JP2023525069A - Method, Apparatus, and System for Fibrillated Nanocellulose Materials - Google Patents

Abstract

A fibrillated nanocellulose material method, apparatus, and system overcomes the shortcomings of the prior art by infusing nanocellulose in fibrillated form to enhance the properties of cellulose pulp. These properties can include, for example, mechanical properties and barrier properties. That is, tensile strength, impermeability to liquids and gases such as oxygen, carbon dioxide, and oil can be substantially improved. The present invention further provides fibrillated cellulose composites that include properties of being strength enhancers, oligomers, carboxylic acids, plasticizers, antimicrobial agents, water repellants, and/or transparent composites.

Description

TECHNICAL FIELD Aspects of the present invention relate generally to renewable and recyclable materials. More particularly, embodiments of the present invention relate to fibrillated cellulose materials made for consumer products.

BACKGROUND The environmental crisis, the growing concern over plastic waste pollution, has triggered extensive research into sustainable and renewable materials. In striving to avoid petroleum-derived polymers, naturally occurring biopolymers, plant-based cellulose fibers, offer an alternative to the materials research industry. Cellulose fibers are receiving increasing attention due to their ubiquitous sources of sustainable, renewable, and more importantly, they are 100% biodegradable in nature. Provide the final product.

However, many existing biodegradable products based on cellulose fibers fall short of that expectation. For example, the cost of manufacturing these cellulosic fiber products is not economically viable for large scale production. Moreover, due to the need for water resistance, oil resistance, or non-stick properties, many products of cellulosic fibers rely heavily on synthetic chemical compositions to achieve these properties or effects. For example, many existing products require a fluorocarbon coating to be applied to surfaces that come into contact with food or beverage items. Additionally, some of these fluorocarbon-based chemicals, such as perfluorooctanoic acid (PFOA or C8), can cause long-term negative health and environmental impacts.

Furthermore, current practice has not produced two or more layers of fibrillated cellulose material. Rather, previous practice only attempts to produce a single layer from a cellulose pulp solution.

SUMMARY Embodiments of the present invention overcome the shortcomings of the prior art by infusing nanocellulose in fibrillated form to enhance the properties of cellulose pulp. These properties can include, for example, mechanical and barrier properties, ie, tensile strength, impermeability to liquids and gases such as oxygen, carbon dioxide, and oil can be substantially improved.

Another embodiment of the present invention is a layer of fibrillated cellulose or a Further provided is a fibrillated cellulose composite comprising the mixture. The composite may also generally be free of chemical additives to enhance the properties described above. In yet another embodiment, the composite may further comprise a substrate (eg, pulp) and another layer (eg, fibrillated cellulose).

BRIEF DESCRIPTION OF THE FIGURES Skilled artisans can appreciate that elements in the drawings are illustrated for simplicity and clarity and that not all relationships and options are shown. For example, common but well-understood elements that are useful or necessary in commercially viable embodiments are often not described so as not to obscure the drawings of these various embodiments of this disclosure. Sometimes. Although certain acts and/or steps may be described and presented in a particular order of appearance, those skilled in the art will understand that such specificity as to order is not necessarily required. It can be further appreciated that it is possible. It is also understood that the terms and expressions used herein may be defined with respect to their corresponding respective fields of research and testing, unless a specific meaning is otherwise indicated herein. can be

1A-1D illustrate the material of the cellulosic fiber aqueous suspension according to one embodiment.

Figure 2 is a scanning electron microscope (SEM) image of a material with fibrillated cellulose (3 wt%) according to one embodiment.

3A-3D are scanning electron microscope (SEM) images of semi-processed cellulose fibers, where a-b are SEM images of Y-cellulose fibers, and cd are B- cellulose fibers according to one embodiment. SEM image of cellulose fibers.

Figures 4A-4D are SEM images of mechanically ground semi-finished fibers, where a-b are Y-cellulose fibers and cd are B-cellulose fibers according to one embodiment.

FIG. 5 illustrates images of containers made from fibrillated celluloses L28b, L29b, L30b, and Y, which were able to retain oil for 10 days according to one embodiment.

FIG. 6A is an image showing a food item with boiling water in the ingredients for about 5 minutes according to one embodiment.

FIG. 6B is an image showing a food item in boiling water and heated at 800 W for 2 minutes under a microwave according to one embodiment.

FIG. 7 is another SEM image of a material relating to the structure of fibrillated cellulose used in food containers according to one embodiment.

Figure 8 is a flow diagram of a method for manufacturing a material according to one embodiment.

FIG. 9 illustrates three images showing film according to one embodiment.

10A-13 illustrate an apparatus according to one embodiment. 10A-13 illustrate an apparatus according to one embodiment. 10A-13 illustrate an apparatus according to one embodiment. 10A-13 illustrate an apparatus according to one embodiment. 10A-13 illustrate an apparatus according to one embodiment. 10A-13 illustrate an apparatus according to one embodiment. 10A-13 illustrate an apparatus according to one embodiment. 10A-13 illustrate an apparatus according to one embodiment. 10A-13 illustrate an apparatus according to one embodiment.

