymer (eg, meta-aramid, also known as Nomex®), quantum dots, various allotropes of carbon (eg, nanotubes). , Activated carbon, graphene and graphene-like materials), as well as natural materials (eg, crab shell, horns, etc.) and derivatives of natural materials (eg, chitosan, microcrystalline cellulose). , Rubber), and/or combinations thereof, without limitation unless so indicated in the following claims.

In one aspect, the welding process may be configured for use with functional materials including polymers. With such a configuration, it is envisioned that selecting a polymer that is not a cross-linked polymer may be advantageous in achieving the desired functional properties. However, the scope of the present disclosure is not so limited unless indicated by the following claims. In one such configuration of the welding process, the polymer may include natural polymers or proteins, cellulosic starch, silk, keratin and the like. In one aspect of the deposition process, the polymer that comprises the functional material may be less than about 1% by weight of the IL-based process solvent. In addition, various natural materials may be used as the functional material.

As mentioned above, the welding process may be configured such that one or more functional materials are predispersed with the natural fibers of the substrate, which substrate is a non-woven mat and paper, knitting yarn, woven yarn, woven fabric. It may be in the form of a cloth or the like and is not limited unless the following claims so indicate. Alternatively, the functional material may be dissolved and/or suspended in the IL-based process solvent prior to applying the IL-based process solvent to the natural fiber substrate. Upon swelling and mobilization of the biopolymer in the natural fiber matrix, the functional material may become entrapped within the matrix of the resulting weld matrix, which may constitute the fiber-matrix composite.

Optimum values for the various process parameters are expected to vary from welding process to welding process, including at least the desired properties of the welding substrate, the substrate selected, the process solvent, the functional material, the substrate in the process solvent application zone 2 and Depending on the time in process temperature/pressure zone 3, and/or a combination thereof. It is envisioned that in one deposition process, the optimum temperature of the process solvent (and consequently the temperature of the process temperature/pressure zone 3) can be from about 0°C to about 100°C.

The welding process may comprise IL-based process solvent and substrate for about 1 second to about 1 hour, or the substrate is at least 1.5% saturated, 2%-5% saturated, at least 10% saturated with IL-based process solvent. It may be configured to include a combining step until the above. Such a deposition process may be configured such that the functional material is mixed with the substrate at the same time as or after the IL-based process solvent is combined with the substrate.

After sufficient exposure to the IL-based process solvent and the functional material, a portion of the IL-based process solvent may subsequently be removed from the process wet substrate. In one aspect, the deposition process is performed by rinsing a portion of the IL-based process solvent with water, methanol, ethanol, isopropanol, acetonitrile, tetrahydrofuran (THF), ethyl acetate (EtOAc), acetone, dimethylformamide (DMF). Alternatively, it may be configured to be removed by any other method and/or apparatus suitable for the particular welding process, without limitation unless so indicated in the following claims.

In one aspect, the deposition process may be configured to entrap the functional material in the natural fibrous substrate by partially dissolving either the biopolymer or the synthetic polymer with the IL-based process solvent. Good. In one configuration of the deposition process, the deposition process may be configured to use an IL-based process solvent containing cations and anions and having a melting point of less than 150° C., the IL-based process solvent as described above. May include a molecular component. However, the scope of the present disclosure is not so limited unless indicated by the following claims. The welding process may be configured to form an ionic bond between the natural fibers of the substrate and the functional material.

In one aspect of a welding process configured in accordance with the present disclosure, one or more functional materials are incorporated into the fibrous substrate prior to introducing the IL-based process solvent for partial dissolution of the fibrous substrate. May be. In another aspect, the functional material may be dispersed in an IL-based solvent for partial dissolution of the fibrous substrate. In another aspect, one or more functional materials may be dispersed in the IL-based solvent. In yet another aspect of the welding process, the welding process may be configured to use heat to activate the partial dissolution of the natural fiber substrate and/or the functional material. In another aspect of the welding process, the partially dissolved functional material may be a biopolymer and/or a synthetic polymer.

In one aspect of the welding process, the welding process may be configured to produce a functional composite of natural fibers by using a natural fiber substrate, an IL-based solvent, and a functional material. First, the natural fiber substrate may be mixed with the IL-based process solvent, and this mixing may continue until the natural fibers are properly swollen. The functional material may then be added to the swollen natural fiber substrate and IL-based process solvent mixture. In one aspect of the welding process, the welding process may be configured to apply pressure and temperature to the mixture over a period of time. Next, at least the pressure and at least a part of the IL-based process solvent are removed to obtain a completed welded base material composed of one, two, or three dimensions as a natural fiber functional composite material. Good.

In one aspect of the welding process, the welding process may be configured to use less than 4 parts by weight of process solvent per 1 part by weight of substrate, the weight ratio being only the outer sheath of the substrate's natural fibers. It may be sufficient to break hydrogen bonds. The degree to which hydrogen bonds are broken and the native structure is modified can depend at least on the process solvent composition, as well as the length of time the natural fiber substrate is exposed to the IL-based process solvent, temperature, and pressure conditions.

The extent to which swelling and mobilization of biopolymers occurs can be qualitatively assessed, and in some cases, at least by X-ray diffraction, infrared spectroscopy, confocal fluorescence microscopy, scanning electron microscopy, and other analytical methods. It can be evaluated quantitatively. In one aspect of the welding process, the welding process controls certain variables to limit the amount of conversion of cellulose I to II that occurs at least as further detailed below with respect to FIGS. 15A and 15B. May be configured as follows. This transformation can be important as long as it demonstrates the formation of a fiber-matrix composite in the welded substrate, in which the natural fiber retains part of its original structure, and thus the corresponding It retains its original chemical and physical properties. Substrate fiber swelling is typically observed along the width rather than the length, and in one aspect of the welding process, the welding process reduces the natural fiber diameter by about 5%, 10%, or even It may be configured to increase by more than 25%.

Mobilization of the outermost biopolymer in substrates containing natural fibers can generally be considered a feature of the welding process according to the present disclosure. The mobilized polymer may be swollen so that the functional material can be inserted and entrapped within the matrix of the fiber-matrix composite in the resulting welded substrate. IL-based process solvents contain relatively large amounts of lignin (generally greater than 10% lignin) as it is believed that the main mechanism of action is to swell and mobilize biopolymers by breaking hydrogen bonds. Natural fiber substrates are generally not suitable for swelling and mobilization in IL-based process solvents. Although these lignocellulosic natural fibers (eg, wood fibers) can be incorporated as relatively inert fiber reinforcements, lignocellulosic fibers containing greater than about 10% lignin are common in cellulose or hemicellulose matrices. Do not provide. This is at least in part because the cellulose and hemicellulose biopolymers, which would otherwise be swollen and mobilized by the IL-based process solvent, are essentially immobilized within the cross-linked lignin biopolymer. is there. As used herein, the term "mobilized" means that the functional material migrates from the outer surface of the base fiber into abutment while leaving the material within the base fiber core in an unmodified state. It includes the action of assimilation with the functional material from the base fiber. Upon swelling and mobilization of the biopolymer and entrapment of the functional material, the IL-based process solvent is generally removed from the freshly formed fiber-matrix composite welded substrate and recycled.

As used herein, the term "reconstitution" is used to refer to the process in which process solvent is rinsed/washed out of the process wet substrate. This is typically done by flowing excess molecular solvent (eg, water, acetonitrile, methanol) around and into the process-wetting substrate or by dipping the process-wetting substrate in a bath of molecular solvent. It is achieved by The choice of reconstitution solvent depends on factors such as the type of biopolymer contained in the substrate, and the composition of the process solvent and the ease with which the process solvent can be recovered and purified for reuse.

After removal of the process solvent, the reconstituted solvent is typically removed. This can typically be accomplished by any combination of sublimation, evaporation, or boiling. Depending on the natural fiber substrate, the choice of functional material, and whether the substrate is physically constrained during all or part of the welding process, the substrate undergoes significant dimensional (dimensional) changes. There is. For example, the diameter of a knitting yarn can be reduced by up to one-half, because the open spaces between the individual natural fibers are integrated into the continuous fiber-matrix composite in the welded substrate.

In aspects of the welding process, the welding process may be configured such that a portion of the natural fibers in the substrate, including the natural fibers, swell from about 2% to about 6% in diameter. More specifically, in one aspect of the welding process, a portion of such natural fibers may be swollen by more than about 3% in diameter.

In one aspect of the welding process, the mixture may be about 90% by weight natural fiber substrate and functional material and about 10% by weight IL-based process solvent. Alternatively, the amount of the IL-based process solvent added to the base material and/or the mixture of the base material and the functional material is about 0.25 part by weight to about 4 parts by weight of the process solvent per 1 part by weight of natural fiber. It may be.

In one aspect of the welding process, the welding process may be configured such that the pressure in the process temperature/pressure zone 3 can be approximately a vacuum. Alternatively, the welding process may be configured such that the process temperature/pressure zone 3 pressure is about 1 atmosphere. In yet another configuration, the process temperature/pressure zone 3 pressure may be from about 1 atmosphere to about 10 atmospheres. As mentioned above, the temperature and/or time that the substrate is exposed to the process solvent may also be controlled.

In one aspect of the welding process, the welding process may include providing a substrate comprising a plurality of natural fibers, providing an IL-based process solvent, and providing at least one functional material. The welding process so configured comprises the steps of mixing the substrate, the IL-based process solvent and the functional material in a predetermined order to cause a chemical reaction to produce the welded substrate that constitutes the natural fiber functional composite. In the natural fiber-functional composite material, the functional material may penetrate into the natural fiber, and the plurality of natural fibers and the functional material may be covalently bonded. In one aspect of the welding process, at least the temperature, pressure and time of the chemical reaction may be controlled. It is contemplated that the deposition process may be configured to remove a portion of the process solvent, and in certain applications it may be advantageous to remove a majority, or substantially all, of the process solvent. R.

In one aspect of the welding process, the welding process is configured such that the functional material is introduced after the natural fiber substrate is mixed with the process solvent and the natural fiber substrate achieves swelling according to a predetermined process sequence. May be done. In one aspect of such a deposition process, the IL-based process solvent may be diluted with a molecular solvent component, where the partial dissolution process of the biopolymer or synthetic polymeric material begins after the removal of the molecular solvent component (such Removal may be carried out by any suitable method and/or apparatus, which is not limited unless so indicated in the claims below, examples include but are not limited to evaporation or distillation).

In one deposition process, a carbon-cotton-process solvent mixture is used to provide a thin coating of carbon/cotton bond to a carbon-cotton bond when the cotton fabric is exposed to a solution containing the process solvent. The material may be made.

In one aspect of the welding process, the process solvent and the natural fiber substrate are blended to transfer the functional material (eg, conductive carbon) into the natural fiber substrate and/or a thin coating of the carbon functional material. Can produce surface tension properties that allow it to be formed on natural fiber substrates such as cotton. The following examples describe welding substrates and/or welding processes in which functionalization is achieved. The following examples are not intended to be read in a limiting sense, but rather as an exemplification of the broader concepts and welding processes disclosed herein.

B. Functional material capture

The following example illustrates a deposition process in which one or more functional materials can be entrapped in a substrate that includes a natural fibrous material and an IL-based process solvent introduced after the functional material is incorporated into the substrate. Detailed description. Again, the following examples do not limit the scope of this disclosure in any way, unless so indicated in the following claims. In one embodiment of the invention, trapping involves incorporating the functional material into the fibrous substrate prior to introducing the ionic liquid-based solvent.

FIG. 3 illustrates a process for the addition and physical entrapment of a solid material within a fiber-matrix composite with the sub-processes or components of FIG. 3 labeled FIGS. 3A-3E. As shown in FIG. 3A, the natural fiber substrate 10 may include a certain amount of empty space. As shown in FIG. 3B, the dispensed functional material 20 may be incorporated into the natural fiber substrate 10. The time after the IL-based process solvent 30 has been introduced into the natural fiber substrate 10 and the functional material 20 (to form the process wet substrate) is shown in FIG. 3C. The controlled pressure, temperature, and time may then be used to make the swollen natural fiber substrate 11 (shown in FIG. 3D) with the dispersed and bonded functional material 21.

In one aspect of the welding process, all or part of the IL-based process solvent 30 is then removed from the bonded functional material 21 and swollen natural fiber substrate 11 to provide the functional properties of the plurality of natural fiber substrates 10. And maintaining the functional properties of the plurality of functional materials 20 while at the same time producing a welded fiber 40 having entrapped functional material 22. Unless otherwise specified, any of the features, characteristics and/or properties described herein with respect to the weld fibers 40, 42 can be extended to fabrics, fabrics, and/or other articles containing the weld fibers 40, 42.

In one aspect of the fusing process, fusing fiber 40 may be a combination of covalently bonded functional material 21 and swollen natural fiber substrate 11. In one aspect of the fusing process, the fusing process is configured such that the resulting fusing substrate comprises a cotton cloth functionalized with entrapped magnetic (NdFeB) particulates, as observed in scanning electron microscopy data. May be. In one aspect of the welding process, the welding process may be configured for a functional material 20 that includes demagnetized particulates that may be incorporated as a dry powder into a natural fiber substrate 10 that includes a fabric material. Surprisingly, the welding process was observed to be able to trap the particles within the biopolymer of the natural fiber substrate 10, which causes the magnetic particles to be strongly retained within the welded fibers 40 and removed even with vigorous washing. Not done. In one aspect of the welding process, the welding process is similar to that described above, with similar advantages, and/or weaving yarns and non-woven fibrous matte natural fiber substrates 10 (cotton and silk). (Including a weaving yarn matrix).

As mentioned above, the deposition process described in the immediately preceding example was performed by exposing the suspension of nanomaterial functional material 20 to biopolymer natural before exposing the functional material or natural fiber substrate 10 to the IL-based process solvent. It may be configured to be added to the fiber base material 10. Depending on at least the surface chemistry of the functional material 20, which may include quantum dots, different molecular solutions such as aqueous or organic (eg toluene) may be used alone or with the IL-based process solvent 30. .. The surface chemistry (ie, hydrophobic/hydrophilic) of the nanomaterial functional material 20 is strong with the natural fiber substrate 10 as well as the final location and dispersion of the nanomaterial functional material 20 within the resulting weld fiber 40. Can affect.

Surface chemistry may be used as a strategy for natural fiber substrate 10 and functional material 20 to self-assemble with IL-based process solvents to create functional microfabrication within the composite. For example, in one aspect of the deposition process, the quantum dots may include a semiconductor material that has size dependent properties. The surface can be functionalized to accommodate different chemical environments for use in pharmaceutical, sensing, and information strategy applications, without limitation unless so indicated in the following claims.

C. Capture of functional material from process solvent/functional material mixture

FIG. 4 describes the process for the addition and physical entrapment of the solid material within the fiber-matrix composite, with the material (pre-)dispersed in the IL-based solvent and labeled as FIGS. 4 is shown with the sub-process or components of FIG. FIG. 4A shows that the initial natural fiber substrate 10 creates a process solvent/functional material mixture 32 with an IL-based process solvent 30 having dispersed functional material 20 therein. As shown in FIG. 4A, prior to the introduction of the natural fibers 12, the functional material 20 may be pre-placed in the IL-based process solvent 30 to form a process solvent/functional material mixture 32.

The natural fiber substrate 10 and process solvent/functional material mixture 32 may then be combined (to produce a process wet substrate) as shown in Figure 4B. At a minimum, controlled pressure, temperature, and/or time may be used to form the swollen natural fiber substrate 112 within the process solvent/functional material mixture 32, as shown in FIG. 4C. In one aspect of the welding process, the welding process then removes all or a portion of the IL-based process solvent 30 from the swollen natural fiber substrate 112 to remove the plurality of natural fiber substrates 10 as shown in FIG. 4D. It may be configured to maintain the functional properties and the functional properties of the plurality of functional materials 20 while at the same time producing a weld fiber 42 having the entrapped functional material 22.

In one aspect of the fusing process, fusing fiber 42 may be a combination of covalently bonded functional material 20 and swollen natural fiber substrate 112. In one aspect of the fusing process, the fusing process is such that the resulting fusing substrate comprises a functional material 20 comprising a molecular dye entrapped within a natural fibrous substrate 10 comprising cotton paper (fibrous mat). The functional material 20 may be configured and dispersed in the IL-based process solvent 30 (to form the process solvent/functional material mixture 32) prior to application to the natural fiber substrate 10. During the welding process, the biopolymer (eg, cellulose in natural fiber substrate 10 including cotton paper) is swollen and the dye-containing functional material 20 is physically diffused and covalently bound within the polymer matrix. May be captured by. After the deposition process, the dye can clearly remain entrapped within the polymer matrix.

In one aspect of the welding process, the welding process may also be configured to controllably fuse certain information and/or chemical functions to the natural fiber substrate 10 in the resulting weld fibers 40, 42. Good. Such fusing fibers 40, 42 have potential applications in at least banknote counterfeiting, garment dyeing (dye fastness), drug delivery devices, and other related technologies. In one aspect of the welding process, the welding process is for use with a functional material 20 that may include a molecular or ionic species that can be dispersed in an IL-based process solvent 30 for incorporation into the natural fiber substrate 10. It may be configured.

In general, the purpose of adding the functional material 20 can be application specific. For example, dyes that have a coupling chemistry that covalently bonds to cellulose can be relatively expensive. In one aspect of the fusing process, the fusing process may be configured to capture low cost alternative dyes within the fusing fibers 40, 42 that do not have special binding chemistries. Functional materials 20 containing one or more dyes entrapped within what was once a swollen and mobilized biopolymer (eg, swollen natural fiber substrates 11, 112) are not easily washed away and at least are woven. And/or may be applicable for barcoded/information storage applications. In other aspects, the electrically conductive functional material 20 can be entrapped within the weld fibers 40, 42 for energy storage applications. The capture of the functional material 20, including magnetic material, may be associated with fabric-based actuators. The entrapment of pharmaceuticals and/or functional materials 20 containing quantum dots may be relevant for medical applications. The capture of the functional material 20 containing clay is associated with flame retardancy enhancement. The addition of biopolymer chitin as functional material 20 may find use due to its known antibacterial properties. In short, the number of possible uses is quite large. The functional material 20 is an organic and/or inorganic material having electron, spectral, thermal conductivity, magnetic, antibacterial and/or antimicrobial properties (for example, chitin, chitosan, silver nanoparticles, etc.), and/or these Suitable clays to act on the combination include, but are not limited to, all carbon allotropes, NdFeB, titanium dioxide, combinations thereof, and the like. Therefore, unless otherwise indicated in the following claims, the scope of the present disclosure is not intended to be limited in any way to the particular application of particular functional material 20 and/or the resulting weld substrate and/or fibers 40, 42. Absent.

In one aspect of the welding process, the welding process does not require special covalent chemistry to ensure entrapment of the associated functional material 20, rather the functional material 20 is physically contained within the weld fibers 40, 42. May be configured to be captured. In one aspect of the fusing process, the functional material 20 may be incorporated with high spatial control for information coding or for making robust dyes, and more generally for integrating device functionality. .. Multi-dimensional printing and manufacturing techniques allow for the layering of many types of functions in a single material or object.

D. Capture of functional material from process solvent/functional material/polymer mixture

As can be seen in FIG. 5, which further illustrates various sub-processes and components in FIGS. 5A-5D, in one aspect, the deposition process operates on a mixture of IL-based process solvent and a solvent that also contains additional solubilizing polymer. The functional material 20 may be configured to be incorporated into the natural fiber substrate 10 by introducing the functional material 20.

As shown in FIG. 5A, such a process may begin with the IL-based process solvent 30 mixed with the natural fiber substrate 10 and the functional material 20, the functional material 20 being dispersed in the IL-based process solvent 30. To form the process solvent/functional material mixture 32. The polymer 53 may be included in the process solvent/functional material mixture 32 such that the polymer 53 is dissolved and/or suspended in the process solvent functional material mixture 32. See also FIG. 5, which illustrates a process for loading and physically entrapping solid material in a fiber matrix composite. The sub-processes or components of Figure 5 are shown as Figures 5A-5D. Process solvent/functional material mixture 32 mixed with polymer 53 prior to application to natural fiber substrate 10 is shown in FIG. 5A. The process solvent/functional material mixture 32 having the polymer 53 therein may then be introduced into the natural fiber substrate 10 to form a process wet substrate, as shown in FIG. 5B. The deposition process involves controlled pressure, temperature, and time to swell the combined process solvent/functional material mixture 32, polymer 53, and natural fiber substrate 10 into the natural fiber substrate 10, as shown in FIG. 5C. It may be configured to form 11, 112.

In one aspect of the deposition process, all or part of the IL-based process solvent 30 is then processed into a wet substrate (which may include bonded functional material 21 and swollen natural fiber substrate 11, 112). And retains the functional properties of the plurality of natural fiber substrates 10 and the plurality of functional materials 20 while having the entrapped functional material 22 and polymer 53, as shown in FIG. 5D. The fused fiber 40 is produced.

In one aspect of the fusing process, fusing fiber 40 may be a combination of covalently bonded functional material 21, polymer 53, and swollen natural fiber substrate 11. The polymer may include biopolymers and/or synthetic polymers. In a welding process configured for use with a particular polymer 53, the additional polymer may act both as a binder (eg, glue) as well as a rheology modifier to alter the solution viscosity. Moreover, such a welding process may allow for additional spatial control over the final location of the functional material 20 within the welding substrate. In one aspect of the welding process, the welding process may be configured for use with the functional material 20 including a carbon material, and the natural fiber substrate 10 may include cotton yarn to produce the weld fibers 40, 42. The fibers have been tested and have been shown to be suitable for use as electrodes for high energy density supercapacitors in woven fabrics. This can be adapted to provide a flexible and wearable energy storage device.

The deposition process may include one or more conductive additions such as organic materials (eg carbon nanotubes, graphene, etc.) or inorganic materials (silver nanoparticles, stainless steel, nickel, fibers coated with metal and metal oxides, etc.). The functional material 20 containing the agent may be used to fabricate the welded fibers 40, 42. Such weld fibers 40, 42 may exhibit enhanced conductivity and, when combined with a suitable electrolyte (eg, gel, polymer electrolyte, etc.), these weld fibers 40, 42 (and/or therefrom). The manufactured fabrics and/or textiles) may be capable of electrochemical reactions and/or capacitive energy storage.

The fusing process may be configured to produce the fusing fibers 40, 42 with the functional material 20 including a capacitive additive (eg, MnO2, etc.). Such welded fibers 40, 42 exhibit enhanced energy storage properties when combined with a suitable electrolyte, including either gel or polymer 20 electrolytes.

The fusing process may be configured to produce the fusing fibers 40, 42 with the functional material 20 including a photoactive additive (eg, TiO2, etc.). Such weld fibers 40, 42 may exhibit enhanced self-cleaning properties (eg, for wide-gap semiconductors such as TiO2) and/or UV resistance.

Other uses for the welded fibers 40, 42 produced by the welding process herein include, but are not limited to, technologies ranging from anti-counterfeiting to drug delivery applications. Furthermore, the above listing of functional materials is not meant to be exclusive and/or limiting, and other functional materials may be used without limitation unless so indicated in the following claims. May be.

8. Modulation welding process

As described herein above, the fusing process is configured to allow a wide variety of fusing substrate finishes (eg, knitting yarn finishes) to be produced from conventional substrates (non-fiber fused). Also, the substrate may include knitting yarn and/or woven substrate in certain configurations of the welding process. For example, the deposition process may involve the use of a process solvent that is pumped at a controlled variable rate and/or a modulated rate, and/or the substrate (eg, weaving thread, sewing thread, fabric, and/or fabric). Temperature and/or pressure in the process solvent application zone 2, process temperature/pressure zone 3, process solvent recovery zone 4 by moving at a variable speed during the deposition process and/or by changing the process solvent composition. May be configured as a modulated deposition process by varying the tension (eg, substrate, process wet substrate, etc.) and/or combinations thereof.

In one aspect, the fusing process is capable of specifically and closely controlling the ratio of process solvent to the substrate containing the fibers such that the fusing process can convert a controllable amount of fibers in the substrate to a fused state. May be configured as. The ratio of process solvent to substrate may be optimized at least depending on the particular process solvent and substrate properties. For example, an ionic liquid (eg, 3-ethyl-1-methylimidizolium acetate, 3-butyl-1-methylimidizolium chloride, etc.) mixed with a polar aprotic additive (eg, acetonitrile), etc. In a deposition process configured to use a process solvent mixture, 1 part by weight of substrate to 1 part by weight process solvent addition to 1 part by weight substrate to 4 parts by weight process solvent addition. Ratios may be used. Another aspect of the deposition process may use a process solvent comprising cold alkali (sodium hydroxide and/or lithium hydroxide) with a urea solution, the ratio of process solvent being 1 part by weight of substrate. It may range from 2 parts by weight of process solvent to more than 10 parts by weight of process solvent with respect to 1 part by weight of substrate. Table 11.1 is an example of process parameters in which the welding system could be successfully used for the production of welded yarn using a process solvent containing an ionic liquid and a process solvent containing an aqueous hydroxide solution. The parameters are shown in Table 11, but the parameters do not limit the scope of the present disclosure unless so indicated in the following claims.

In one deposition process using a process solvent that includes an aqueous solution of hydroxide and urea, the hydroxide may include NaOH and/or LiOH. In the deposition process, the hydroxide may include 4-15 wt% LiOH and 8-30% urea. In certain applications, it may be advantageous to configure the process solvent to contain 6-12 wt% LiOH and 10-25% urea. In yet another application, it may be advantageous to configure the process solvent to contain 8-10 wt% LiOH and 12-16% urea.

Note that for the temperature ranges specified in Table 11.1, the temperatures may be optimized for the particular composition of the process solvent system. Further, the temperature and composition of the process solvent system is co-optimized with at least solvent application zone 2 hardware and/or process control software and/or equipment to effect deposition at desired amounts and locations on the substrate. May be done. That is, fiber fusing that provides either consistent welded substrate properties or modulated substrate properties. This can also be achieved during solvent application as well as by applying viscous drag as needed in the process temperature/pressure zone 3.

As shown in Table 11.1 and described herein above, the process solvent system may be configured as a mixture of IL liquid and molecular additive. The molar ratio of IL liquid to molecular additive can vary from deposition process to deposition process and can affect the optimum temperature of the process solvent system during its application to the substrate. For example, in a deposition process configured to utilize a process solvent system containing 1 mol BMIm 2 Cl to 1 mol ACN, if the temperature rises above 120° C. (in which case the deposition rate may be optimal), ACN The vapor pressure of can result in process conditions that are difficult to control (in terms of health and safety). As a result of this constraint, the deposition temperature is set to a lower temperature (eg 105° C.), but such a temperature requires a longer duration (>30 seconds). In contrast, in a deposition process configured to use a process solvent system containing EMIm OAc, the optimum temperature is between 80°C and 100°C, since the effectiveness of the process solvent is higher than that of BMImCl. The deposition time of EMIm OAc in the temperature range can be in the range of 5-15 seconds. Thus, the optimum temperatures of at least the process solvent application zone 2, the process temperature/pressure zone 3, and other steps of the deposition process may vary from application to application and are therefore not so indicated in the following claims. As long as it does not limit the scope of the present disclosure in any way.

See Table 9.1, Table 10.1, and Table 11.1 (all of which provide the main process parameters of the deposition process configured to use a process solvent containing an aqueous hydroxide solution). The optimal ratio of process solvent to substrate (mass or weight ratio) can then vary based at least on the type of substrate format. For example, a welding process configured for use with a 2D substrate may have a ratio of 0.5 to 7, with some welding processes optimally configured with a ratio of about 3.7. Welding processes configured for use with 1D substrates may have ratios of 4 to 17, with some welding processes optimally configured with a ratio of about 10. When the ratio is greater than or equal to about 10, specifically 17, the process-wet substrate results in over-saturation with the process solvent, whereby excess solvent not absorbed by the substrate and/or process-wet substrate is It was observed to reside outside the process wet substrate. However, the specific ratios for the deposition process using IL-based process solvents or aqueous hydroxide process solvents do not limit the scope of the present disclosure unless so indicated in the following claims.

It should be noted that for the process solvent values and compositions shown in Table 11.2, the additional functional material additive allows spatial modulation of the weld and unique controlled volume consolidation. The addition of functional materials such as dissolved cellulose to the welding process with appropriate hardware and controls can have a surprising effect on the shell welded yarn, at least as detailed above with respect to FIGS. 9I and 9J. .. That is, the amount of deposition may be controlled by the cross-section of the substrate (ie, the yarn diameter in the embodiment of FIGS. 9I and 9J) to provide a measure of toughness and elongation as compared to a control sample of the raw substrate. Weld substrates with both improved (ie, weld yarn substrates in this embodiment) can be produced.

The type of reconstituted solvent and its temperature, along with the various values listed in Table 11.1 can also have a surprising effect on the controlled volume consolidation when the reconstituted wet substrate is dried. Also be careful. A SEM image of a raw 1D substrate containing 18/1 ring spun cotton yarn is shown in FIG. One welded substrate is shown in Figure 14A and another welded substrate is shown in Figure 14B, both made from the substrate shown in Figure 13. Both the welding base materials shown in FIGS. 14A and 14B were manufactured using the welding process and apparatus shown in FIG. 9A.

Table 12.1 shows various characteristics of the raw substrate shown in FIG. Characteristic values are averages performed on about 20 unique samples of welded yarn substrate. The characteristic values were collected by using a mechanical characteristic tester manufactured by Instron Co., Ltd. by operating in a tensile test mode similar to ASTM D2256. The mechanical properties of each column heading in Table 12.1 are the same as described above for Table 1.2.

Table 13.1 shows some of the key process parameters used to make both the weld substrate shown in Figure 14A and the weld substrate shown in Figure 14B. The process parameters for each column heading in Table 13.1 are the same as described above for Table 1.1.

Table 13.2 shows various properties of the weld substrate shown in FIG. 14A manufactured using the parameters set forth in Table 13.1. Characteristic values are averages performed on about 20 unique samples of welded yarn substrate. The characteristic values were collected by using a mechanical characteristic tester manufactured by Instron Co., Ltd. by operating in a tensile test mode similar to ASTM D2256. The mechanical properties of each column heading in Table 13.2 are the same as described above for Table 1.2.

Table 13.3 shows various characteristics of the weld substrate shown in FIG. 14B manufactured using the parameters set forth in Table 13.1. Characteristic values are averages performed on about 20 unique samples of welded yarn substrate. The characteristic values were collected by using a mechanical characteristic tester manufactured by Instron Co., Ltd. by operating in a tensile test mode similar to ASTM D2256. The mechanical properties of each column heading in Table 13.3 are the same as described above for Table 1.2.

Comparing FIG. 14A with FIG. 14B reveals how volume controlled consolidation can be manipulated to obtain a particular quality of the welded yarn substrate. Specifically, the comparison between FIGS. 14A and 14B shows that the method, the composition of the reconstituted solvent, and/or the configuration of the process solvent recovery zone 4 (and/or other steps of the welding process) is We will show how it can affect the controlled volume consolidation and consequently the mechanical properties and/or other important attributes of the welded substrate. One of such attributes is the "feel" (i.e., how people feel when touching) of knitted and woven yarns and fabrics made therefrom.

Specifically, both the welded yarn base material shown in FIG. 14A and the welded yarn base material shown in FIG. 14B were manufactured using a welding process in which the reconstituted solvent contains water. However, the temperature of water was 22° C. in the knitted or knitted yarn base material of FIG. 14A, and was 40° C. in FIG. 14B. As is clear from the comparison between FIG. 14A and FIG. 14B, the welding substrate obtained by the welding process used to manufacture the welding substrate shown in FIG. 14A (cold reconstitution solvent) is the same as that of FIG. 14B (warmer reconstitution solvent). It has a significantly softer hand than the welding base material shown in FIG. Fabrics made with a similar weld yarn substrate made using a welding process having a reconstitution solvent above 40° C. are made from a weld yarn substrate made using a welding process having a reconstitution solvent at room temperature. It may have texture properties that are very different from the textured fabric. Therefore, the configuration of the process solvent recovery zone 4 (for example, the reconstruction method) and its conditions are important new parameters.

Still referring to FIGS. 14A and 14B, these were produced from the same welding process, but with different reconstitution solvent temperatures, and the temperature of reconstitution plays an important role in the controlled volume consolidation of the welded yarn substrate. It is clear that they will fulfill. Again, some mechanical properties of the welded yarn substrates of Figures 14A and 14B are shown in Table 13.2 and Table 13.3, respectively. All of the welded yarn substrates show significant improvement in mechanical properties over the original yarn substrate (eg, 15-23% improvement over the original yarn substrate), but were treated with reconstituted solvent at elevated temperature. The welded yarn substrate shown in Figure 14B (see also Table 13.3) was slightly larger in diameter and had more loose fibers/hair on the surface. 14B is slightly fibrous than the substrate shown in FIG. 14B, but the amount of fibers in FIG. 14B may be less than the corresponding amount of raw yarn substrate shown in FIG. Recognize. Further, the fibers on the welded yarn base material of FIG. 14B are fixed to the welded yarn base material so as to withstand separation from the welded yarn base material as lint. Throughout the fusing process, the modified fibers/hairs at or near the surface of the fusing substrate can be an important attribute that affects the feel of fabric knitted or woven from the fusing substrate.

In general, the solvent ratio of a particular value within the range just described will remain constant, as long as the ratio remains constant, and other important variables such as temperature will also remain constant during the deposition process. That ratio can be used to produce a very consistent welded yarn to a substrate that includes a knitted yarn. The fusing process may then be configured to produce a fusing substrate that exhibits a certain amount of fusing such that there may be a certain amount of fusing fiber in the length of the fusing yarn.

The dynamic process solvent ratio (defined herein as the ratio of the weight of the process solvent to the weight of the substrate), the composition of the process solvent, the pressure, and the appropriate control of the method of applying the process solvent allow The effect is obtained. For example, suitable dynamic controls can be used in the welding process to produce a welded substrate with the appearance of heather and/or space dyeing (multicolor effect), where the welded substrate containing the knitting yarn or fabric is , May have varying degrees of coloration, which may be the result of dynamic control of the welding process. The production of heather and/or space dyeing effects can only be apparent during dyeing and finishing if these textile manufacturing steps are achieved after the welding process.

However, the modulation welding process is not limited to producing a heather or space dyeing effect, having a variable diameter (having different yarn weights, without the need for substrates of variable length and/or diameter) "embossed. It can also be configured to produce any number of other unique effects, such as knitting yarns or the technical terms that describe them do not yet exist in the textile industry. The degree to which the effect is observed can also be correlated with the yarn or textile substrate on which it acts. For example, the types of spinning processes (eg, ring spinning, open-end spinning, vortex spinning, etc.) used to produce the substrate containing the knitting yarn are different from each other under different welding conditions (eg, different process solvent ratios and/or application methods). ) May be required.