Figures 14A-14D illustrate an exemplary final product manufactured according to aspects of the above embodiments.

DETAILED DESCRIPTION Embodiments may now be described more fully with reference to the accompanying drawings, which form a part hereof and show, by way of illustration, specific exemplary embodiments that may be practiced. Although these illustrations and exemplary embodiments are illustrative of the principles of one or more embodiments, this disclosure is not intended to limit any one of the illustrated embodiments. It can be shown in conjunction with the understanding that there is The embodiments may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments provide a thorough and complete disclosure. is provided so as to fully convey the scope of the embodiments to those skilled in the art. Accordingly, the following detailed description should not be taken in a limiting sense.

Embodiments of the present invention include materials such as Green Composite Material ^™ (GCM ^™) , which may include fibrillated cellulose as a core material without any material. , pulp and fibrillated cellulose.In another embodiment, the composite may be generally free of chemical additives or agents.In yet another embodiment, the composite is made entirely of plant fibers. In one embodiment, the chemical additive or agent may be naturally-based or non-toxic, In another embodiment, the chemical additive or agent is made by a laboratory. In some embodiments, these plant fibers are derived from bagasse, bamboo, manila hemp, sisal hemp, thyme, flax, hops, jute, kenaf, palm, coir, corn, cotton, wood, and any combination thereof. In still other embodiments, the plant fiber can be preprocessed or semi-processed cellulose, hi other embodiments, the green composite material with fibrillated cellulose can be obtained through a refining process (e.g., high pressure by processing plant fibers through a homogenizer or refiner.In a further embodiment, a composite with fibrillated cellulose can be obtained via bacterial strains (without cellulogenic microorganisms).Alternative implementations In form, materials having fibrillated cellulose can be obtained from marine sources.

In one embodiment, the shape and size of the cellulose may depend on the origin of the fiber or combination of fibers and the process of making it. Nevertheless, fibrillated cellulose generally has diameters and lengths as described below. The fibrillated cellulose, in one embodiment, can have a diameter of about 1-5000 nanometers (nm). In yet another embodiment, the fibrillated cellulose can have a diameter of about 5-150 nm or about 100-1000 nm. In yet another embodiment, the fibrillated cellulose can have a diameter of about 5000-10000 nm.

In still further embodiments, the materials may have enhanced properties that enhance, enhance, or improve properties without toxic chemical additives or agents. In another embodiment, materials having various properties suitable for carrying food or liquid items are generally free of chemical additives or agents. For example, as shown in the prior art, various toxic chemical additives or Drugs have been added to or coated onto the material during the manufacturing process. Aspects of the present invention include composites having fibrillated cellulose that is generally free of various toxic chemical additives or agents instead of adding these additives or agents to the materials.

For example, the fibrillated cellulose can have a length of about 0.1-1000 microns, about 10-500 microns, about 1-25 microns, or about 0.2-100 microns. In some embodiments, materials having different diameters of fibrillated cellulose can have a weight ratio of, for example, 1:100. In another embodiment, the fibrillated cellulose may have a weight ratio of 1:50. In further embodiments, materials with mixed fibrillated cellulose have properties such as improved tensile strength (either dry or wet), enhanced oil barrier, gas and/or liquid impermeability, and cost savings. can provide advantages.

In some embodiments, materials comprising fibrillated cellulose can have oxygen permeability properties of about 8000 cm ³ m ⁻² 24 h ⁻¹ or less. In another embodiment, the oxygen permeability is about 5000 cm ³ m ⁻² 24 h ⁻¹ or less. In yet another embodiment, the oxygen permeability is about 1000 cm ³ m ⁻² 24 h ⁻¹ or less.

Additionally, in some further embodiments, the material may have a moisture vapor transmission rate property of about 3000 g m ⁻² 24 h ⁻¹ or less. Further, for another embodiment, the water vapor transmission rate may be about 1500 g m ⁻² 24 h ⁻¹ or less.

In some embodiments, the material can have a dry tensile strength property of about 30 MPa or greater. In another embodiment, the dry tensile strength can be about 70 MPa. In yet another embodiment, the dry tensile strength may be about 100 MPa or greater. In some embodiments, the material can have a dry tensile modulus property of about 4 GPa or greater. In another embodiment, the dry tensile modulus is about 6 GPa or greater.

In some embodiments, the material can have a dry tensile index property of about 45 Nm g ⁻¹ or greater. In another embodiment, the property may be about 80 Nm g ⁻¹ or greater.

In some embodiments, the material can have wet tensile strength properties of about 5 MPa or greater. In another embodiment, the wet tensile strength may be about 20 MPa or greater.

In some embodiments, the material can have a wet tensile modulus property of about 0.4 MPa or greater. In another embodiment, the wet tensile modulus may be about 1.0 MPa or greater.

In some embodiments, the material can have a wet tensile index property of about 5 Nm g ⁻¹ or greater. In another embodiment, the wet tensile index may be about 20 Nm g ⁻¹ or greater.

In alternate embodiments, the material may include an adhesive to enhance dry and/or wet strength. In one embodiment, the adhesive may contain a polymer. In other embodiments, the adhesive may include metal salts. In another embodiment, the adhesive may comprise oligomers. In still other embodiments, the adhesive may include carboxylic acid. In further alternative embodiments, the adhesive may include a plasticizer. In some embodiments, the weight ratio of fibrillated cellulose to the adhesive in the present invention can be from about 33:1 to 1:1.

For example, the polymer can include polyester, gelatin, polylactic acid, chitin, sodium alginate, thermoplastic starch, polyethylene, chitosan, chitin glucan, polyvinyl alcohol, or polypropylene. In one embodiment, the polymer may contain chemical additives that may be applied to the composites of aspects of the invention. For example, the chemical additives may be embedded within the material itself, or sprayed or coated thereon.

In yet another embodiment, the adhesive may contain metal salts. For example, the metal salts can include potassium zirconium carbonate, potassium aluminum sulfate, calcium carbonate, and calcium phosphate. In some embodiments, the weight ratio of fibrillated cellulose to the adhesive in the present invention can be from about 33:1 to 1:1.

In another embodiment, the adhesive may comprise oligomers. In one example, the oligomers can include oligonucleotides, oligopeptides, and polyethylene glycol. In some embodiments, the weight ratio of fibrillated cellulose to the adhesive in the present invention can be from about 33:1 to 1:1.

In still other embodiments, the adhesive may include carboxylic acid. For example, the carboxylic acid can include citric acid, adipic acid, and glutaric acid. In some embodiments, the weight ratio of fibrillated cellulose to the adhesive in the present invention can be from about 33:1 to 1:1.

In embodiments, adhesives with the plasticizer can reduce the brittleness and gas permeability of the bonded composite. In some embodiments, the plasticizer can include a polyol. In one embodiment, the polyol may include glycerol. In one embodiment, the polyol may include sorbitol. In one embodiment, the polyol can include pentaerythritol. In some embodiments, the polyol can include polyethylene glycol. In some embodiments, the weight ratio of plasticizer to the composite to adhesive is from about 5:33:1 to about 1:1:1.

In another embodiment, the plasticizer may include branched polysaccharides, waxes, fatty acids, fats and oils.

Aspects of the invention may further include water repellent agents as chemical additives to render water impermeable in gaseous and/or liquid states. In some embodiments, the water repellent agent comprises animal-based waxes, animal-based oils or animal-based fats. In one embodiment, the water repellent agent comprises a petroleum-derived or petroleum-based wax. In other embodiments, the water repellent agent comprises plant-based waxes, plant-based oils or plant-based fats.

In some embodiments, animal-based water repellents may include beeswax, shellac and whale oil.

In some embodiments, petroleum-based wax repellents may include paraffin wax, paraffin oil and mineral oil.

In some embodiments, plant-based water repellants can include carnauba wax, soybean oil, coconut oil, coconut wax, carnauba wax and coconut oil.

In some embodiments, water repellants can include adhesives such as potassium zirconium carbonate, potassium aluminum sulfate, calcium carbonate and calcium phosphate.

In further embodiments, the material may comprise fibrillated cellulose, and optionally an antimicrobial agent. In some embodiments, the antimicrobial agent can include chapolyphenols. In some embodiments, antimicrobial agents can include pyrithione salts, parabens, paraben salts, quaternary ammonium salts, imidazolium, benzoic acid sorbic acid, and potassium sorbate.

Additionally, another embodiment of the present invention may include a material having fibrillated cellulose optionally further comprising a transparent composite to increase transmission of light having wavelengths between about 300-800 nm. In some embodiments, the material can include branched polysaccharides. In some embodiments, the weight ratio of the material to transparent composite can range from, for example, about 99:1 to about 1:99, which can depend on the transparency required. .

In some embodiments, branched polysaccharides may include starch, dextran, xantham gum, and galactomannans.

In some embodiments, dextrans can include agarose, pullulan, and curdan.

In some aspects, the manufacture of articles made from the materials disclosed herein is provided herein and is readily formed into designed shapes, e.g., in either two or three dimensions. do. For example, a two-dimensional example can be a flat sheet, where the flat sheet can be used to break apart to form the final product. In another example, the materials can be in solution, which can be ready to form the final product. In yet another embodiment, the three-dimensional example can be the final product.

In one aspect, in some embodiments, the final product may include a container for edible or edible items (eg, those shown in FIGS. 5-7). For example, the final product embodying materials as described in this application may include food containers or packages. By way of example and not limitation, such food containers or packages include airplane or airline meal containers, disposable cups, ready-to-eat food containers, capsules, ice cream. and chocolate containers. In some embodiments, the product may include instant food containers (eg, instant cup noodles, instant soup, etc.) that may further include spices. In such instances, in order for the consumer to eat or consume the edible or edible items contained in the container embodying aspects of the invention, the container is subjected to elevated temperatures (e.g., about 100°C). ) water or liquid can be applied.

In another embodiment, the products that may be used include in-flight meal and beverage containers. Currently, in-flight meal containers are made from various forms of plastic due to their properties such as light weight, stiffness and oil resistance. Additionally, existing plastic containers can be subjected to heat via an oven. Heating can also release carcinogens from plastic containers into edible or edible items. Such effects are therefore undesirable. Embodiments of the present invention may exhibit properties such as water resistance, high heat resistance, and oil resistance, along with the above properties, without releasing carcinogens.