A. Modulation and non-modulation welding processes compared

One representative example of a modulated welding process is now described and compared to a non-modulated welding process (as above). However, the above illustrations are not meant to imply any limitation, and the particular parameters thereof, therefore, do not limit the scope of the disclosure, unless so indicated in the following claims.

In the non-modulation deposition process, the deposition process may be configured for a substrate that includes 30/1 ring spun yarn, which substrate is consistently colored, consistently operated by consistently operating the deposition process. It can be converted to a highly consistent weld substrate with a feel and finish, and a consistent amount of visible outer fiber "hair". For example, by configuring the fusing process to use a stable process solvent to substrate mass ratio, constant yarn transfer rate throughout the fusing process, consistent temperature and pressure, etc. It may also represent all or part of the weld substrate described herein above.

Alternatively, if desired, the modulation welding process may have the appearance of a multicolored heather or space dyeing substrate with 30/1 ring spun yarn by dramatically changing some parameters of the modulation welding process. It may be configured to be converted into a welding base material including a knitting yarn. The fusing process uses a substrate containing a 30/1 ring spun yarn of a commodity, which is a mass-produced, generally uniform product, with a unique appearance, feel, and/or texture for a number of end uses and applications. This is a surprising and very useful result because it can be automated to convert to a welded substrate that includes a welded yarn with a finish. In a correlated modulation welding process, the welding process is based on heavier (including but not limited to Ne18 knitting yarn) and light (including but not limited to Ne40 knitting yarn) articles and substrates that include special knitting yarn. It may be configured for use in wood and is not limited unless so indicated in the following claims.

Furthermore, the modulation welding process is not limited to configurations that produce effects and finishes that are specific to only substrates that include knitting yarns. For example, application of process solvents including, but not limited to, mixed inorganic solvents such as aqueous solutions of lithium hydroxide and/or sodium and urea may be applied to substrates including textile yarns as well as conventional materials (eg, welding processes). It can also be applied to substrates including whole fabrics made from either unthreaded textile yarns) or welded substrates (eg welded yarns).

Treatment of the fabric using the fusing process can be performed on localized area(s) of the fabric or garment. For example, processes such as those used for inkjet and/or screen printing of process solvents can be very useful methods for achieving area-specific deposition processes on 2D and/or 3D substrates. Alternatively, the welding process may be configured to produce a 2D and/or 3D welded substrate with relatively uniform properties compared to the overall material or garment.

When a welding process is configured and used with its various parameters properly controlled (eg, limited welding time, relatively low process solvent ratio, etc.), the welding process produces a knitting yarn bond within a fabric. It is possible to produce a welded substrate in which the strength and pilling properties of the woven and knitted fabrics are improved compared to the corresponding conventional raw substrate without undue excessive welding. Alternatively, welding processes of different configurations (e.g., longer welding times, higher process solvent ratios, etc.) can be used for weaving and weaving with welded yarn joints welded and/or partially welded into weaving and knitting materials. Welded substrates may be produced that include a knitted material to provide a stiffer and/or more robust material. The advantage of using a welding process for 2D and/or 3D substrates (eg fabrics, textiles) as compared to 1D substrates (eg weaving threads, sewing threads) is that a large amount of material is processed simultaneously. .. However, as described above, by welding the base material including the knitting yarn and/or the sewing yarn before the weaving and/or the knitting, a large number of synergistic effects in manufacturing and performance may be obtained. The choice of when and how a given deposition process is applied to a particular substrate is highly dependent on the type of outcomes aimed at/the end use application of the deposited substrate, and thus as such in the following claims. Unless otherwise indicated, the scope of the present disclosure is not limited in any way.

In addition to the above possibilities, 1D (eg knitting and/or sewing threads), 2D and/or 3D substrates (eg fabric and/or fabrics corresponding to 2D and/or 3D substrates) and/or To make the cross-sections of the components of the substrate (eg individual knitting or sewing threads of 2D and/or 3D substrates) other than circular, or to form a welded substrate having a circular cross-sectional shape. , It is possible to configure the welding process. Possible shapes include, but are not limited to, flat oval or ribbon-like shapes. This may utilize appropriately shaped dies and/or rollers located within process solvent application zone 2, process temperature/pressure zone 3, process solvent recovery zone 4, drying zone 5, and/or combinations thereof. Can be achieved by configuring a welding process for

Conventional knitting yarns used as substrates typically produce a welded substrate that exhibits a generally circular cross-sectional shape after welding. In general, this is because when the fibers are welded/fused, the capillary forces wick the process solvent towards the core of the textile yarn, so that potential energy can be minimized. The welding process provides a non-circular cross section by using at least a unique molding method and/or apparatus for operating the process wet substrate and/or by molding the reconstituted wet substrate during its drying. It may be configured so as to obtain a welded yarn base material having the same.

B. Modulated and non-modulated deposition processes using spatially controlled heating and/or spatially controlled process solvent application

Spatial control of the addition of chemicals to substrates (eg inkjet printing of ionic liquids) has already been disclosed in US Pat. No. 6,048,388 (Patent Document 4) and the like. Spatial control of the deposition process is at least to thermally activate selected areas within the substrate (to manipulate any properties and/or characteristics of the resulting deposited substrate, as detailed above). Can also be controlled directly, where the welding process may be configured as a modulation welding process using spatially controlled heating. IL-based solvents typically do not appreciably deposit (modify) the natural fiber substrate 10 at room temperature (about 20° C.) over a time frame on the order of minutes. Typically, the application of heat can be advantageous to activate and/or speed up the welding process. This involves heating the entire substrate at a temperature above about 40° C. for at least a few seconds.

A schematic of a welding process that may be configured as a modulation welding process is shown in FIG. 11A, which may utilize a 2D substrate. The modulated deposition process shown in FIG. 11A may be configured to use infrared (laser) light to heat specific locations on the substrate to which the process solvent was previously applied. Heat from the directed energy beam can activate the welding process at specific locations on the substrate, and in one configuration of the welding process, cellulose I (natural cotton substrate) to cellulose II (after welding) (Cotton substrate) and controlled volume consolidation (ie the thickness of the substrate may be reduced in the unaffected areas).

As is apparent by comparing FIGS. 10B and 11E, changes to the surface of the substrate are apparent upon visual inspection, which changes are the result of exposure by the directional energy source. Furthermore, by controlling the output of the energy source (keeping the output low enough), the substrate (cellulose in this example) was not abraded. The welding process may be configured using electromagnetic energy of any suitable wavelength to achieve spatially controlled heating, without limitation unless so indicated in the following claims, examples of which Include, but are not limited to, visible light, microwaves, ultraviolet light, and/or combinations thereof.

Referring now to both FIGS. 11A and 11B, there is shown a schematic diagram of a modulation welding process applied to a 2D substrate, FIG. 11A showing spatially controlled heating, and FIG. 3 shows spatially controlled process solvent application. Again, FIG. 11A shows heating with a directed energy beam to the substrate, process wet substrate, and/or process solvent. The amount and/or composition of process solvent may be modulated at a particular location on the substrate or widely throughout. Referring to FIG. 11B, the amount of process solvent and/or its composition may be modulated at a particular location and then a large area of the process wet substrate may be heated by a broad energy source. Any modulation welding process can result in volume controlled consolidation of the substrate after reconstitution and drying.

Referring now to both FIG. 11C and FIG. 11D, there is shown a schematic diagram of a modulation deposition process applied to a 1D substrate, FIG. 11C showing spatially controlled heating, and FIG. 3 shows spatially controlled process solvent application. As shown in FIG. 11A, heat may be added to the substrate, process wet substrate, and/or process solvent by a pulsed energy source. The amount and/or composition of process solvent may be modulated at a particular location on the substrate or widely throughout. Referring to FIG. 11D, the amount of process solvent and/or its composition may be modulated at a particular location, after which a large area of the process wetting substrate is heated by a broad energy source and/or a pulsed energy source. May be. Any deposition process may be configured to carefully control the process solvent effectiveness and rheology and associated viscous drag to achieve the desired effect.

An image of a modulated weld yarn substrate produced by a modulated weld process in which the process solvent flow rate is modulated (eg, pulsed in a manner similar to FIG. 11D) is shown in FIG. 11E. Once the modulated deposition process is configured to achieve the desired viscous drag (in this example, by physical contact with the process wetting substrate and spreading the process solvent from the initial contact point), the deposition substrate Lightly welded portions and firmly welded portions alternate along the length direction of the. In FIG. 11E, the right part of the figure is lightly welded and the right part of the figure is firmly welded.

An image of a fabric made from a welded substrate treated with the modulation welding process is shown in FIG. 11F. The fusing substrate used to fabricate the fabric of FIG. 11F may be produced by the fusing process and apparatus described above herein, as shown in FIG. 9A. The modulated deposition process was achieved by modulating the process solvent pump speed and viscous drag. With proper control of the welding process, varying degrees of controlled volume consolidation and specific degrees of welding were achieved. The net result was a modulation of the amount of bristles and open spaces in the welded yarn substrate.

After knitting a modulated welded yarn substrate into a fabric and dyed, the depth of color was found to vary with the degree of welding. This resulted in a surprising "space stain" or "heather" effect, as is apparent from Figure 11F. Typically, in the fashion industry, achieving this effect requires knitting multiple knitting yarns into a single fabric. Modulated fiber fusing not only adds the previously mentioned benefits of shorter drying times and enhanced moisture management, but in this case also adds a unique but controllable color modulation of interest in various fashion applications. Combining the modulation welding effect with a given stitch length and/or the tightness factor of the woven fabric further enhances the color and texture of the fabric. This new result may find application in any number of conventional and functional products.

As briefly mentioned above, the welding process may be configured to control the amount of cellulose I crystals converted to cellulose II crystals. Referring now to FIG. 15A, an X-ray diffraction data (XRD) of a cotton yarn substrate (Plot A) and cotton yarn completely dissolved in excess ionic liquid process solvent and then reconstituted (Plot B) is illustrated. There is. Plot B, as used herein, is based on the fact that the entire yarn base material has been modified and the structure of the unmodified biopolymer has been completely altered, unless otherwise noted in the claims below. Material" or "welded yarn substrate" or any other substrate made in accordance with the present disclosure. In plot A, the unmodified cotton cellulose polymer is clearly shown in the cellulose I state. In plot B there is a distinctly less crystalline character of cellulose II. This represents cotton that has been completely dissolved and its native structure completely destroyed.

Table 14.1 shows some of the main process parameters used to make three separate weld substrates, where the first two rows of process parameters are for the welding process and equipment shown in FIG. 9A. The third row welding process and apparatus may be used for the welding process and apparatus shown in FIG. 10A. The process parameters for each column heading in Table 6.1 are the same as described above for Table 1.1.

Referring now to FIG. 15B, a plot of XRD data for three welded yarn substrates made using the process parameters shown in Table 14.1 is provided, with Plot A being one row of Table 14.1. Corresponding to the eye, plot B corresponds to the second row, plot C corresponds to the last row of Table 14.1. By comparing and contrasting FIGS. 15A and 15B, the welded yarn substrates produced with the welding process and apparatus of FIGS. 9A and 10A using the process parameters of Table 14.1 respectively have a cotton unmodified cellulose I structure. At the same time, it is clear that the welded yarn substrate is controllably modified to exhibit enhanced properties and/or attributes. Preservation of the unmodified Cellulose I structure can be achieved using a variety of process solvent systems and a variety of equipment, as detailed herein above.

9. Welding process for dyeing and resulting product

A. Background technology of indigo dyeing

Indigo dyes are widely used in the treatment of cotton fabrics. The indigo molecule, 2,2'-bis(2,3-dihydro-3-oxoindolidene), is generally water soluble and therefore not used directly for dyeing textiles. Instead, in the prior art, a water-soluble reductant called leuco indigo (or white indigo) is used for dyeing textiles. Upon subsequent exposure to oxygen, it reverts to its oxidized state, which has a characteristic blue color. The prior art indigo dyeing process is very water intensive and requires large amounts of auxiliary process chemicals such as sodium dithionite (sodium hydrosulfite), sodium hydroxide and detergents (wetting and cleaning agents). And In the prior art indigo dyeing process, the dye can penetrate into the knitting yarn only for a short distance and therefore requires multiple passes (dipping) through the dye vat in order to accumulate the desired color strength.

Techniques for improving the dyeing process have been proposed in the art, but none significantly reduce the water demand and the required amount of acid and/or alkaline solution. Bianchini et. al, ACS Sustainable Chem. Eng. 2015, 3, 2303-2308 (Non-Patent Document 1) propose to improve the uptake of disperse dyes in fabric by adding 2 g/L of ionic liquid to the dye solution. Although this technique has been shown to be effective for this class of dyes that have some level of water solubility, it is not applicable to water insoluble dyes (eg, indigo).

US Pat. No. 7,731,762 discloses the use of ionic liquids as carriers for dyes. The ionic liquids disclosed in the above patents are not known to interact strongly with cellulosic materials and are not considered chaotropic. Moreover, the above patent does not disclose ionic liquids specifically selected for use with indigo dyes in the dyeing of cellulosic products.

U.S. Patent Application Publication No. 2006/0090271 discloses the use of ionic liquids to partially dissolve the outer surface of cellulosic fibers, and dyes or dye fixing agents, either simultaneously or sequentially. The application of benefit agents including is disclosed. Nowhere in the above disclosure is the specific embodiment of the ionic liquid and dye combination particularly suitable for the indigo dyeing process.

In conventional dyeing as defined herein, colorants such as molecular dyes are dissolved/dispersed in solution at the molecular level. Upon exposure to such a solution, the substrate (eg, textile yarn, fabric, etc.) absorbs the dye and assumes the color of the dye. Dyes can react with special linking chemicals that form covalent bonds between the dye and the substrate. Alternatively, the dye is non-reactive, simply by absorbing and by intermolecular association (eg, dispersion, dipole-dipole, hydrogen bond, ion-dipole, ion-ion, and/or other attractive forces). Can be associated with a substrate.

In the cross section of a typical ring-spun undyed textile yarn base material 90 shown in FIG. 16A, individual undyed textile textile substrates 92 are displayed, and the undyed textile yarn base material 90 is colorless (under ambient conditions. It is displayed so that it looks white). A cross-sectional view of the same undyed knitted yarn base material 90 after being treated with a prior art indigo dyeing process is shown in FIG. 16B. A dyed knitted yarn base material 90' and an individual dyed fiber base material 92' are displayed. As shown in FIG. 16B, there is a color gradient that progresses from the outer surface of the dyed knitting/woven yarn base material 90′ toward the inside thereof in a substantially radial direction, and as a result, the dyed fiber base close to the outer surface of the dyed/knitted textile yarn base material 90′. The material 92' is more colored than the fiber base material that is closer to the inside of the dyed knitting or weaving yarn base material 90'.

In conventional pigment padding as defined herein, a colorant, such as, but not limited to, micro- to nanometer-sized pigment particles of a colorant (eg, indigo) is a binder (often a polymeric binder material). ) Is also dispersed in the solution containing. Upon exposure to such a solution, the binder and pigment particles are placed on the substrate fiber, and the binder holds the pigment particles in and on the substrate. The binder may be reactive (forming a new chemical bond) with the substrate or non-reactive (associating by intermolecular interactions, including but not limited to those mentioned above).

B. Overview of dyeing and welding process

The dye fusing process according to the present disclosure enables a surprising new pigment padding technique for indigo. Specifically, the dye welding process may be configured as one type of pigment padding process in which indigo pigment particles are added to a cellulosic substrate (eg, cotton substrate). For example, in one of the dye fusing processes disclosed herein, the process may be configured with an aqueous process solvent, the aqueous process solvent comprising alkali metal hydroxide and urea, indigo on cotton yarn. The cellulose and indigo pigment particles that can be used for addition may be used in a dissolved state. The dye fusing process can be carried out to achieve key aspects of the pigment padding technology. While accomplishing this, the use of the harsh chemicals currently used in commercial indigo dyeing processes (which serve to reduce indigo to its anionic form) is avoided. This has a significant impact on the process costs, especially on the amount of water used to carry out the indigo dyeing. The dyeing and welding process described herein has heretofore not been possible with traditional dyeing and/or pigment padding techniques because the welding process can also be configured to adjust the physical properties of the natural fiber substrate. In a manner, it also allows for additional conditioning of the fabric (ie, fabric).

Further, the use of a process solvent that is a solvent for the biopolymer material (ie, cellulose, silk, etc.) that can also dissolve some amount of pigment (molecules and/or ions) adds pigment particles with a binder. In addition, it may enable new “hybrid” dyeing techniques, in which molecular and/or ionic dye species can be introduced into and into the fiber substrate. Such hybrid techniques can incorporate elements of both traditional dyeing techniques and pigment padding techniques. In one dye fusing process, the indigo dye particles can be dispersed in a process solvent that contains a solubilizing polymer (eg, a cellulosic binder) and that also has an additive effect on the dissolution of the indigo dye molecules. Specifically, ionic liquid-based solvents with specific molecular cosolvent additives can be tailored for this hybrid method. A material in which a process solvent is dissolved or suspended in a process solvent with suitable viscous resistance and in a novel and unique manner using a welding process as described herein above, such as a cellulosic binder. And with indigo dye (both pigment particles and molecular indigo species) applied to textile yarns.