In another embodiment, an example of a capsule can be a machine capsule for hot beverages. For example, the capsule may contain coffee, tea, herbs, or other drinks. For example, the capsule can be a single-use capsule. In another example, the capsule can be a disposable coffee bag or pouch. In such an example, an electrically powered beverage machine would deposit or inject hot or high pressure water into the capsule, such that the beverage making process could begin and coffee would flow from the capsule or pouch into the consumer's cup. and can be brewed. Since the capsule or pouch comprises a biodegradable and sustainable material having one or more properties as described above, the capsule or pouch is easily recycled without impacting the environment. can be

In one embodiment, the capsule can have sidewalls with a thickness of about 500 microns. In one embodiment, the capsule may include a top or lid having a thickness of about 500 microns. In yet another embodiment, the capsule can include a bottom thickness of about 300 microns. In still further embodiments, the capsules may be formed/made in one pass from a former (discussed below), with top, sidewall and bottom thicknesses having different thicknesses.

In some embodiments, the article of manufacture may include a filter to separate, either permanently, semi-impermeable, or lightly impermeable, particles or molecules in the fluid. For example, the product may include a face mask or filter membrane with solid-liquid separation, liquid-liquid separation, or gas-liquid separation effect.

In some embodiments, products may include cosmetic or skin care container products, medical products such as powder cases, pallets, protective glasses, or medical grade disposable products. In some embodiments, the products may form part of medical devices, automobiles, electronic devices, and building materials (as reinforcements).

Generally, in one embodiment, containers embodying the materials of the present invention can be in the form of containers, flat sheets, trays, plates, reels, boards, films. In such embodiments, the width or length of the material can range from about 0.01 mm to 10000 mm or greater. In one embodiment, the width or length can range from about 0.01 mm to 1000 mm. In embodiments in which the film can be a thin film, the thickness is about 0.01-3.0 mm. In one embodiment, the thickness can be about 0.02-0.20 mm. In still other embodiments, the product may constitute a food package comprising an oil to water weight ratio of about 100:1 to about 1:100.

In another embodiment, aspects of the invention may provide processes for manufacturing, producing, or making materials comprising fibrillated cellulose having the properties described above.

Example 1
In addition to the materials provided above, aspects of the invention can include processes or methods of cellulose fibrillation.

Referring now to FIG. 8, a flow diagram may illustrate a method for making such materials according to one embodiment. In one embodiment, the examples presented below are generally free of toxic chemical additives to improve the mechanical properties of the composite. For example, cellulose cardboard (approximately 3.0% by weight) was torn into pieces, such as A4 size paper. The shredded pieces of paper are fed into a pulp former (not shown in FIG. 8). The pulping process takes about 20 minutes. The process can then begin, for example, using refiner 802 . For example, the refiner 802 can be a homogenizer, a grinder, a chemical refinement chamber/bath, a combination of mechanical and chemical fiber refinement devices, and the like. In one embodiment, in the example of a grinder, refiner 802 may include two rotating grinding discs facing each other. The separation or distance between the two rotary grinders can be adjusted depending on the desired final product. In another embodiment, the surface grooves or patterns can be adjusted according to the desired end product. Thus, the pulp suspension 806 is then fed to the refiner, making about 1-10 passes as needed. In other cases, pulp suspension 806 may be fed to a refiner (not shown), such as a colloid mill, double disc grinder, to further refine the cellulose pulp before entering refiner 802. .

In one embodiment, FIGS. 1a-1d show the condition of fibrillated cellulose with increasing number of passes. For example, FIG. 1a may represent a cellulosic fiber aqueous suspension with 0 cycles or passes. In other words, the content of pulp suspension 806 as shown in FIG. 1a is such that the pulp does not form fibrillated material to achieve the qualities and properties of aspects of the present invention.

In one embodiment, FIG. 1b may illustrate the refined material 808 after the pulp suspension 806 passes through the refiner 802 once. For example, post-purification material 808 may now include an aqueous suspension of fibrillated cellulose fibers. In another example, FIG. 1 c illustrates an image of refined material 808 after two passes or cycles through refiner 802 . In one example, the fibrillated cellulose fibers of post-purification material 808 are finer than those shown in FIG. 1b. FIG. 1d may illustrate an image of purified material 808 after 3 cycles/pass. In such embodiments, post-purification material 808 may comprise fibrillated cellulose fibers that are even finer than in FIG. 1c.

In one embodiment, different cellulose starting concentrations were evaluated and tested. For example, post-purification material 808 may include fibrillated cellulose fibers and water, about 2.5% by weight cellulose (and 97.5% water), about 3.0% by weight cellulose, about 3.6% by weight % cellulose, and concentrations of fibrillated cellulose at about 4.0% cellulose by weight were tested and used.

For example, poor purification was found for a cellulose concentration of about 2.5% by weight, the properties of which were not tested. In other words, a fibrillated cellulose fiber concentration or even a normal pulp suspension solution having about 2.5% by weight is insufficient to achieve the properties of aspects of the present invention. The fibrillated cellulose in post-purification material 808 having about 3.0 wt%, about 3.6 wt%, and about 4.0 wt% is referred to herein as L028, L029, and L030, respectively, in FIG. called.