In the dyeing and welding process constituted by using a process solvent containing an ionic liquid, a molecular co-solvent such as acetonitrile (“CAN”), dimethylsulfoxide (“DMSO”), dimethylformamide (“DMF”) is appropriately used, For example, the effect of the solvent on the cellulosic binder and the molecular indigo dye/indigo pigment particles can be adjusted. Assuming appropriate viscous drag is used throughout the dye deposition process (eg, at least process solvent application zone 2, process temperature/pressure zone 3, and/or process solvent recovery zone 4), the entire dye deposition process is It may be configured to provide a weld substrate having a desired color (either a consistent, controllable shade and/or a modulated color, if desired). In addition, by adding an additional process solvent containing an additional binder (eg, cellulose dissolved in an ionic liquid-based process solvent), the effects described above (at least shown in FIGS. 9I and 9J, “shell welding ( )))) to control the degree of entrapment of dye in the resulting weld substrate, while at the same time controlling the physical properties of the resulting weld substrate (eg, controlled volume consolidation, substrate The effect of adjusting the amount of hair on the material surface, strength, and other mechanical properties) can be obtained. That is, the dye fusing process can be configured to simultaneously deliver and adjust the color of the resulting fusing substrate (eg, fusing yarn substrate) and, at the same time, adjust its physical properties.

The following description generally relates to a method of making a welded substrate, in which the welding process may be configured such that the resulting welded substrate is also colored and/or dyed simultaneously with welding (the present Generally referred to herein as the "dye welding process"). Although the following description focuses primarily on indigo dyes applied to cellulosic substrates, the scope of the present disclosure is not so limited, unless otherwise indicated in the claims below, and in general The concepts may be applied to other coloring and/or dyeing agents and/or substrates, if applicable.

In one aspect of the dye deposition process, a process solvent system comprising a chaotropic ionic liquid (ie, an ionic liquid capable of at least partially dissolving cellulose) in a solution with an aprotic solvent comprises an indigo dye of a cellulosic-based substrate. It can be carried in and do an effective dyeing. As used herein, "fiber", "cellulosic fiber", "cellulose", "braided yarn", and "suture" may all be used interchangeably and the scope of the present disclosure is as follows: Unless otherwise indicated in the claims, it extends to all such cellulosic materials. In another aspect of the fusing process configured for use with a coloring and/or dyeing agent, the substrate may be configured as a 2D substrate or a 3D substrate, unless so indicated in the following claims. , Not limited.

Surprisingly, during reconstitution of the process wet substrate (eg, in the process solvent recovery zone 4 where ionic liquid and aprotic solvent are removed from the fiber), removal of the process solvent or a portion of the process solvent is There may be no or negligible amount of the indigo dye molecule that is applied. That is, when the indigo dye molecule is carried into the cellulose fiber, it is thereby strongly bound to the cellulose fiber and the removal required to remove (wash) the process solvent (in this case, the ionic liquid and aprotic solvent). The force is insufficient to remove bound indigo dye.

In contrast to the prior art, the dye fusing process may also add fiber modification benefits that may occur concurrently with the dyeing process. This fiber modification is through a welding process as disclosed in US Pat. No. 8,202,379, which is incorporated herein by reference in its entirety, or in any of the above-mentioned co-pending applications. It may be configured to smooth and/or strengthen the knitting yarn. In a fusing process configured to provide both dyeing and modification of the fiber through the fusing process, the ionic liquid can carry the indigo dye into the yarn and partially dissolve the outer layer of the fiber. In some cases, it may be possible to improve its strength and/or smoothness and/or to add other functional materials to the fiber by the welding process.

As detailed above with respect to the capture of functional materials by the fusing process (and at least with reference to FIGS. 4A-D and 5A-D), the dye fusing process involves the addition of a colorant (eg, indigo dye) to a biopolymer. It may be configured to capture in a matrix. Such a dye fusing process may produce a fusing substrate that is colored in a manner similar to pigment padding, where the biopolymer may act as a binder.

In addition, the dye-fusing process is subject to various compatibility constraints (eg, chemical compatibility, property compatibility, etc.) that are characteristic of the fusing substrate described herein above with respect to fusing substrates produced by the dye-fusing process. May be configured to impart any of the following, and is not limited unless so indicated in the following claims.

C. Exemplary dye welding process

Various examples of dyeing and fusing processes designed for indigo dyeing of cellulose fibers are detailed below. However, the above illustration is not meant to imply any limitation, and its specific parameters, temperatures, pressures, ratios, etc., therefore, do not limit the scope of the present disclosure, unless so indicated in the following claims. Absent.

In one aspect of the dye fusing process, the indigo dye powder may be suspended and partially solubilized in a process solvent that includes a chaotropic ionic liquid solvent. Such solvents include, but are not limited to, 1-ethyl-3-methylimidazolium acetate (“EMIm OAc”), 1-butyl-3-methylimidazolium chloride (“BMIm Cl”), 1- Propyl-3-methylimidazolium acetate ("PMIm OAc"), and as described in US Pat. No. 7,671,178 (Patent Document 3), which is incorporated herein by reference in its entirety. Other known ionic liquid solvents (those capable of dissolving natural fibers) can be mentioned. However, the scope of the present disclosure is not limited by the particular ionic liquid, unless so indicated in the following claims. Moreover, the process solvents used to deliver indigo dyes and/or other materials are rarely pure. In fact, the process solvent is often a mixture of ionic and molecular species (eg EMIm Ac+DMSO+ACN or LiOH+urea+water), and the process solvent may even consist solely of molecular species. In general, the smaller the individual particle size of indigo in powder form, the greater the effectiveness of coloring using the dye welding process. In some dyeing and coloring processes it may be advantageous to use indigo powder with a particle size in the range of 0.01 to 10 μm. In other processes, it may be advantageous to use indigo powder with a particle size in the range of 0.1-1.0 μm. Therefore, the particular particle size, physical properties, and/or other characteristics of the indigo used in the dye welding process do not limit the scope of the present disclosure unless so indicated in the following claims. ..

The use of aprotic polar solvents (eg DMSO, DMF, etc.) as co-solvents (forming process solvent systems) with ionic liquids can reduce the viscosity of the process solvent and is thus particularly useful for facilitating processing. It has been found to be advantageous. However, other additives may be used with the ionic liquid and are not limited unless so indicated in the following claims. In general, ionic liquids and any additives to such liquids are referred to herein as "process solvents", but may also be referred to as "process solvent systems". The indigo dye is only slightly soluble in DMSO and DMF. Therefore, the benefits of direct dyeing with a mixture of ionic liquids and DMSO or DMF in a particular dye deposition process are not primarily attributed to the improved solubility of the indigo dye in the process solvent. However, in other dye fusing processes, process solvents containing DMSO or DMF can result in a relatively large amount of coloration on the fusing substrate (as opposed to pigment padding).

It has been found that the indigo dye is slowly reduced in EMIm OAc over time, changing from a characteristic blue to green hue. Therefore, it is envisioned that in many applications it may be advantageous to use the suspension within 48 hours of its initial preparation.

In the experiment, the indigo dye was successfully applied to the yarn according to the following process steps. Indigo dye powder (0.5-3% by weight) is suspended in a solution of EMIm OAc and DMSO in a weight ratio of 50:50. The mixture is agitated to prepare a microfluidic suspension. The suspension is then filtered through a >50 mesh screen to remove unsuspended particles of dye that could lead to application inconsistencies or blockage of process equipment. This process solvent is sent to an injector for application to the textile yarn. When using a process solvent in which EMIm OAc and DMSO are blended, it is preferable that the ratio of the process solvent to the fiber is 1 to 6 times the mass of the process solvent with respect to the mass of the yarn to be treated. The time of fusing and simultaneous dyeing is 5 to 15 seconds at a process temperature of 70°C to 100°C. The welded and dyed textile yarn may then proceed to a rinsing and reconstitution step to stop the welding process. It has been found that removing the process solvent from the textile yarn does not remove the indigo dye. The welded and dyed textile yarn may then be dried and packaged by methods similar to those currently practiced in the industry.

In general, the raw 1D substrate comprising cotton yarn is melted in a fusing process as described above, in particular a fusing process of similar construction to that shown in FIG. 9A in which the indigo dye is included as part of the process solvent. There are cases where The process solvent may include an ionic liquid (eg, EMIm OAc), a co-solvent, an indigo powder, and optionally dissolved cellulose. In these experiments, certain co-solvents (eg acetonitrile (ACN), DMSO, DMF, etc.) have been shown to have a relatively short residence time in process temperature/pressure zone 4 so as not to chemically modify the indigo dye. It has been found to be ideally performed with a welding process configured to. Such cosolvents can cause reduction of the indigo powder if the indigo powder is exposed to the cosolvent for an extended period of time. In contrast, dimethyl sulphoxide (DMSO), when used with EMIm OAc, does not reduce the indigo dye quickly and DMSO (or DMF) can solubilize at least a portion of the indigo dye in comparison with other dyes. It can be an advantageous co-solvent for the welding process. Furthermore, in certain dye-fusing processes, it may be advantageous to include some cellulose dissolved in the process solvent.

The resistance of the dyed textile yarn to clocking (dye erosion) is measured according to AATCC 8 using a crock meter. According to this procedure, the knitting yarn is wound on a rigid panel and mounted parallel to the direction of movement of the device arm. A clean white test fabric patch is rubbed against the knitting yarn for a total of 20 strokes (10 strokes) and the color of the test fabric patch is compared to the grayscale control. The dyed sample having no color transfer is given a rating of 5 (very good), and the test cloth patch with severe contamination is given a rating of 1 (very bad). Textile yarn samples were prepared according to various process conditions and then tested according to AATCC 8 as described in the experimental description below.

First exemplary dye welding process

In this dyeing and welding process, a raw substrate containing 10/1 ring spun cotton yarn was prepared by adding 3% by weight of indigo powder to a process solvent containing EMImOAc:ACN at a weight ratio of 67:33 (1M:2M). Used and welded. This mixture was subjected to a double asymmetric centrifugal mixing process in a FlackTek mixer to ensure thorough mixing of the process solvents. This process solvent was applied to the textile yarn substrate in a welding process. At this time, the knitting yarn was not completely dissolved, but the properties of the knitting yarn were improved by partially dissolving the knitting yarn, thereby fusing the knitting yarn fibers together. Here, the process solvent application zone 2 is configured with an injector 60 (where the process solvent impinges on the weaving yarn) kept at 75° C. and a substrate outlet 64 (this is the process temperature/pressure zone 3). Which may constitute all or part of) was kept at 100°C. The process solvent was applied to the weaving yarn at an applied amount of 3 times the weaving yarn weight (that is, for every 10 g of the weaving yarn passing through the injector, 30 g of the process solvent was pumped into the injector 60). The knitted yarn was drawn through the welding column (ie process temperature/pressure zone 3) at a speed such that the total welding time was approximately 10 seconds. The knitted yarn was then reconstituted in a countercurrent column at 70°C ACN. The countercurrent velocity was greater than 10 times the process solvent dose rate. After winding the fused thread base material on a spool, the spool was rinsed with water and then dried. The resulting welded yarn substrate was then wound onto a rigid holding device and tested according to AATCC8. As a result of the test, the clocking resistance was very low, and the score was 1.5.

Second exemplary dye welding process

The second exemplary process is a dye fusing process very similar to the process used in the first dye fusing process discussed immediately above, in which the raw yarn substrate is the dispersed indigo powder 3 It was prepared with a process solvent containing both wt% and 0.3 wt% dissolved cellulose. The textile yarn substrate was similarly fused and reconstituted, then rinsed and dried as described above for the first exemplary dye fusing process. The resulting welded yarn substrate was tested according to AATCC8. As a result of the test, the clocking resistance was very low, and the score was 1.5.

Third Exemplary Dye Welding Process

The weld yarn substrate made by the first exemplary dye welding process was treated in a second welding process in an attempt to further secure the dye to the textile yarn and minimize clocking. The second welding process used a process solvent containing no indigo powder but 0.5% by weight of dissolved cellulose. Process solvent application zone 2 and process temperature/pressure zone 3 for the second fusing were constructed as described for the first dye fusing process. The double welded yarn was reconstituted in countercurrent ACN at 70°C as well. The twice-welded yarn was rinsed with water, dried, and then subjected to the AATCC8 clocking test. The clocking resistance of this double-bonded yarn improved to a rating of 2.5, but the test fabric patch also had a green hue rather than an indigo blue color.

Fourth exemplary dyeing and welding process

The welded yarn substrate made by the second exemplary dyeing and welding process was treated in a second welding process in an attempt to further secure the dye to the textile yarn and minimize clocking. Here, the second welding process used a process solvent containing 0.5 wt% dissolved cellulose. Process solvent application zone 2 and process temperature/pressure zone 3 for the second fusing were constructed as described for the first exemplary dye fusing process. The double welded yarn was reconstituted in countercurrent ACN at 70°C as well. The twice-welded yarn was rinsed with water, dried, and then subjected to the AATCC8 clocking test. The clocking resistance of this double-bonded yarn was improved to a rating of 2, but the test fabric patch had a green hue rather than the true indigo blue color.

Fifth exemplary dyeing and welding process

The welded yarn substrate was treated in exactly the same manner as the fourth exemplary dyeing and welding process described above, except that water at 70° C. was used instead of using hot ACN as the reconstitution solvent. The double-bonded yarn exhibited a slightly improved clocking resistance with a rating of 2.5. The test fabric patch was still not true indigo blue, but was less green than the test fabric patch used to test the double-bonded yarn substrate twice in the third exemplary dye-weld process.

Sixth Exemplary Dyeing and Welding Process

A double fusing yarn made by the fourth exemplary dye fusing process was treated with a third fusing process in an attempt to further lock the dye to the textile yarn and minimize clocking. The third welding process used a process solvent containing 0.5 wt% dissolved cellulose. The three times welded yarn was reconstituted in countercurrent water at 70°C. The three times welded yarn was rinsed with water, dried, and then subjected to the AATCC8 clocking test. The clocking resistance of this three-time fused yarn was improved to a score of 3.5. The test fabric patch was still not true indigo blue, but was less green than the test fabric patch used to test the double-bonded yarn substrate twice in the third exemplary dye-weld process.

Seventh exemplary dyeing and welding process

In this dyeing and fusing process, a green substrate containing 10/1 ring spun cotton yarn was treated with 2.5% by weight of indigo powder and 0.25% by weight of process solvent containing EMIm OAc:DMSO in a weight ratio of 50:50. Welding was performed using the one to which cellulose was added. This mixture was subjected to a double asymmetric centrifugal mixing process in a FlackTek mixer to ensure thorough mixing of the process solvents. This process solvent was applied to the textile yarn in a natural fiber welding process. At this time, the knitting yarn was not completely dissolved, but the properties of the knitting yarn were improved by partially melting the knitting yarn, thereby fusing the knitting yarn fibers together. Here, the process solvent application zone 2 is configured with an injector 60 (where the process solvent impinges on the weaving yarn) kept at 75° C. and a substrate outlet 64 (this is the process temperature/pressure zone 3). Which may constitute all or part of) was kept at 100°C. The process solvent was applied at an applied amount of 4 times the weight of the weaving yarn (that is, 40 g of the process solvent was pumped into the injector 60 for each 10 g of the weaving yarn passing through the injector). The knitted yarn was drawn through the welding column (ie process temperature/pressure zone 3) at a speed such that the total welding time was approximately 10 seconds. The braided yarn was then reconstituted in a 70° C. water countercurrent passage. The countercurrent velocity was greater than 10 times the process solvent dose rate. After winding the fused thread base material on a spool, the spool was rinsed with water and then dried. The fused yarn substrate was then wound onto a rigid holding device and tested according to AATCC8. As a result of the test, the clocking resistance was very low and the score was 1.

Eighth exemplary dyeing and welding process

Weld yarn substrates made by the seventh exemplary dye welding process were treated in a second welding process in an attempt to more firmly secure the dye to the textile yarn and minimize clocking. The second welding process used a process solvent containing EMIm OAc:DMSO in a weight ratio of 50:50 without indigo powder but with 0.5% by weight of dissolved cellulose. The double welded yarn was similarly reconstituted in countercurrent water at 70°C. The twice-welded yarn was rinsed with water, dried, and then subjected to the AATCC8 clocking test. The clocking resistance of the double-bonded yarn was improved to a score of 3, and the test fabric exhibited a characteristic indigo blue color.

Ninth Exemplary Dye Welding Process

A Kelvar® knitting yarn substrate was used as a second exemplary dyeing and fusing process (ie, process solvent was 3 wt% dispersed indigo powder, 0.3 wt% dissolved cotton, weight ratio 67: 33 of EMIm OAc:ACN) and reconstituted indigo blue cotton was examined to see if it adhered to the yellow Kevlar® knitting yarn substrate. The resulting welded yarn substrate did not turn blue and the blue tint was easily removed by rinsing.

Tenth Exemplary Dyeing and Welding Process

In this dye welding process, the dye welding process comprises two or more process solvent application zones 2, two or more process solvents, two or more process temperature/pressure zones 3, and/or two or more process solvent recovery zones. 4 (which may also be referred to as the reconstruction zone). Therefore, such a dyeing and fusing process results in a fusing yarn substrate that is similar to the two and/or three times fusing yarn substrate described above, but with one substrate feed zone 1, one process solvent recovery zone 4, 1. It may be configured to achieve the efficiencies obtained from one drying zone 5 and/or one deposition substrate collection zone 7. In general, the various zones of the dye welding process (or steps thereof) may be separate from each other, or one or more zones may be adjacent to each other with a gradual transition from one zone to the next. And it may not be possible to determine the specific end point of one zone and the start of another zone.

The dye deposition process may be configured to apply two separate process solvents to the substrate sequentially, using two process solvent application zones 2 and two process temperature/pressure zones 3. However, the dye fusing process may be configured to require only one process solvent recovery zone 4, which removes all or part of both process solvents. Alternatively, the dye deposition process may be configured with two separate process solvents and one process solvent application zone 2 and process temperature/pressure zone 3.

In yet another dye fusing process, two separate process solvents may be applied to the substrate sequentially and two process solvent application zones 2 and two process temperature/pressure zones 3 may be used, in which case dyeing The deposition process uses two process solvent recovery zones 4. The first process solvent recovery zone 4 may be associated with the first process solvent (hence the first process solvent application zone 2 and the first process temperature/pressure zone 3) and the second process solvent recovery zone Zone 4 may be associated with a second process solvent (hence, second process solvent application zone 2 and second process temperature/pressure zone 3). The composition, temperature, flow characteristics, etc. of the process solvent recovery zone 4 may be different for each process solvent and/or dye welding process, based at least on the desired properties of the resulting weld substrate. Therefore, these parameters do not limit the scope of the present disclosure unless so indicated in the following claims. In the light of the present disclosure, one of ordinary skill in the art will appreciate that the scope of the present disclosure is to include two process solvents, two process solvent application zones 2 and two process temperature/pressure zones 3, and/or two process solvent recovery zones 4. It will be understood that it is not limited, and extends to any number without limitation unless so indicated in the following claims.

Eleventh Exemplary Dyeing and Welding Process

In another dye welding process, the process solvent may include an aqueous hydroxide salt. Such a dye welding process may be configured to use the equipment and/or apparatus shown in FIG. 10A. For example, a process solvent containing 8 wt% lithium hydroxide, 15 wt% urea, and 2.5 wt% indigo powder is not reduced by the indigo powder (ie, the process solvent only suspends the indigo powder. , Which does not dissolve or chemically modify), and may be applied to a substrate comprising 30/1 ring spun cotton yarn. The process solvent application zone 2 and the process temperature/pressure zone 3 may be configured such that the mass ratio of process solvent to substrate is 7:1. The temperature of the process solvent application zone 2 and the process temperature/pressure zone may be kept at -12°C and the process solvent may interact with the substrate for 3-4 minutes, after which water is applied to the substrate. Then, the process solvent may be recovered to obtain a welding substrate colored with indigo. The welded yarn was rinsed with water, dried, and then subjected to the AATCC8 clocking test. The flocking resistance of this fused yarn was a rating of 1, and the test fabric exhibited a characteristic indigo blue color.

A view of a welded yarn substrate 100 that may be produced using one process solvent is shown in FIG. 17A, and from the welded yarn substrate 100, individual tightly welded substrate fibers 105 are shown in FIG. 17B. It is envisioned that the dyeing and fusing process may be configured such that the degree of fusing of the fusing yarn substrate 100 decreases radially from the outer surface of the fusing yarn substrate 100 inward. Thus, going from the outside to the inside, the firmly welded substrate fibers 105, the medium welded substrate fibers 104, the lightly welded substrate fibers 103, and the substrate fibers 102 (generally, the welded yarn substrate) One or more layers (around the center of the material 100) may be present. The degree of deposition on the welded yarn substrate 100 may be manipulated by adjusting the various process parameters described above.

Dyes and/or colorants are trapped via the binder 106 in the individual welded substrate fibers 103, 104, 105 and/or in the region between these welded substrate fibers 103, 104, 105. May be done. The optimum chemical composition of the binder 106 may vary from dye to dye deposition process and may vary depending at least on the chemical composition of the substrate. In dyeing and welding processes where the substrate comprises cotton threads, it has been found to be advantageous to configure the binder to include a biopolymer, especially when the biopolymer comprises cellulose. The binder 106 may be applied to the weld yarn substrate 100 by dissolving the binder 106 in a suitable solvent, which solvent may then be applied to the substrate or the weld substrate. In some dye welding processes, the solvent may be a process solvent having cellulose dissolved therein, such that in process solvent recovery zone 4 (eg, the reconstitution zone), binder 106 is deposited. Placed on and/or in the substrate.

Referring now to FIG. 17B, individual pigment particles 109 are shown on the outer surface of the individual fused substrate fibers 103, 104, 105 and are entrapped within the binder 106. Not only is there a radial color gradient from the outer surface to the inner portion of the welding thread base material 100 between the individual welding base material fibers 103, 104 and 105, but also among the individual welding base material fibers 103, 104 and 105. Also, there may be a color gradient that advances radially from the outer surface of the individual welded base fiber 103, 104, 105 to the inside thereof. The concentration of pigment particles 109 that engage the individual welded substrate fibers 103, 104, 105 can be greatest near their outer surface, as shown in FIG. 17B. Generally, a portion of the pigment particles 109 may be entrapped within the welded substrate fibers 103, 104, 105 and a second portion thereof may be entrapped between the welded substrate fibers 103, 104, 105. Alternatively, the third portion may be entrapped within the binder 106. The pigment particles 109 located at the farthest radial positions of the individual base fibers 103, 104, 105 (the individual base fibers 103, 104, 105 are located at the farthest radial positions of the welding yarn base 100). It is envisaged that the (positioned) may exhibit a relatively low dyefastness when compared to the other pigment particles 109.

A view of a welded yarn substrate 100 that may be manufactured using multiple process solvents is shown in FIG. 18A, and individual, firmly welded substrate fibers 105 from the welded yarn substrate 100 are shown in FIG. 18B. Here again, it is envisioned that the dyeing and fusing process may be configured such that the degree of fusing of the fusing yarn substrate 100 decreases radially from the outer surface of the fusing yarn substrate 100 toward the interior. Thus, going from the outside to the inside, the firmly welded substrate fibers 105, the medium welded substrate fibers 104, the lightly welded substrate fibers 103, and the substrate fibers 102 (generally, the welded yarn substrate) One or more layers (around the center of the material 100) may be present. The degree of deposition on the welded yarn substrate 100 may be manipulated by adjusting the various process parameters described above.

Similar to the welded yarn substrate 100 of FIG. 17A, the dyes and/or colorants of FIG. 18A can be incorporated into and/or within the individual welded substrate fibers 103, 104, 105. , 105, may be captured via the binder 106. The optimum chemical composition of the binder 106 may vary from dye to dye deposition process and may vary depending at least on the chemical composition of the substrate. In dyeing and welding processes where the substrate comprises cotton yarns, it has been found to be advantageous to configure the binder to comprise a biopolymer, especially when the biopolymer comprises cellulose. The binder 106 may be applied to the substrate by dissolving the binder 106 in a suitable solvent, which solvent may then be applied to the substrate or the welded substrate. The binder 106 may be applied to the substrate in the same step as the dye and/or colorant (eg, by mixing the indigo powder with the process solvent). In some dye welding processes, the solvent may be a process solvent having cellulose dissolved therein, such that in process solvent recovery zone 4 (eg, the reconstitution zone), binder 106 is deposited. Placed on and/or in the substrate.

The welded yarn substrate 100 shown in FIG. 18A may also include a binder shell 108 located on a radially outer portion of the substrate. The binder shell 108 may be applied to the fused yarn substrate 100 to which the dye and/or colorant and/or binder 106 has already been applied, the dye and/or colorant and/or binder 106 Application may be done by applying one or more process solvents to the substrate. In one dye welding process, the binder shell 108 may be applied by dissolving the binder 106 in a suitable solvent, which is then applied to the substrate or the welded substrate knitted yarn substrate 100. May be done. In general, in some dye fusing processes, it has been found that removal of dyes and/or colorants from the process solvent when applying the binder shell 108 can be beneficial to the dye fastness of the fused yarn substrate 100. Has been issued.

Referring now to FIG. 18B, individual pigment particles 109 are shown on the outer surface of individual fused substrate fibers 103, 104, 105 and are entrapped within binder 106. The binder shell 108 without the pigment particles 109 entrapped therein may be located around the outer surface of the fused yarn substrate 100. Such a binder shell 108 can increase the dyeing fastness of the fused yarn base material 100 as compared to the prior art. Not only is there a color gradient between the individual welded substrate fibers 103, 104, 105 that progresses radially from the outer surface to the inside of the welded yarn substrate, but also within the individual welded substrate fibers 103, 104, 105. Also, there may be a color gradient that advances radially from the outer surface of the individual welded substrate fibers 103, 104, 105 to their interior. The concentration of pigment particles 109 that engage the individual welded substrate fibers 103, 104, 105 can be greatest near their outer surfaces, as shown in FIG. 18B.

In some dye welding processes, the chemical composition of binder 106 and binder shell 108 may be similar or identical (eg, a cellulosic polymer). However, in other dye fusing processes, the binder 106 and binder shell 108 may have different chemical compositions, which may depend at least on the pigment particles, substrate, etc.

The welded yarn substrate 100 of FIG. 17A is manufactured by a dyeing and coloring process that uses the injector 60 for process solvent application, and the injector 60 may be configured similar to the method shown in FIG. 6A. Similarly, the fused yarn substrate 100 as shown in FIG. 18A may be manufactured by a dyeing and coloring process that uses the injector 60 for process solvent application. The dye fusing process configured to produce the fusing yarn substrate 100 shown in FIG. 18A uses two separate process solvents (eg, one having a dye and/or a colorant for the first application). Such an injector 60 may be used as a solvent for the second, which does not include dyes and/or colorants, and may be used for subsequent applications that apply the binder shell 108. It may be configured to have more than one process solvent inlet 62 and application interface 63. However, other structures and/or methods for applying one or more process solvents may be used without departing from the spirit or scope of the present application, unless so indicated in the following claims. ..

19A-19C are cross-sectional views of several types of welded yarn substrates that may be produced by a welding or dyeing and welding process. For brevity, the term "fusing process", as used with reference to Figures 19A-19C, is limited to the dye fusing process as well as the fusing process as previously described herein, unless otherwise specified in the claims. It includes, but is not limited to, the later-described developments that do not occur. The uniformly welded yarn base material (uniformly welded yarn base material) is shown in FIG. 19A. As used herein, the term "uniformly welded" (uniform weld) is used to indicate spatially consistent, controlled volume consolidation across the cross section of the welded yarn substrate.

The shell welded yarn substrate is shown in Figure 19B. In contrast to a uniform welded yarn substrate, a shell welded yarn substrate allows the polymer to swell and move so that the outermost fibers of a given substrate achieve intimate molecular level welding interactions and welding effects. Resulting from a tailored welding process. As a result, there may be a ring-like gradient in the fiber-welded substrate that is different from the core fibers in the substrate, and the core fibers are not significantly disturbed by the welding process.

The core welded yarn base material is shown in FIG. 19C. In the core-welded substrate (which can also be produced by the welding process disclosed herein), the biopolymer of the innermost fiber is swollen and mobilized, so that the core of the welded substrate forms intimate molecules. Although exhibiting a level of interaction gradient, the outer rings of the fiber remain largely undenatured. In Figures 19A-19C, the darker gray color indicates that the molecular level interactions between fibers are relatively large.

It is important to note that the degree of uniform, shell, or core deposition of the weld substrate has significant effects and consequences on the physical properties of the weld substrate. For example, the uniform welded yarn base material has a significant decrease in fluff while at the same time having a modulus (calculated by dividing strength/tensile strength by elongation as shown in Table 2.2, Table 3.2, etc.). May show an increase. For example, a welding base material produced by a dyeing and welding process has a modulus that is 100% greater than that of its raw yarn base material equivalent, while at the same time having a fluff of about 30% compared to its raw yarn base material equivalent. ˜99% (as measured by the Worster Hairiness Index). In contrast, the shell welded yarn substrate may show a significant reduction in fluff, but does not have as large a modulus increase as the uniform welded substrate, which is unfused, knitted and/or welded yarn substrate. This is because there is a fiber core that can slip against. Conversely, core welded yarn substrates exhibit increased modulus, while at the same time maintaining a desired amount of fluff. The ability to select, or even modulate, the properties of a uniform weld, a shell weld, or a core weld substrate is a very important aspect for producing a weld substrate knitting yarn with optimized properties for fabrics. By using an optimized welded yarn substrate with spatially controlled volume consolidation of the welded yarn substrate, surprising new fabrics can be constructed from knitting yarns containing natural fibers.

The deposition process involves the effectiveness and rheology of the process solvent and the method of application (viscosity that can occur at various suitable points while the substrate passes through process solvent application zone 2, process temperature/pressure zone 3, and process solvent recovery zone 4). With suitable control in combination with (including the amount of resistant solvent) it may be configured to produce a uniform welded yarn substrate. The extent to which consistent deposition results are obtained depends on the temperature and heating method (ie, radiative or non-radiative heat transfer or a combination thereof), atmospheric pressure, atmospheric composition, process solvent recycling in process solvent recovery zone 4. It is related to the type and method (eg, choice of reconstitution solvent type, temperature, flow characteristics, etc.) as well as the type and method of the drying process used to remove the reconstitution solvent from the substrate.

Referring now to FIGS. 19B and 19C again, showing a shell weld core and a core weld core, respectively, the weld process is illustrated by careful manipulation and control of the weld process parameters for these alternative weld bases. May be configured to manufacture. In addition, the modulated fiber deposition process, as described in detail above, modulates the substrate at least during the uniform, shell, and/or core deposition results when the key process variables are modulated in real time. To be able to do.

In general, shell deposition refers to process solvent composition (which affects solvent effectiveness, rheology, or both), process solvent application temperature and pressure, process temperature/pressure zone 3 residence time, heat transfer method. (Including but not limited to, the composition of the process solvent recovery zone 4 (reconstituted solvent composition, flow characteristics, temperature, etc.), and/or the method used for removing the reconstituted solvent, etc.) ) May be carried out by spatially limiting the welding conditions to the outside of the textile yarn substrate.

For example, shell welding may be performed by increasing the solvent viscosity so that the process solvent adheres primarily to the outer surface of the textile yarn substrate, and process solvent application zone 2 and/or process temperature/pressure zone 3 The duration and temperature of the can be adjusted to limit the extent to which the process solvent enters the substrate and is effective in swelling and mobilizing the biopolymer of the fibrous substrate. Specifically, a relatively small amount (0.02-1% by weight) of solubilized biopolymer may be added to the process solvent to achieve varying degrees and/or thickness of shell welding effect.

Core welding may be performed with all alternatives to the above conditions and/or process parameters including, but not limited to, variations in viscous drag conditions. For example, process solvent application may be performed with a suitable process solvent delivery system that limits the amount of process solvent applied, and for example, for a suitable length of time before welding occurs, when the process solvent is applied to the substrate. May be adjusted using conditions that allow it to enter the core of Particularly in this case, it is beneficial to compound the process solvent and separately control the temperature of the process solvent application zone 2 and/or the process temperature/pressure zone 3 so that the welding conditions are not achieved until the temperature reaches the appropriate range. Can be.

In another example, deposition inhibitors (eg, water, steam, etc.) are applied to the process wetting substrate (at the end of process solvent application zone 2 and/or in process temperature/pressure zone 4). In any case, the composition of the process solvent on the outer surface of the process-wet substrate may be modified (by diffusion) to affect the degree of deposition across the cross section of the substrate. That is, if the deposition inhibitor diffuses into the process solvent adjacent to the outer surface of the process-wet substrate, the deposition may be suppressed and/or stopped at that location, but the deposition still occurs within the process-wet substrate. It may be happening.

17A-19C show the separate boundaries for each of the individual weld substrate fibers 103, 104, 105 therein, although the weld process used to make the weld yarn substrate 100 or The dyeing and welding process may actually cause the boundaries between adjacent welded substrate fibers 103, 104, 105 to mix. That is, the biopolymers of the individual welded substrate fibers 103, 104, 105 may be swollen and mobilized and their individual boundaries no longer exist. Thus, adjacent weld substrate fibers 103, 104, 105 in weld yarn substrate 100 may be fused together, as detailed above.

A dye fusing process configured to at least partially dye the substrate and to use the binder 106 to at least partially engage the one or more pigment particles 109 to the substrate comprises: Sometimes referred to as the hybrid stain welding process, as briefly described in. Such a dye welding process may be configured with a process solvent comprising DMSO or DMF, wherein the process solvent may swell and mobilize the biopolymer while at the same time dissolving the desired dye and/or colorant. It is thought. A process solvent containing DMSO or DMF provides the required solubility of the indigo dye in the process solvent so that a portion of the substrate is dyed (in the traditional sense of the term). Further, in such dye fusing processes, the amount of dye and/or colorant in the process solvent may be such that the process solvent exceeds the saturation point of the particular dye and/or colorant. That is, the process solvent may be fully saturated with the dye and/or colorant, and a portion of the dye and/or colorant may be suspended in the fully saturated process solvent.

In another dye fusing process, the indigo dye may be wholly solubilized in the process solvent. In such a dye fusing process, the resulting fusing substrate may lack recognizable pigment particles 109 entrapped within the binder 106. That is, the welded substrate may be exclusively dyed in character, so that the individual welded substrate fibers 103, 104, 105 and the outer surface of each welded yarn substrate 100 are homogeneous. It becomes a color. In a dye fusing process so configured, the reconstitution solvent used in the process solvent recovery zone 4 may retain less than 10% of the amount of solubilized indigo dye in the process solvent. More specifically, the reconstitution solvent may retain less than 5% of the amount of solubilized indigo dye in the process solvent. Again, the dye fusing process may be configured to impart to the fusing substrate 100 any of the properties previously disclosed. It is envisioned that the welded substrate 100 produced by such a process may exhibit relatively high clocking resistance.