In one embodiment, various properties of fibrillated cellulose were tested. For example, in Table 1 the mechanical, water vapor and gas permeability properties are shown.

In one embodiment, FIG. 2 may illustrate an SEM image of fibrillated cellulose at a concentration of about 3% by weight.

Example 2
In one example, instead of using the direct pulp solution obtained in post-refining material 808 in Example 1 above, semi-processed cellulose fibers may be obtained from commercial sources. Thus, semi-processed cellulose fibers (eg, about 3% by weight) are fed to a colloid mill and ground for about 1 minute. If desired, the fibrillated cellulose fibers may be further processed in refiner 802 .

In one example, FIG. 3 may illustrate an SEM image of a semi-processed fiber after colloid milling for 1 minute. For example, Table 2 shows the properties of different fibrillated celluloses derived from different sources.

For example, FIG. 3 may illustrate that ab are SEM images of the Y-cellulose fibers in Table 2 and cd are SEM images of the B-cellulose fibers.

In another embodiment, Figure 4 shows an SEM image of the semi-finished fiber after mechanical grinding for 1 cycle/pass. For example, Figures 4a-b are for Y-cellulose fibers and Figures 4c-d are for B-cellulose fibers.

In one aspect, the mixer 804 can provide a pulp suspension 806 of cellulose pulp-in-water comprising a mixture of cellulose pulp-in-water. Here the weight ratio of cellulose to water is about 0.01 to 100. In another embodiment, the weight ratio can be about 0.03 to 0.10. In some embodiments, the refined material 808 from the refiner 802 can be set aside where it can be used to be ground again by the refiner 802 . For example, as noted above, the number of passes the refined material 808 makes through the refiner 802 can be between 1 and 100 passes. In another embodiment, the number of passes or cycles may be further limited to 1-10.

In another embodiment, the weight ratio of fibrillated cellulose to water and/or the number of passes through refiner 802 may depend on the desired properties of the final product. For example, if the final product calls for low water vapor transmission, and low oxygen transmission, the post-purification material 808 will have a cellulose to water ratio closer to about 0.03-0.04 3-4% (as indicated by L28b-L30b). and/or the number of passes may be increased. In yet another embodiment, relatively low water vapor transmission and relatively low oxygen transmission may indicate high shelf life, while relatively high water vapor transmission and relatively high oxygen transmission may indicate low shelf life.

In one embodiment, purified material 808 may be processed by former 810 . For example, former 810 may produce intermediate material 818 based on post-purification material 808 into a desired material having fibrillated cellulose. For example, intermediate material 818 can be in a weight ratio of fibrillated cellulose to liquid (eg, water) of about 0.001 to 99. In another embodiment, the ratio can be about 0.001-0.10. In one embodiment, former 810 may comprise a mesh or fiber network. For example, former 810 may include negative pressure and/or positive pressure or any combination thereof. In one embodiment, former 810 may apply pressure to separate fibrillated cellulose in post-purification material 808 from liquid to form intermediate material 818 . Due to the fibrillated nature of the fibrillated cellulose fibers, and through the process of the refiner 802, fibers with different lengths are produced in the intermediate material 818, as shown by the various SEM images in Figures 2-4 and 7. can form

In another embodiment, base layer 812 may be used with post-purification material 808 to form intermediate material 818 . In one embodiment, the GCM of aspects of the present invention may comprise a composite having a pulp base layer (eg, base layer 812) and a fibrillated cellulose layer (eg, from post-refining material 808). For example, former 810 may subject base layer 812 to a mesh, mold, or frame to form a construction for intermediate material 818 . For example, the base layer 812 may initially be in the form of a solution or slush of water and pulp material. The slush may be in the tank and the mesh may also be in the tank. Via negative pressure (eg, vacuum), water from the tank can be removed or reduced and a base layer 812 can be formed on the mesh.

Thereafter, in one embodiment, former 810 may include a sprayer or applicator to spray or apply post-purification material 808 onto base layer 812 to form intermediate material 818 . The refined material 808 is infused into the base layer 812 with the fibers of the base layer 812 and the refined material 808 having different sizes. In one embodiment, the post-purification material 808 can be applied or sprayed onto the surface of the intermediate material 818 carrying the edible item. For example, if the final product is a bowl, post-purification material 808 may be applied or sprayed onto the inner surface of the final product.

In one embodiment, intermediate material 818 may exhibit a mesh or fiber network pattern on its exterior surface, as shown at 502 or 504 .

In yet another embodiment, former 810 may spread intermediate material 818 onto a flat surface for drying or forming by natural processes.

In another embodiment, dryer 814 may further be provided to dry or remove moisture from intermediate material 818 . In one embodiment, dryer 814 may provide drying conditions between 30°C and 200°C. In another embodiment, dryer 814 may include a heated surface (eg, infrared heating). In alternate embodiments, microwave heating or air heating may be used without departing from the spirit and scope of the embodiments. In yet another embodiment, dryer 814 may also be assisted by negative pressure and/or positive pressure.