Overview of dyeing and welding process

The indigo powder may be fixed to the cotton yarn substrate using a dye welding process. The indigo powder may be bonded onto the cotton yarn substrate by a dye welding process, and the solubility of the substrate in the process solvent may be the key to retention of the pigment in the resulting weld substrate. The fact that Kelver® yarns were not appreciably dyed using this dye fusing process indicates that the pigment is not merely attached to the surface of the yarn substrate. Indigo powder can be abraded (mechanically) from the surface of the welded yarn substrate by friction, whether or not the cellulose is dissolved in the process solvent used for the dyeing and welding process. Subsequent process solvent application using a colorless process solvent containing dissolved cellulose (eg, subjecting the welded yarn substrate to another welding process) effectively immobilizes the indigo powder pigment and reduces clocking. Possible (see Table 15.1 below). In one dye welding process, DMSO is a preferred cosolvent for welding because it does not chemically reduce indigo and does not produce a green hue on the yarn when indigo is exposed to the cosolvent for a long time.

Generally, the optimum weight percent of indigo powder in a given process solvent for use in a dye welding process is limited by the cellulose (or unless otherwise indicated in the claims below) dissolved therein. It may vary from application to application, as well as the weight percentage of other binders not included). For some dye welding processes, the optimum weight percentage of indigo powder in the process solvent may be 0.25 to 8.5 and the optimum weight percentage of dissolved cellulose is 0.01 to 1.5. May be In other dye welding processes, the optimum weight percentage of indigo powder in the process solvent may be 1.0-4.0 and the optimum weight percentage of dissolved cellulose is 0.1-1.0. It may be. Accordingly, unless otherwise indicated in the claims below, the scope of the present disclosure is in no way limited by the weight percent of indigo powder in the process solvent or weight percent of cellulose dissolved therein.

D. Examination of reconstituted solvent

As mentioned above, ACN causes a chemical change in indigo, which may result in a green hue on the welded yarn substrate upon prolonged exposure, making it an ideal reconstitution solvent for certain dyeing and welding processes. Not always. Generally, when water is used as the reconstitution solvent, similar color shifts do not occur, but water may exhibit other undesirable effects, such as high drag.

Pulling the textile yarn through the process solvent recovery zone 4 (sometimes referred to as the reconstitution zone) can create a high drag force on the yarn that can exceed its breaking strength. In one dye-weld process, in a 7 foot long reconstitution zone, when water was used as the reconstitution solvent (towed through 1/4 inch PFA tubing), the yarn was up to 80 gram (gf). Experienced the drag of. In a comparative experiment, the addition of soap (0.5 wt% Murphy Oil Soap) to water reduced the drag to about 55 gf. When pure ACN was used as the reconstituted solvent, the drag dropped to about 45 gf, while when pure ethyl acetate was used as the reconstituted solvent, the drag dropped to 35 gf. However, in certain dye welding processes, pure ethyl acetate may be relatively ineffective at removing ionic liquids from textile yarns. Therefore, reconstituted solvents containing approximately 5% by weight of ethyl acetate in water have been identified because such reconstituted solvents have an effect approximately equal to pure ethyl acetate in drag reduction while maintaining the reconstitution properties of water. Can be ideal for the dyeing and welding process of

E. Effect and application

A textile yarn dyed using a method constructed in accordance with the present disclosure may exhibit various benefits as compared to a textile yarn produced by conventional means. Indigo dye deposited in a yarn in a manner constructed in accordance with the present disclosure tends to "clock" (ie, be removed by subsequent washing and/or removed by rubbing or other physical contact). Is lower. A knitted yarn produced in accordance with the present disclosure may exhibit beneficial physical properties associated with the welded outer surface, including, but not limited to, improved strength, improved smoothness. (Less fluff), shorter drying time, and better knitting characteristics. The combination of color retention and the benefits of the physical properties of the knitting yarn results in an improved fabric that is at least widely available in the denim industry.

The commercial dyeing process consumes about 125 liters of water per kg of dyed fiber. A manufacturing process constructed according to the present disclosure may significantly reduce the water required in the dyeing process. In addition, the rinse and reconstitution steps of such manufacturing processes may be designed to recover greater than 98% of ionic liquids, which may reduce the cost and environmental impact of current weld dyeing processes.

A further benefit of simultaneously welding and dyeing textile yarns is that the presence of the dye verifies a consistent welding of the textile yarn. Welding without dyes is known and has mechanical benefits, but without easy means of detection, the welding process may be inconsistent. Inclusion of the dye in the process solvent creates a textile yarn that can be easily detected by color changes if there is inconsistency in the deposition process.

10. Welding process using anti-wool substrate and resulting product

A. Anti-hair background technology

Generally, fluff is a recycling process in which textiles and other fibrous materials are disassembled or destroyed and returned to individual fibers, threads or pieces of textile. The resulting fibers can then be re-spun into yarns with similar qualities as the fibril yarns, but the re-spun yarns generally have lower strength than the corresponding fibril yarns. is there. Also, re-spun yarns often remove much more lint (often referred to as "fly") than the corresponding fibril yarns. The denim before use or after use can be fluffed (recycled) to recover individual cotton fibers, and then re-spun into another denim yarn. The fluff of the new yarn is sometimes referred to as the "up-cycled content" and may be mixed with the raw cotton fiber at a constant weight percentage during the spinning process. Denim is generally a mixture of ring-dyed indigo warp yarns and undyed weft yarns, while yarns made from some of the fluff fibers are light blue with a very variable color. As used herein, the terms "refurbished" and "recycled" are used interchangeably without limitation or restriction, unless expressly specified in the claims. Further, the advantages and improvements described below are short or medium (as defined below) regardless of the source of the fiber (eg, fluff, recycled, virgin, etc.), unless otherwise specified in the claims. Applies to any yarn and/or fabric having at least a portion of staple fibers of length.

The loss of strength in the fluff (recycled) yarn compared to an equivalent yarn made from fibrils may be due to the reduced staple fiber length that occurs during the fluff (recycle) process. Therefore, a method of improving yarn strength without resorting to the addition of fibrils or the removal of particularly short fibers is desired. In addition, fluff (recycled) yarns generally exhibit a variegated (and generally bright) color, so that the yarns are evenly colored, without any secondary dyeing, color (eg saturation) and darkness. There is a demand for a method of improving the conversion.

Generally, short staple fibers may be defined herein as staple fibers having a length of 0.25 to 0.99 inches, medium length staple fibers having a length of 1.00 to 1.10 inches. Staple fibers having a length of 1.11 to 1.26 inches, long staple fibers having a length of 1.11 to 1.26 inches, and ultra-long staple fibers having a length of 1.27 to 2.00 inches. May be defined as staple fibers having a toughness. Generally, fluffed, recycled and/or up-cycled fibers have short staple fiber lengths, combed high up cotton yarns have long staple fiber lengths, and Suupima cotton yarns have very long staple fiber lengths. Often. Of course, not all fibers are neatly classified into any of the above length categories. Therefore, when referring to the staple fiber length of a yarn as defined herein, the staple fiber length means the average value of the staple fiber length of the yarn. Further, the symbols for referring to the yarns used above (for example, "30/1" indicates a single yarn of 30 weights and "26/2" indicates a double yarn of 26 weights) are as follows. Also used.

There are at least three major limiting factors that determine when and how cotton with short staple fibers (short staple fibers obtained from up-cycle material, fluff material, etc.) is returned to the woven fabric. Factors are (1) spinning technology restrictions, (2) textile construction restrictions, and (3) trading restrictions. These limits are shown in the graph of FIG. Plot the percentage of short staple fibers ("Up Cycle Content (%) on the Y axis") against yarn weight on the X axis. One line shows spinning technology limits, another one shows textile construction efficiency limits, and the last one shows trade limits. The following summary of each limitation is not exhaustive, but discloses various deficiencies in the prior art that may be overcome by the methods and/or apparatus described herein.

Restrictions on spinning technology (dotted line at the top of Figure 24)

The fibers obtained from fluff fabrics for industrial use and after use are much shorter than the fibrils. In general, staple fibers weaken spun yarns, which are more prone to breakage and produce unwanted lint and debris (also known as "fly") during their handling, especially during the construction of textiles. It In fact, too much short fiber content can cause problems for spinning machines for making spun fiber yarns. For relatively light and thin yarns (eg 60/1 NE cotton yarn towards the left in Figure 24) the inclusion of short staple fibers can cause damage to the spinning machine and limit the production of these yarn substrates. Absent. For relatively heavy overlapping yarns (eg, 60/1 NE cotton yarn to the right of Figure 24), it may be possible to spun yarn from 100% short staple fibers, but such yarns are not manufactured and obtained. Both fabrics have significant performance drawbacks. The absolute amount of short fibers that can be used during spinning depends on the fiber length histogram, the spinning machine used, and the operating parameters of the chosen spinning technique. The dotted line in FIG. 24 shows the upper limit of what is possible with the currently available technologies.

Restrictions on fabric construction (dotted line in the center of Fig. 24)

Generally, spun yarns containing fibers obtained from industrial and post-use fluff fabrics are very weak and subject to failure in fabric construction, either by knitting (eg warp and weft) or by weaving. In addition, a significant increase in problems due to increased lint has been observed and must be dealt with when short fiber spun yarns are converted into fabrics by knitting and weaving machines. This includes connecting and breaking the sewing needle and thread guide, cutting and reconnecting thread, and the like. In general, all of the problems caused by lint-producing weak yarns increase manufacturing costs and reduce manufacturing speed.

Another problem is the yarn "torque" problem. While yarn strength generally increases with increasing twist per unit length, densely spun yarn also has a greater tendency to "untwist" (known as "torque"), which results in fabric bending. Can cause defects in certain types of fabrics called. Distorted fabric is generally defined as the weft threads being parallel to each other but not perpendicular to the width of the fabric. This defect often occurs when the torque of the yarn is too high. In short, spun yarns made of extremely short fibers are often made with higher (per unit of length) twists, resulting in higher torques that can cause unnecessary weave bowing. Will cause it.

Trading restrictions (dotted line at the bottom of Figure 24)

In addition to the technical limitations described above, the limited opportunities to manufacture and sell fabrics containing short (up-cycle) products are due to various commercial reasons. Many functional fabrics that require the use of thin yarns, if any, cannot be made with yarns that are rich in short staple fibers, as thin yarns containing so many upcycles are not available. .. In addition, woven fabrics made from yarns that produce staple fibers are prone to pilling and poor wear resistance. These factors (and others) at the same time create an environment in which many products that can utilize up-cycle products suffer too much degradation in performance compared to economic or market benefits.

B. Examples of welding process and resulting products

The boundary between the “textile construction” and “transaction” restrictions in FIG. 24 is currently relatively small. This is consistent with the fact that few products are manufactured and sold today that use important industrial and/or post-consumer goods. It is well known that technical solutions that can increase the content of short staple fibers in yarns (and the resulting fabrics) to a much greater extent are very advantageous and beneficial to the environment.

Weld yarns containing more staple fiber than is possible today in the prior art can use the welding process disclosed herein. Fused yarns are generally stronger and/or thinner than their raw yarn counterparts. Moreover, because the weld yarns generally have less torque, fabrics made from the weld yarns will not have the fabric bowing problems associated with conventional raw yarns. The use of fusible threads allows for more efficient and faster fabric construction (eg by knitting or weaving) while producing superior fabrics with unprecedented thinness and durability (eg pilling resistance) at the same time. It is possible. Various other advantages, attributes and/or properties of the welded substrates described hereinabove are provided by the welding process utilizing a green substrate comprising short staple fiber yarn 110, unless otherwise specified in the claims. It depends on the obtained welding base material. Since the fusible yarn has few restrictions on fabric construction, the fusible yarn can fill the range of opportunities close to the restrictions on the spinning technology, and is indicated by the shaded portion in FIG. Fused yarns represent a significant advance in using short, natural staple fibers of textiles (eg, cotton, silk, etc.).

The welding process described hereinabove has been found to be particularly useful in improving the low strength of anti-wool yarns, the results of which are applied to yarns made from fibrils. Consistent with the above observations on the welding process disclosed in the publication. For the sake of brevity, the term "fusing process" as used in reference to Figures 20A-28B is limited to the dyeing and fusing processes as well as the fusing processes previously described herein, unless otherwise specified in the claims. It includes, but is not limited to, the developments described below that are not done.

Surprisingly, when the fusing process is performed on short staple fiber yarn 110 containing denim fibers made from fluff denim waste, the fusing yarn is suitable as a warp for denim without the need for additional dyeing. A welded yarn substrate is obtained which exhibits a uniform color of the yarn, increased saturation and darkening of the color of the welded yarn.

During the fusing process, partial dissolution of the indigo-dyed fibers present in the short staple fiber yarn 110 (eg, the raw yarn substrate) redistributes the dye around and throughout the substrate, resulting in hairs. Partial compaction and reduction may eliminate interfaces that may cause light diffraction, while improving the uniformity of dye distribution and thus increasing saturation and resulting welded yarn. Thicken 111. The resulting improvements in color uniformity, darkening, and increased saturation of the welded yarn 111 and the strongly associated improvements were applied to the short staple fiber yarn 110, which had never been disclosed or anticipated. It is attributed to the welding process. This set of beneficial attributes may be applied to any short staple fiber yarn 110 that is subjected to the welding process as disclosed herein without limitation, unless otherwise indicated in the appended claims.

The fusing process configured for use with the raw substrate comprising short staple fiber yarn 110 may be any suitable fusing process, including ionic liquid based process solvents, cold alkaline processes including NaOH or LiOH. Examples include, but are not limited to, those disclosed herein using a solvent or process solvent including onium hydroxide. In the two embodiments described below with reference to FIGS. 20A-22, the short staple fiber yarn 110 comprises 50% by weight of 20/1 ring spun yarn of unused combed high cotton fiber and 50% by weight of fluff. Made of wool denim fiber. However, these embodiments are for illustrative purposes only and in no way limit the scope of the present disclosure, unless expressly specified in the appended claims.

Referring now to FIGS. 20A-22, typically a substrate comprising raw short staple fiber yarns 110, one of which is shown in FIG. 20A, is a process device that applies a process solvent to the substrate. Is supplied to. This step may constitute the process solvent application zone 2 of the deposition process, as detailed above. The substrate may then move through the process temperature/pressure zone 3 (or "fusion zone") after which the substrate enters the process solvent recovery zone 4 (or "reconstitution zone") The welding process may stop within 4 and the process solvent may be recovered. Various aspects of a suitable welding process have been described in detail above, but are not repeated here for the sake of brevity. It has been surprisingly found that the process solvent does not remove the dye from the substrate during the deposition process, but instead only partitions the dye around and in the substrate. That is, the process solvent removed during the reconstitution step is not itself colored, but rather the dye remains in the yarn substrate.

In one embodiment, the substrate containing short staple fiber yarns 110 may be fed to a process solvent application zone 2 that applies a process solvent containing an ionic liquid to the substrate. As detailed above, the process solvent may be applied to a liquid containing a co-solvent that enhances the welding effect. Suitable ionic liquids include, but are not limited to, 1-ethyl-3-methylimidazolium acetate (“EMIm OAc”), 1-butyl-3-methylimidazolium chloride (“BMIm Cl”). , 1-Ethyl-3-methylimidazolium diethylphosphate (EMIm DEP), 1-allyl-3-methylimidazolium chloride (AMImCl) and similar imidazole-type ions unless otherwise specified in the claims. A liquid can be mentioned. Suitable co-solvents for such ionic liquids include dimethyl sulfoxide (DMSO), dimethylformamide (DMF), acetonitrile (ACN) and 1-methylimidazole.

Again, as detailed above, the short staple fiber yarn 110 (base material) to which the process solvent is applied enters the process temperature/pressure zone 3 where a portion of the short staple fiber yarn 110 melts. In a deposition process configured to use a process solvent composed of an ionic liquid, the process temperature/pressure zone 3 may be heated to a temperature of 50°C to 120°C. The residence time of the substrate in the process temperature/pressure zone 3 may be between 2 and 60 seconds. The substrate enters the process solvent recovery zone 4 before it completely dissolves. Here, the welding process may be stopped by using a cellulosic anti-solvent that removes the process solvent from the substrate. In a deposition process configured to use a process solvent containing an ionic liquid, the reconstituted solvent may be water (or water based), or based on an alternative solvent that is easier to recover the ionic liquid. Is also good. The substrate then proceeds to the drying zone 5 and/or the welded substrate collecting zone 6 where the welded yarn 111 is dried and/or collected.

In another embodiment of the fusing process configured to utilize a substrate comprising short staple fiber yarn 110, short staple fiber yarn 110 is fed to process solvent application zone 2 where process solvent including cold alkaline solution is added. Applied to the substrate. Cold alkaline process solvents generally contain a suitable base such as NaOH or LiOH, as described in more detail above. Other additives can be added to the cold alkaline process solvent to make the process solvent system and improve the effectiveness of the process solvent. Such additives include, but are not limited to, urea, thiourea, polyethylene glycol surfactants, cyclic crown ethers and/or zinc oxide, but not otherwise specified in the appended claims. As long as it is not limited.

One exemplary process solvent system contains about 9 wt% LiOH and about 16 wt% urea in aqueous solution. The substrate treated with the cold alkaline process solvent solution passes through the process temperature/pressure zone 3 where it is partially dissolved and migrates. The process temperature/pressure zone 3 may be cooled to a temperature of -17°C to -5°C. The residence time of the substrate in the process temperature/pressure zone 3 is 40 seconds to 345 seconds.

The substrate moves to the process solvent recovery zone 4 before the substrate is completely dissolved. At that stage, the welding process may be stopped by increasing the temperature and removing the process solvent solution. Suitable reconstitution solvents can include water (or aqueous liquids), but are not limited to these unless explicitly stated in the claims, and the alkaline component of the process solvent system can be readily recovered. Alternative solvents can be based. Next, the base material moves to the welding base material collecting zone 6 and/or the solvent collecting and collecting zone 7, where the welding yarn 111 is dried and/or collected. The welded yarn 111 made in accordance with this embodiment of the welding process has a strength improvement of about 50% compared to the raw short staple fiber yarn 110, as shown in FIG. 22 and as further described below. showed that.

20B and 21B are diagrams of a green substrate including a welded yarn 111 and a short staple fiber yarn 110 made by a welding process using a process solvent containing a hydroxide. The welded yarn 111 made according to this embodiment of the welding process showed a strength improvement of about 50% compared to the raw short staple fiber yarn 110. 20C and 21C are diagrams of a green substrate including a weld yarn 111 and a short staple fiber yarn 110 made by a welding process using a process solvent containing an ionic liquid. The welded yarn 111 made according to this embodiment of the welding process showed a strength improvement of about 50% compared to the raw short staple fiber yarn 110.

A graph showing this increase in strength due to the welding process is shown in FIG. In FIG. 22, a raw short staple fiber yarn 110 sample (shown in FIGS. 20A and 21A), a welded yarn 111 (made from a raw short staple fiber yarn 110 substrate using a process solvent containing hydroxide). 20B and 21B) and elongation of the tensile strength (cN/dtex) of a welded yarn 111 (FIGS. 20C and 21C) made from a raw short staple fiber yarn 110 substrate using a process solvent containing an ionic liquid. It is plotted against rate.

Continuing to refer to FIG. 22, the improvement in strength observed in the welded substrate can be achieved with any green substrate having relatively short staple fibers, unless otherwise specified in the claims. It is not limited to raw substrates including 110. This strength improvement, normalized to strength per cross-sectional area, is often observed at the same time by performing the welding process on the 1D yarn base material, as will be described in more detail below. It becomes more remarkable by the reduction of.

C. First example of strength improvement

In the first experiment, a raw yarn base material composed of 50% fluff denim fiber and 50% raw cotton fiber was subjected to open-end spinning to obtain a 20/1 Ne heavy yarn. This raw yarn substrate is processed in the welding process using the following parameters.

1. The process solvent mixed with EMIm OAc and DMSO at 30 wt% and 70 wt% respectively was applied to the yarn base material at an application rate of 4 times the weight of the raw yarn base material.
2. The substrate was drawn through a 2 m long weld column (ie, process temperature/pressure zone 3) at a rate of 12 m/min.
3. The deposition column was maintained at a temperature of 80° C. and had tubular passages that exhibited viscous resistance to the substrate.
4. The substrate was reconstituted with water at about 50° C. and a tension of about 35 g (ie, applied to process solvent recovery zone 4).
5. The substrate was finish washed and dried.

The raw yarn base material used in this experiment had a diameter before welding of 0.32 mm, a strength of 270 cN (9.2 cN/tex) and an elongation of 6.7%. The resulting welded yarn substrate produced according to this experiment exhibited a post weld diameter of 0.20 mm, a strength of 380 cN (12.7 cN/tex) and an elongation of 4%. Considering the diameters of the raw yarn base material and the fused yarn base material, the strength of the raw yarn base material is 34 MPa and the modulus is 0.5 GPa. The strength of the fused yarn base material is 118 MPa and the modulus is 3.0 GPa.

The raw yarn substrate and the fused yarn substrate of this experiment were subjected to a dry clocking test according to AATCC Test Method 8-2007. A sample of the base yarn base material is shown in FIG. 23A, and a sample of the welded yarn base material is shown in FIG. 23B. The raw yarn substrate showed a 3-4 clocking measurement. The fused yarn substrate showed a 4-5 clocking measurement (although the fused yarn substrate color is actually darker than the original yarn substrate color).

D. Second example of strength improvement

In the second experiment, a raw yarn base material containing 100% of raw pima fiber was ring spun to obtain a 30/1 Ne heavy yarn. This raw yarn substrate is processed in the welding process using the following parameters.

1. The process solvent mixed with EMIm OAc and DMSO at 30 wt% and 70 wt% respectively was applied to the yarn base material at an application rate of 5 times the weight of the yarn base material.
2. The substrate was drawn through a 2 m long deposition column (ie, process temperature/pressure zone 3) at a rate of 18 m/min.
3. The fusing column was maintained at a temperature of 95°C and had tubular passages that exhibited viscous resistance to the substrate.
4. The substrate was reconstituted with water at about 50° C. and a tension of about 35 g (ie, applied to process solvent recovery zone 4).
5. The substrate was finish washed and dried.

The raw yarn base material used in this experiment had a diameter before welding of 0.22 mm, a strength of 350 cN (17.8 cN/tex) and an elongation of 6.1%. The resulting welded yarn substrate prepared according to this experiment exhibited a post weld diameter of 0.15 mm, a strength of 340 cN (17.3 cN/tex) and an elongation of 4.3%. Considering the diameters of the raw yarn base material and the welded yarn base material, the strength of the raw yarn base material is 89 MPa, and the modulus is 1.5 GPa. The strength of the welded yarn base material is 197 MPa and the modulus is 4.6 GPa.

Comparing the first and second experimental results described above, a raw yarn substrate made from substantially short staple fibers generally contains long staple fibers when treated by a welding process. It can be seen that a welded yarn base material having a significantly increased strength per weight, strength per cross-sectional area and modulus as compared to the case where the welding process is applied to a base material containing Table 16.1 below summarizes this information.

In other experiments, short staple fiber yarn 110 was found to have a strength of less than 8 cN/tex. For example, the strength of 26/1 composed of 70% by weight of raw cotton and 30% by weight of anti-wool fiber is 7.3 cN/tex, and the strength of the welded yarn 111 after the welding process treatment is Although it was reduced by 50% or more compared with the base material, it exceeded 11 cN/tex. Furthermore, the elongation at break of the welded yarn 111 exceeded 3%. In another experiment, the diameter of the welded yarn 111 was reduced by 30% compared to the raw yarn base material.

It has also been found that treating the green substrate by a welding process increases the density of the weld yarn 111 compared to the density of the green substrate. For example, the density of raw cotton is approximately 1.55 g/cc, while the effective density of raw short staple fiber yarn 110 is approximately 0.36 g/cc and that of raw pima yarn is approximately 0.53 g/cc. To determine the density, one simply finds the average cross-sectional area (based on various diameter measurements) and calculates the density of the yarn of a particular length. After welding, the effective density of the welded yarn 111 made of raw short staple fiber yarn is about 0.92 g/cc, whereas the effective density of the welded yarn 111 made of the original pima yarn is about 1. It is 13 g/cc.

Therefore, by testing the density and strength of the weld yarn 111, it is possible to determine whether the weld yarn 111 was made by welding a substrate containing short staple fiber yarn 110. If the fusing yarn 111 is made by fusing a base material including the short staple fiber yarn 110, the fusing yarn 111 has a density of 0.5 to 1.0 g/cc and a strength of 10 to 15 cN/tex. It is expected to be. These values show that the welded yarn 111 made from the raw yarn base material containing medium, long or ultra-long staple fiber exhibits a strength exceeding 15 cN/tex as described above, so that the base material containing the short staple fiber yarn 110 is used. Peculiar to the welded yarn 111 produced from. Inspection of the weld yarn 111 for fusing the individual fibers can determine the extent of the weld (eg, mild, moderate or highly welded).

Table 16.2 shows experimental data for various weld yarns 111 made by the welding process configured to use a substrate that includes short staple fiber yarn 110. Various welding processes were carried out on three different raw yarn substrates, (1) 26/1 open-end spinning short staple fiber yarn 110 (referred to as "up-cycle yarn" in Table 16.2), (2) 30/1 ring spinning. This was done for the combed high ground yarn and (3) 30/1 pima yarn. The measured raw yarn control values for each attribute are shown in Table 16.2 below the experimental data recorded for the fused yarn 111.

As shown in FIG. 16.2, the densities of all the welded yarns 111 were significantly increased as compared with the corresponding base yarn base material. In addition, in all of the welded yarns 111, the strength was improved as compared with the corresponding base yarn base material. However, the welded yarn 111 made from the base material containing the short staple fiber yarn 110 is far more than the corresponding original yarn base material than the increase in the relative strength by the welded yarn 111 made from the base material containing highland or pima yarn. Showed a high relative strength improvement. In addition, the strength of the welded yarn 111 made from the base material including the short staple fiber yarn 110 shows a significant strength increase over the corresponding base yarn base material, but the strength of the welded yarn 111 is the same as that of the raw high ground yarn. It is equivalent and lower than the strength of the original pima yarn.

As described above in connection with Figures 15A and 15B, the welding process may be configured to control the amount of cellulose I crystals converted to cellulose II crystals. Generally, cellulose I crystals are considered unmodified cellulose crystals, and raw cotton generally has an amount of cellulose I crystals of at least 65% by weight of a given sample of raw cotton. When the welding process is carried out, the amount of cellulose I crystals in the cotton is reduced and the amorphous cellulose and cellulose II crystals are increased. Accordingly, the weld yarn 111 is recognized as having, without any limitation, less than 75% by weight of Cellulose I crystallite per given sample, unless otherwise specified in the claims, and otherwise given. Recognized to have less than 70% by weight of Cellulose I crystals per sample, and in yet other cases recognized to have less than 65% by weight of Cellulose I crystals per sample, and in other cases to a predetermined amount. It is recognized as having a Cellulose I crystal content of less than 60% by weight per sample.

Here, the strength increase (Y axis on the left side) and the strength increase per cross-sectional area (Y axis on the right side) that occur when the raw yarn base material is treated by the three different welding processes disclosed herein are displayed in a graph. With reference to FIGS. 25A-25C, it can be readily observed that the increase in measured value for both strength metrics is greatest in the green substrate containing short staple fiber yarn 110 (“up cycle”). Labeled Figures 25A-25C, leftmost column). In the graphs shown in FIGS. 25A-25C, the left Y-axis corresponds to the solid bar and the right Y-axis corresponds to the linear bar. The data used to build the graphs shown in Figures 25A-25C are shown in Table 16.3.

In general, the three graphs shown in Figures 25A-25C represent the three different degrees of deposition described above. FIG. 25A shows experimental data for a raw substrate treated by a welding process configured to highly weld the substrate (also referred to as hard welding). Accordingly, FIG. 25B shows experimental data for a raw substrate treated by a welding process configured to moderately weld the substrate (also referred to as medium welding), and FIG. 25C shows the substrate 7 shows experimental data for a raw substrate treated by a welding process configured to lightly weld (also referred to as soft weld).

Highly welded and medium welded base material data shown in FIGS. 25A and 25B respectively show three types of raw yarn base materials, (1) a raw yarn containing short staple fibers, and (2) combing. The present invention is applied to a raw yarn containing the above-mentioned highland fiber and (3) a raw yarn containing pima fiber. No data is available for a raw yarn substrate containing pima fibers that have been subjected to a welding process configured to produce a lightly welded substrate (see Figure 25C). A 26/1 ring spun cotton yarn consisting of 70% by weight of raw high cotton and 30% by weight of fluff cotton was used as the yarn containing short staple fibers used in three experiments on three different welding processes. The yarn containing the combed upland fibers was 30/1 ring spun and the yarn containing the pima fibers was also 30/1 ring spun. However, the scope of the present disclosure is not limited to the particular proportions, types, percentages, compositions, etc. of the fluff fibers and/or fibrils, unless otherwise specified in the following claims. Instead, these examples and data show that a welded substrate obtained by treating a raw substrate containing short staple fibers with the welding process disclosed herein is more dramatic than the corresponding raw substrate. Compared to the attributes obtained when a raw substrate that is strong, thinner, and has medium, long and/or ultralong fibers is treated with the welding process disclosed herein, it should be noted that it is stronger and thinner. Showing. That is, for a particular deposition process and raw substrate, unless otherwise specified in the claims, without any limitation, the lower the general properties of the raw substrate, the less the deposition process disclosed herein. The improvement realized by treating the raw substrate with

In general, the ability to make raw substrates containing short staple length fibers may be limited according to the discussion above with reference to FIG. Applicants have found that polyester carrier fibers are often used to increase the weight percentage of recycled cotton (ie, the weight percentage of short staple fibers) in a given yarn. However, the present disclosure may eliminate the need for synthetic or any other carrier fiber. Generally, in addition to the yarns disclosed herein above, Applicants have found that a raw substrate comprising 6/1 yarns composed only of fluff fibers (ie short staple fibers), 50% by weight. 20/1 yarn containing 50% by weight of raw highland cotton fiber and 50% by weight recycled denim as raw materials, 26/1 yarn containing 70% by weight of highland cotton fiber and 30% by weight of anti-wool fiber, 50 As a result of the welding of 30% yarn containing 50% by weight of raw high cotton fiber and 50% by weight of fluff fiber, the same improvement in strength and strength per cross-sectional area as the raw substrate was found. Again, unless otherwise specified in the claims, the scope of the present disclosure is not limited to the particular proportions, percentages, configurations, etc. of roving fibers and/or fibrils. Instead, these examples and data show that a welded substrate obtained by treating a raw substrate containing short staple fibers with the welding process disclosed herein is more dramatic than the corresponding raw substrate. Compared to the attributes obtained when a raw substrate that is strong, thinner, and has medium, long and/or ultralong fibers is treated with the welding process disclosed herein, it should be noted that it is stronger and thinner. Showing.

E. Improving the color of the welding substrate

The fusing process performed in accordance with the present disclosure can result in a fusing yarn 111 substrate that exhibits both reduced yarn diameter and reduced yarn hairiness (as shown by a comparison of at least FIGS. 21A-21C). In addition, the fusing process configured to use a process solvent that includes an ionic liquid has a saturation and darkening of the fusing yarn 111, as shown by at least the comparison of FIGS. 20A-20C and the comparison of FIGS. It has been found to be particularly effective in increasing This change in saturation and darkening can be achieved without the need for additional dyes or other color-enhancing additives, but it is short staple fiber with some fibers containing some of the dye. This is the result of performing the welding process on the yarn 110.

This finding of dye enhancement in short staple fiber yarn 110 applies not only to one-dimensional substrates (eg, yarns), but also to two-dimensional (eg, fabrics, panels, mats, etc.) and three-dimensional substrates. That is, a minimum or partially or completely reduced size (up to staple fibers) recycled fabric is placed on the panel and applied to a welding process configured for such substrates. It has been found that the fusing process substantially increases the saturation and darkness in two-dimensional and three-dimensional substrates, similar to the increase in saturation and darkness observed in the short staple fiber yarn 110 described above. Was issued.

Quantitatively, short staple fiber yarn 110 made from denim can have a global average color in the following L ^* C ^* h ^* color space.
L ^* =40-60 (bright thread)
C ^* =3-12 (low saturation)
h ^* =250°-310° (Indigo color)
(See also Figures 20A-20C and 21A-21C)

Weld yarn 111 obtained from short staple fiber yarn 110 (weld yarn 111 shown in FIGS. 20B and 21B) treated by the welding process disclosed herein configured to use a process solvent that includes hydroxide. , The luminance L ^* shifts to the dark side by 2 to 6 units, the saturation C ^* shifts to the side of 0 to 5 units, and the hue h ^* changes little or not. A fusing yarn 111 obtained from a short staple fiber yarn 110 (fusing yarn 111 shown in FIGS. 20C and 21C) that has been treated by the fusing process disclosed herein configured to use a process solvent that includes an ionic liquid. , The luminance L ^* shifts to the dark side by 20 to 40 units, the saturation C ^* shifts to the side of 2 to 10 units, and the hue h ^* changes little or not.

In one set of experimental data, the short staple fiber yarn 110 had an initial global average color of L ^* C ^* h ^* =(52,8,304°), as analyzed by image processing of the taken short staple fiber yarn 110. Indicated. When treated by the welding process disclosed herein configured to use a process solvent with hydroxide (fused yarn 111 shown in FIGS. 20B and 21B), the resulting fused yarn 111 has L ^* Image processing analysis of the imaged weld yarn 111 at C ^* h ^* =(50,8,299°) showed a global average color. When treated by the welding process disclosed herein configured to use a process solvent with an ionic liquid (fused yarn 111 shown in FIGS. 20C and 21C), the resulting fused yarn 111 has L ^* C ^* h ^* =(23, 11, 294°) imaged analysis of the imaged welded yarn 111 showed a global average color.

Referring now to FIGS. 26A and 26B, which are photographs of fabrics knitted from 30/1 highland yarn and fabrics welded with 30/1 highland yarn, both fabrics were dyed at 35° C. for 30 minutes and then the standard Machine washed and tumbler dried. The welding process of the welded yarn was configured to use a process solvent having a solution of EMIm OAc and DMSO in a weight ratio of 30:70, and the substrate was welded to a 2 m long weld column (ie process temperature/pressure zone). It was pulled through 3) at a speed of 12 m/min. The deposition column was maintained at a temperature of 82.5°C and had tubular passages that exhibited viscous resistance to the substrate. With particular reference to FIG. 26A, the woven fabric made from the raw yarn substrate exhibits L ^* C ^* h=(51.39, 48.63, 143.00°). In contrast, as shown in FIG. 26B, the fabric made with the welded yarn substrate exhibits L ^* C ^* h=(46.90, 44.95, 146.89°).