Example 3
In one example of a final product that may embody aspects of the invention, a cellulose-based bowl is successfully manufactured by employing the combination of materials and methods previously described. In one embodiment, the functionality of a cellulose-based food container can be used to demonstrate a typical cooking oil filling of the container, as shown in FIG. 5, in this example. In this example, the cooking oil and cellulose-based food container can be heated by microwaves at 800 W for 4 minutes and observed for 10 days. This is shown in FIG. In such an illustration, the container in FIG. 5 could represent a container made from fibrillated celluloses L28b, L29b, L30b, and Y. In one embodiment, each of the containers in Figure 5 may be capable of holding oil for about 10 days.

In another embodiment, another set of tests was also performed by filling instant noodles (after being cooked with the addition of hot water) into a container embodying a composite according to one embodiment. Observations were recorded on the second day. FIG. 6A shows an example of a fibrillated cellulose structure in a container (eg, food container). For example, FIG. 6A illustrates a series of images of fibrillated cellulose filled with boiling water and allowed to sit for about 5 minutes.

In another embodiment, FIG. 6B illustrates a series of images of fibrillated cellulose filled with boiling water and microwaved at 800 W for about 2 minutes.

FIG. 7 is another image showing an SEM image of the structure of fibrillated cellulose in the food container in FIGS. 6A and 6B according to one embodiment.

Example 4
Referring now to Figures 9a-9c, the images illustrate a film according to Example 4 of the embodiment.

In one embodiment, a composite according to aspects of the invention can be a transparent composite film based on fibrillated cellulose. In one example, the film can be produced by dissolving fibrillated cellulose and pullulan powder in water to separately produce a solution containing about 1% by weight of solute. For pullulan powder dissolution, the powder can be added gradually and the solution can be heated via microwave at a power of 800 W for 1 minute. In one embodiment, this process can be repeated about 4-5 times until a clear solution is formed.

In one embodiment, fibrillated cellulose (e.g., post-purification material 808) to pullulan can be in a ratio of about 1:1 to produce a composite film, e.g., about 250 g of post-purification material 808 (e.g., , about 1% fibrillated cellulose) can be mixed with about 250 g of pullulan solution to produce a solution having about 0.5% solute. About 100 g of the mixed solution was then poured onto a hydrophobic surface, such as a silicone surface, and left to dry at room temperature.

In another embodiment, fibrillated cellulose to pullulan has a ratio of 2:1, and 250 g of post-purification material (e.g., about 2% fibrillated cellulose) produces a solution having about 1% solute. can be mixed with about 250 g of pullulan solution to About 100 g of the mixed solution was then poured onto a hydrophobic surface, eg a silicone surface, and left to dry at 50° C. and 12 hours.

As illustrated, Figures 9a-9c show that fibrillated cellulose vs. pullulan is a. ) 0:1, b. ) 1:1, and c. ) image of a cellulose-based film with a 2:1 ratio.

In one embodiment, the addition of pullulan may enhance the film formation process to smooth the surface of the film. Here, films made from fibrillated cellulose (eg, post-purification material 808), hereinafter referred to as L41b, are highly wrinkled. In contrast, other films with pullulan provide a smoother and more uniform surface. In one embodiment, the composite film with fibrillated cellulose and pullulan appears generally free of uneven surfaces.

In yet another embodiment, the mechanical properties of the transparent composite film are shown below, where fibrillated cellulose is referred to as L41b and pullulan is referred to as B.

Table 3 Properties of fibrillated cellulose films with added pullulan

Example 5
Fibrillated cellulose with water repellent

In one embodiment, aspects of the invention may include fibrillated cellulose with a water repellent agent. In one example, the mixture may contain the correct ratio of cellulose and water repellent and be blended for 3 minutes using a mechanical blender. The mixture can be further diluted to 4000 mL and poured onto former 810 . In one aspect, the former 810 can apply negative and/or positive pressure to produce a wet preform having a dryness of 25-35%. The mechanical and barrier properties of the mixture can be shown in Table 4.

Table 4 illustrates the properties of fibrillated cellulose films with different water repellent agents.

Additionally, the above embodiments can be made using the device shown in FIGS. 10A-13. From the simplified diagram in FIG. 10A, 1000 components can be considered a container. After being loaded with pulp, paper fibers can be received by 1001 using its vacuum principle from a water tank containing pulp. For example, 1001 may include a fiber catcher. For example, the fiber joint can be a mesh. Because the paper fibers in the water tank can stay inside the mesh body and the liquid will pass through the mesh. The vacuum principle involves first pumping out the water in the water tank and then subjecting the 1001 component strictly to the vacuum environment to create the first material. In one embodiment, component 1001 can be rotated such that the component enters container 1000 facing up or down to form the final product. Component 1001 can again be rotated (eg, 180 degrees) so that any residual moisture, water or liquid can be drained.

In another embodiment, component 1004 can be connected to component 1002, component 1004 can move its vacuum function up, down, left and right, component 1004 can be installed with its component 1002, can be configured. In one embodiment, component 1002 can be used to receive the first material over element 1001 . As shown in FIGS. 10A and 10B, components 1002 and 1004 can be moved to a third unit or water removal device. Similarly, in one embodiment, component 1002 can be rotated to remove water. Moreover, the alignment of the present invention in components 1000, 1002, 1004, 1006, and 1008 does not require linear alignment. Because component 1004 can move in multiple directions, 1000, 1006 or 1008 can be circular, triangular, up, down and other relative positions. Additionally, component 1004 may include a robotic arm or device for movement. In another embodiment, component 1004 can be manually moved to 1006 or 1008 by a mechanical rotating disc or with the aid of rails, manually or with the aid of motorization ( for example, using a robotic arm). In some embodiments, components 1004 may be moved individually or collectively where multiple components 1004 may be used.

In some embodiments, a second material can be received through 1002 and 1004 in one manufacturing process (eg, one product item or mold loading process). In such embodiments, the second material is effectively added to the first material by components 1002 and 1004. FIG. For example, a second material is jointed to a first material through component 1006 and, as in the example above, the first and second materials are intimately mixed to form a third material. be done. In another embodiment, the third material may indicate that the first and second materials indicate different layers.

In another embodiment, components 1000 and 1001 may receive a first material when a multi-station configuration is used. Components 1001 and 1006 can receive a second material. Thus, such a multi-station configuration can produce two different products. As components 1002 and 1004 move material to the next station, the two different products can be manufactured at the same time or substantially the same time. In such embodiments, the time required to manufacture different products can be greatly reduced and the space required for equipment can be reduced as well.

In some embodiments, the container or workstation storing the second material further adds a heat source or heating. For example, component 1002 or 1004 itself, or an additional heat source, may hold the container so that the second material may be mixed with the first material or before the second material is mixed with the first material. or heated to about 40° C. or higher to serve the function of efficiently obtaining the best and most efficient production of the final product. In another embodiment, the heat source may be heated by means of electrical heating, steam, liquids, and the like.

In one embodiment, after the first and second materials are mixed, as described above, components 1002 and 1004 are combined to perform a water removal or water reduction step. 1008 Moved to Drain Station. For example, after mixing the first and second materials for components 1002 and 1004, a third material can be moved from component 1006 to component 1008. FIG. In another embodiment, the third material is vacuum sealed during the mixing process of components 1002, 1004, 1006, and 1008 while mixing the third material. A positive pressure or pressure function is then used on the component 1008 to load the material into the space for mating. As the pressure increases, the moisture or water in the third material is displaced and the original negative pressure design of 1002 and 1004 either pumps the combined material further or reduces the dryness of the combined material. humidity). In some embodiments, component 1008 can be rotated.

Finally, the materials are combined into a molding stage to create the final product.

In another embodiment, the second material can also serve directly as the main body of the third material, as shown in FIG. 10B. For example, after entering the second component in FIG. 10B, the second material is not mixed with the first material.

A device of the invention can be an automated device, as shown in FIG. 11A. That is, the first unit, second unit, and third unit are a series of coherent devices.

In another embodiment of the invention, the third material can be made removable and separate from the combination of components, as shown in FIGS. 11B, 11C, and 11D.

Additionally, although FIGS. 11A-D show component 1004 being moved by a passageway, those skilled in the art may readily employ other methods of moving component 1004 without departing from the underlying principles of the present invention. . The movement need not be constrained to be moved in the same plane.

Further, embodiments of the present invention also include software systems for operating the devices of the present invention (including the sensors in components 1000, 1001, 1002, 1004, 1006, 1008, etc.) and communicating parameter information. The software system may also include different interfaces, whether it is a centralized interface or may be presented on a mobile device via a network. Further, as shown in FIGS. 11B-11D, in different embodiments separate components may have serial or separate interfaces and software to communicate with and operate the operation of the unit or components. The software system may also report notification and alert functions that provide administrators with efficient management of the production process.

Molds and transfer molds, in some embodiments, have rotational features. For example, component 1001 (eg, mold) may include rotation or flip capability through an axis. During the molding process, the mold surface can be raised or lowered into the 1000 slurry container or bucket using a vacuum or suction mechanism. In one example, component 1002 that moves component 1001 may also include rotation functionality. In one aspect, component 1001 can be rotated after the product has been moved and water or moisture can be evacuated by vacuum or gravity.

Grouting: When 1001 and 1002 are paired or jointed, in one example, a pouring cavity may be inside component 1001 to displace material in container 1000. A pump is used to supply the cavity of component 1001, and the water therein can then be withdrawn or removed by a vacuum or other force. Once the first material is completed, the second material can be completed by applying component 1006 in the same manner. In one example, in using components 1000 and 1006, a slurry bucket (eg, container 1000) can be placed anywhere below or above the apparatus.

Figures 12A and B may now illustrate another embodiment of the device. This is also an extension of Figures 10A-11D. For example, the paper forming process may include:1. The paperboard is broken down into pulp through a pulping system. The pulp may be mixed with other materials required for the pulp prior to entering the forming system. 2. Vacuum or suction force is used as an output to adhere the pulp material to the surface of the mold, and then a drainage system is used on the surface of the mold to drain excess water, resulting in a wet process. A thin layer of wet embryo material is formed on the surface of the mold. 3. After molding, the product surface needs a lot of moisture. Air drying, hot air, air pressure, mold heating and other methods can be used to assist hot pressing to expel residual moisture from the material.