Referring now to FIGS. 27A and 27B, which are photographs of the fabrics shown in FIGS. 26A and 26B, respectively, after the pilling test, the fabric constructed from the welded yarn (shown in FIGS. 26B and 27B) is It can be observed that it performed in a very good way compared to the constructed fabric (shown in Figures 26A and 27A). The pilling test was ASTM D4970-a standard test method for pilling resistance of woven fabrics and other relevant surface changes: a Martindale tester was used and each fabric was subjected to 1,000 rub cycles. After the pilling test, fabrics made from the raw yarn substrate show significant pilling and L ^* C ^* h=(46.95, 43.46, 142.68°). In contrast, the fabric made from the fused yarn substrate showed little or substantially no pilling, as shown in Figure 27B, with L ^* C ^* h = (43.81, 41.61, 145.81. °).

28A is a photograph of a 20/1 ring spun yarn composed of 50% raw high-grade cotton fiber and 50% recycled denim fiber (that is, short staple fiber) and a fused yarn using the raw yarn as a base material. FIG. And 28B, it is observed that the color characteristics of the fused yarn are excellent (FIG. 28B). As shown in FIG. 28A, the raw yarn showed L ^* C ^* h=(53.18, 55.62, 286.87°). In addition to having a small amount of hairs and a small diameter, the welded yarn shown in FIG. 28B exhibited L ^* C ^* h=54.66, 68.18, 290.86°).

The fusing processes described and disclosed herein (and the fusing dyeing process, without limitation unless otherwise specified in the claims) may be configured to use a substrate comprising natural fibers. However, the scope of the present disclosure, any discrete process steps and/or their parameters, and/or the apparatus for use in the process are not so limited and are set forth in the following claims. Unless otherwise limited, it is extended to its beneficial and/or advantageous uses.

The materials used to construct the equipment and/or its components of a particular process will vary depending on its particular application, but may be polymers, synthetic materials, metals, metal alloys, natural materials, and/or It is envisioned that these combinations may be particularly useful in some applications. Accordingly, the elements described above may be constructed of any material known or later developed by one of ordinary skill in the art, which material, unless otherwise indicated in the claims below, has the spirit and scope of the disclosure. It is suitable for the particular application of the present disclosure without departing from it.

While preferred aspects of various processes and apparatus have been described, other features of the present disclosure, as well as numerous modifications and variations of the embodiments and/or aspects illustrated herein, will no doubt become apparent to those skilled in the art. , All of which may be implemented without departing from the spirit and scope of this disclosure. Accordingly, the methods and embodiments illustrated and described herein are for purposes of illustration only, and the scope of the present disclosure includes various benefits and advantages of the present disclosure unless the claims below are so indicated. And/or extend to all processes, devices, and/or structures to provide features.

The fusing process, dye fusing process, process steps, components thereof, apparatus therefor, and fusing substrate according to the present disclosure have been described in connection with the preferred aspects and examples, but not in the embodiments and/or herein. Aspects are intended in all respects to be illustrative rather than restrictive, and thus are not intended to limit the scope of the present disclosure to the particular embodiments and/or aspects described. Absent. Accordingly, the processes and embodiments illustrated and described herein are not intended to limit the scope of the disclosure in any way, unless so indicated in the following claims.

Although some of the drawings are drawn to scale, any dimensions given herein are for illustration purposes only and do not limit the scope of the present disclosure unless so indicated in the following claims. It is not limited. The welding process, the apparatus and/or the equipment therefor, and/or the welding substrate produced thereby are not limited to the particular embodiments illustrated and described herein, and are inventive according to the present disclosure. It should be noted that the range of features is defined by the following claims. Those skilled in the art will make modifications and variations to the described embodiments without departing from the scope and spirit of the invention.

Various features, components, functions, advantages, aspects, configurations, process steps, process parameters, etc. of the welding process, any of the dyeing and welding processes, process steps, substrates, and/or welding substrates, their features, components , May be used alone or in combination with another, depending on compatibility with features, advantages, aspects, configurations, process steps, process parameters, etc. Therefore, there are almost limitless variations of the present disclosure. Modifications and/or substitutions of one feature, component, function, aspect, configuration, process step, process parameter, etc., to another, unless otherwise indicated in the claims below, are within the scope of the disclosure. Is not intended to be limited.

It is understood that the present disclosure extends to all alternative combinations of one or more of the individual features disclosed, apparent from the text and/or figures, and/or essentially disclosed. All of these different combinations constitute various alternative aspects of the present disclosure and/or its components. The embodiments disclosed herein describe the best known modes for practicing the devices, methods, and/or components disclosed herein, and which other persons skilled in the art can use. Is possible. The claims should be construed to include alternative embodiments, to the extent permitted by the prior art.

Unless specifically stated in the claims, any process or method described herein is not intended to be construed to require that the steps be performed in a particular order. Therefore, if a method claim does not actually list the order in which the steps should be followed, or if there is no indication in the claims or the description to be limited to a particular order, the order may be inferred at any point. Not intended. This provides all possible implied grounds for interpretation, including but not limited to: logical arrangement of process steps or operational flow; explicit meaning derived from grammatical construction or punctuation; The number or type of the embodiments described in the specification.

List of embodiments of methods, processes, and apparatus for making dyed and deposited substrates

1. A fused cellulosic yarn having an effective yarn density of 0.5 g/cc to 1.0 g/cc and a strength of the fused yarn of 10 cN/tex to 15 cN/tex.
2. A weld yarn according to embodiment 1, having all of the disclosed features and structures separately or in combination, wherein the weld yarn utilizes a welding process from a raw substrate having short staple fiber yarns. A fused yarn, which is further defined as produced by
3. A weld thread according to embodiment 1 or 2 having all of the disclosed features and structures separately or in combination, wherein the weld process for making the weld thread further comprises an ionic liquid based process solvent. A fused yarn that is configured for use.
4. A welded yarn according to embodiments 1-4, having all of the disclosed features and structures separately or in combination, and further wherein said welded yarn has a Cellulose I crystal structure of less than 65 weight percent (%). , Welding thread.
5. A welded yarn according to embodiments 1-4, having all of the disclosed features and structures separately or in combination, and further wherein said welded yarn has a Cellulose I crystal structure of less than 60 weight percent (%). , Welding thread.
6. A method for producing a fused yarn,
a. Preparing a raw substrate, said raw substrate comprising short staple fiber yarns;
b. Applying a process solvent to the substrate to make a process wet substrate, wherein the process solvent swells and mobilizes at least one polymer in the substrate;
c. At least controlling the temperature and time at which the process solvent interacts with the process wet substrate; and d. A method comprising removing at least a portion of the process solvent from the process wet substrate.
7. The method according to embodiment 6, further comprising all of the disclosed features and structures, separately or in combination, and further wherein said short staple fiber yarn has an average short staple fiber length of less than 1.00 inches. A defined method.
8. A method according to embodiment 6 or 7, further defined as having all the disclosed features and structures separately or in combination, further wherein said short staple fiber yarn has at least 5% by weight of fibrils. The method wherein the remainder of the short staple fiber yarn is made from short staple fibers.
9. The method according to embodiments 6-8, having all of the disclosed features and structures separately or in combination, further wherein the welded yarn has a strength of at least 20 percent (%) greater than the short staple fiber yarn. A method of showing an increase in
10. The method according to embodiments 6-9, having all of the disclosed features and structures, separately or in combination, wherein the fusible yarn has at least 50 percent (%) more breaks than the short staple fiber yarn. A method of exhibiting increased strength per area.
11. The method according to embodiments 6-10, further defined as having all of the disclosed features and structures, either separately or in combination, and wherein the short staple fiber yarn exhibits a strength of 8 cN/tex or less, Method.
12. The method according to embodiments 1 to 11, having all the disclosed features and structures separately or in combination, further defined as the fusible thread exhibiting a strength of at least 11 cN/tex.
13. The method according to embodiments 1-12, having all of the disclosed features and structures separately or in combination, wherein the weld yarn is at least 50 percent (%) greater than the diameter of the short staple fiber yarn. The method, further defined as having a small diameter.
14. The method according to embodiments 1-14, further comprising all of the disclosed features and structures, either separately or in combination, and further wherein the short staple fiber yarn has a density of 0.38 g/cc or less. Will be done.
15. The method according to embodiments 6-14, further defined as having all the disclosed features and structures separately or in combination, and further wherein said weld yarn has a density of at least 0.5 g/cc. ,Method.
16. A method according to embodiments 6-15, further defined as having all the disclosed features and structures separately or in combination, and wherein said short staple fiber yarns have at least 30% by weight of short staple fibers. Wherein the remainder of the short staple fiber yarn is made from fibrils.
17. The method according to embodiments 6-16, further comprising all of the disclosed features and structures, separately or in combination, and further wherein the fibrils have a short staple fiber length of at least 1.00 inches. A defined method.
18. The method according to embodiments 6-17, having all of the disclosed features and structures, separately or in combination, wherein the weld yarn is at least 20 percent (%) stronger than the short staple fiber yarn. A way to show an increase.
19. 19. The method according to embodiments 6-18, having all the disclosed features and structures separately or in combination, further defined as utilizing a process solvent with an ionic liquid.
20. A welded yarn made from a combination of natural fibrils and natural wool fibers,
The welding thread is
a. Said natural fibrils in the range of 0 weight percent (%) to 90 weight percent (%); and b. Said anti-wool fibers in the range of 10 weight percent (%) to 100 weight percent (%),
Made from a raw yarn base material having
The welded yarn is produced by chemically welding the amount of the natural fibrils to the amount of the wool fibers.
21. A fusion splicer according to embodiment 20, having all of the disclosed features and structures, either separately or in combination, wherein the strength per cross-sectional area of the fusion yarn is A fused yarn that is at least 20 percent (%) greater than the strength.
22. A weld yarn according to embodiment 20 or 21, wherein the weld process for making said weld yarn is configured to use an ionic liquid based process solvent.
23. Welded yarns according to embodiments 20-22, having all disclosed features and structures separately or in combination, and further wherein said welded yarns have a Cellulose I crystal structure of less than 65 weight percent (%). , Welding thread.
24. Welded yarns according to embodiments 20-23, having all disclosed features and structures separately or in combination, and further wherein said welded yarn has a Cellulose I crystalline structure of less than 60 weight percent (%). , Welding thread.
25. A welded yarn produced from a base yarn base material, wherein the base yarn base material has natural fibrils and natural reaction fibers, and the strength of the base yarn base material is less than 8 cN/tex. The strength is at least 11 cN/tex, the cross-sectional area of the weld yarn is at least 50 percent (%) smaller than the diameter of the base yarn base material, and the elongation at break of the weld yarn is at least 3 percent (%). yarn.
26. A weld yarn according to embodiment 25, having all of the disclosed features and structures, separately or in combination, wherein said diameter of said weld yarn is 30 percent (%) of said diameter of said raw yarn substrate. ) To 50 percent (%).
27. A welded yarn according to embodiment 25 or 26 having all of the disclosed features and structures separately or in combination, further wherein said strength of said welded yarn is at least greater than said strength of said base yarn substrate. 20% (%) larger, welded yarn.
28. A welded yarn according to embodiments 25-27, having all of the disclosed features and structures separately or in combination, wherein the strength per cross-sectional area of the welded yarn is greater than that of the base yarn substrate. A welded yarn that is at least 30 percent (%) greater than the strength per hit.
29. A weld yarn according to embodiments 25-28, having all of the disclosed features and structures separately or in combination, wherein the weld yarn has a Cellulose I crystal structure of less than 65 weight percent (%). , Welding thread.
30. Welded yarns according to embodiments 25-29, having all disclosed features and structures separately or in combination, and further wherein said welded yarn has a Cellulose I crystalline structure of less than 60 weight percent (%). , Welding thread.

(Figs. 1 and 2)
1 Base Material Supply Zone 2 Process Solvent Application Zone 3 Process Temperature/Pressure Zone 4 Process Solvent Recovery Zone 5 Drying Zone 6 Weld Base Material Collection Zone 7 Solvent Collection Zone 8 Solvent Recycle 9 Mixed Gas Collection 10 Mixed Gas Recycle (Figure 3A-22)
10 Natural Fiber Substrate 11, 112 Swelled Natural Fiber Substrate 12 Weld Substrate 20 Functional Material 21 Bound Functional Material 22 Entrapped Functional Material 30 IL-Based Process Solvent 32 Process Solvent/Functional Material Mixture 40, 42 Welded Fiber 53 Polymer 60 Injector 61 Base Material Inlet 62 Process Solvent Inlet 63 Application Interface 64 Base Material Outlet 70 Tray 72 Base Material Groove 82 First Plate 84 Second Plate 90 Undyed Knitting Yarn Base Material 92 Undyed Fiber Base Material 90' Dyeing woven yarn base material 92' Dyeing fiber base material 100 Welding yarn base material 102 Unmodified base material fiber 103 Lightly welded base material fiber 104 Mediumly welded base material fiber 105 Firmly welded base material Material fiber 106 Binder 108 Binder shell 109 Pigment particles

Claims (30)

A fused cellulosic yarn having an effective yarn density of 0.5 g/cc to 1.0 g/cc and a strength of the fused yarn of 10 cN/tex to 15 cN/tex. The weld yarn of claim 1, wherein the weld yarn is further defined as being made from a raw substrate having short staple fiber yarns utilizing a welding process. The weld yarn of claim 2, wherein the weld process for making the weld yarn is configured to use an ionic liquid-based process solvent. The weld yarn of claim 1, wherein the weld yarn has a Cellulose I crystal structure of less than 65 weight percent (%). The fusible thread of claim 1, wherein the fusible thread has a Cellulose I crystal structure of less than 60 weight percent (%). A method for producing a fused yarn,
a. Preparing a raw substrate, said raw substrate comprising short staple fiber yarns;
b. Applying a process solvent to the substrate to make a process wet substrate, wherein the process solvent swells and mobilizes at least one polymer in the substrate;
c. At least controlling the temperature and time at which the process solvent interacts with the process wet substrate; and d. A method comprising removing at least a portion of the process solvent from the process wet substrate. 7. The method of claim 6, wherein the short staple fiber yarns are further defined as having an average short staple fiber length of less than 1.00 inches. 8. The method of claim 7, wherein the short staple fiber yarn is further defined as having at least 5% by weight of fibrils, and the remainder of the short staple fiber yarn is made of short staple fibers. 9. The method of claim 8, wherein the fusible yarn exhibits a strength increase of at least 20 percent (%) over the short staple fiber yarn. 9. The method of claim 8, wherein the fusible yarn exhibits an increase in strength per cross-sectional area of at least 50 percent (%) over the short staple fiber yarn. 7. The method of claim 6, wherein the short staple fiber yarn is further defined as exhibiting a strength of 8 cN/tex or less. 8. The method of claim 7, wherein the fusible yarn is further defined as exhibiting a strength of at least 11 cN/tex. 13. The method of claim 12, wherein the fusible yarn is further defined as having a diameter that is at least 50 percent (%) less than the diameter of the short staple fiber yarn. 14. The method of claim 13, wherein the short staple fiber yarn is further defined as having a density of 0.38 g/cc or less. 15. The method of claim 14, wherein the fusible yarn is further defined as having a density of at least 0.5 g/cc. 8. The method of claim 7, wherein the short staple fiber yarn is further defined as having at least 30% by weight of short staple fiber, and the balance of the short staple fiber yarn is made from fibrils. 17. The method of claim 16, wherein the fibrils are further defined as having a short staple fiber length of at least 1.00 inches. 18. The method of claim 17, wherein the fusible yarn exhibits a strength increase of at least 20 percent (%) over the short staple fiber yarn. 19. The method of claim 18, wherein the method is further defined as utilizing a process solvent having an ionic liquid. A welded yarn made from a combination of natural fibrils and natural wool fibers,
The welding thread is
a. Said natural fibrils in the range of 0 weight percent (%) to 90 weight percent (%); and b. Said anti-wool fibers in the range of 10 weight percent (%) to 100 weight percent (%),
Made from a raw yarn base material having
The welded yarn is produced by chemically welding the amount of the natural fibrils to the amount of the fluff fibers. 21. The weld yarn of claim 20, wherein the weld yarn has a strength per cross-sectional area that is at least 20 percent greater than a strength per cross-sectional area of the raw yarn substrate. 22. The weld yarn of claim 21, wherein the weld process for making the weld yarn is configured to use an ionic liquid-based process solvent. 21. The weld yarn of claim 20, wherein the weld yarn has a Cellulose I crystal structure of less than 65 weight percent (%). The weld yarn of claim 20, wherein the weld yarn has a Cellulose I crystal structure of less than 60 weight percent (%). A welded yarn produced from a base yarn base material, wherein the base yarn base material has natural fibrils and natural reaction fibers, and the strength of the base yarn base material is less than 8 cN/tex. The strength is at least 11 cN/tex, the cross-sectional area of the weld yarn is at least 50 percent (%) smaller than the diameter of the base yarn base material, and the elongation at break of the weld yarn is at least 3 percent (%). yarn. 26. The weld yarn of claim 25, wherein the diameter of the weld yarn is between 30 percent (%) and 50 percent (%) of the diameter of the raw yarn substrate. 26. The weld yarn of claim 25, wherein the strength of the weld yarn is at least 20 percent (%) greater than the strength of the base yarn substrate. 26. The weld yarn of claim 25, wherein the weld yarn has a strength per cross-sectional area that is at least 30 percent greater than a strength per cross-sectional area of the raw yarn substrate. 26. The weld yarn of claim 25, wherein the weld yarn has a Cellulose I crystal structure of less than 65 weight percent (%). 26. The weld yarn of claim 25, wherein the weld yarn has a Cellulose I crystal structure of less than 60 weight percent (%).