The above description provides the following molding process:

(A) Slurry molding method - The molding method is to use the interior of the mold to create a vacuum cavity. Under vacuum operation, the fibers of the pulp can be evenly layered and adhered to the forming net on the surface of the mold, the mold surface facing upwards into the pulp in the tank, allowing a large amount of water to flow. , is removed by vacuum suction. When the product reaches a certain thickness, the product mold leaves the pulp tank and the wet intermediate pulp on the surface of the mold is dewatered.

(B) Injection method - the surface of the above mold is facing upwards, a pulp tank is made around the mold, the pulp is connected to the pulp tank by a pulp pipeline, and the pulp is fed according to the thickness of the product. A quantity of pulp is given and made inside the mold. In the vacuum cavity, the pulp fibers can be uniformly layered and adhered to the forming net on the surface of the mold under vacuum operation, and a large amount of water is taken out by vacuum suction, which is the same as the above Form a wet intermediate on the surface of the mold. The pulp is then dewatered.

(C) Reverse Suction Molding - The surface of the mold faces down into the pulp tank and a large amount of water is drawn out by vacuum suction. When the product reaches a certain thickness, the product mold leaves the pulp tank and the wet intermediate pulp on the surface of the mold is dewatered.

In one aspect, embodiments of the present invention effectively combine at least two materials through the characteristics of the fibers themselves and the fibrillated cellulose using specific arrangements in the process. Two or more layers are brought together or bonded more tightly.

In one example, FIGS. 12A and B illustrate a horizontal, linear or substantially linear system, where 1204, 1204' and 1204'' can be stationary units, 1202, 1202' and 1202 1201, 1201′ can be a mold or mesh, 1200 can be the first layer of material; 1206 can be the second material; or may be a positive pressure component. This equipment features can be a horizontal or linear system (in terms of final product flow), a multi-station system, or an assembly line, and 1202 or 1201 can be rotated and 1201' can also be rotated. obtain.

Or the vertical system is as described in FIG. The vertical system includes 1304 as the fixed unit, 1301 as the mold, 1300 as the first material, 1306 as the second material, and 1308 for dewatering, drainage, positive pressure, hot air, compression, heating, and other machines. include. Among them, the 1301 mold can be designed for rotation.

In another embodiment, the systems of Figures 12A and B and Figure 13 can be partially combined.

From the above embodiments, the method of forming the first material container 1 and the second material container 2 may include one or more of the following features:

A vertical system can be coordinated with rotary actuation if two molding molds are to be completed at the same time. Molding workstations may use injection + suction or suction + injection. The rotary actuation described above can be used:1. a motor drive mechanism for rotating the mold;2. Vertical movement of the mold drives connecting rods, racks, or mechanical structural devices to rotate.

Additionally, the present invention may further enable combinations of the following to achieve processes not previously possible:

Thus, the above table shows that the apparatus of the present invention can be equipped with multiple (more than one) slurries during the molding stage, which can result in different molding processes to meet other different product requirements. shows that:

Thick material finished products of 2 mm or greater:

After the forming station is completed, it can be connected or moved to the 1008 dewatering process. The dewatering unit of this equipment is equipped with a positive pressure and compression device, which accelerates pulp discharge and forming times and is beneficial for forming thick products.

Multilayer transfer stacking molding (including composites)

The use of a linear transfer system or a vertical rotation system can complete the connection of the first layer material and the second layer material simultaneously. The 1002 and 1004 transfer products can be used to stack two or more or the same materials together to create thick and thin composites.

multicolor molding

The use of a linear transfer system or a vertical rotation system can complete the molding of multi-colored materials at the same time, and the blister process using different colored pulps can be completed for one product.

dyeing and molding

In the pulp blister forming process, the pulp dye has to be replaced with another color. Cleaning pipelines is a very time consuming task. A multi-pulp bucket can be used to put the pulp dye into separate molding buckets. After the material of the first layer is formed, it can be moved to the dye of the second layer so that the surface of the pulp absorbs the plastic dye so that it adheres to its color and then dried. can be moved to a process. This system can reduce the time to change dyes of different colors without having to clean the pulping system.

Additive optimization

The timing of pulp additives in pulp molding is very important. It can be added and placed in separate molded barrels. We can choose the right timing to add them to increase the ability of the additives to combine with the pulp fibers. A separate additive can also reduce the chance of pulp return water being contaminated by additives in other systems, improving return water quality.

Multilayer material molding

With this, the process of forming the first layer material and the second layer material can be completed simultaneously. Transfer products 1002 and 1004 can be used to stack two or more or the same materials together to create a composite.

In FIG. 14A, special features of the container elements can enhance this usage. For example, airline meal containers need to be lightweight, durable, and reheatable or heatable. Additionally, ovens or steamers onboard commercial aircraft may be used to heat meals. Also, food items may be accompanied by sauces, soups, or other liquids or fluids, and some of these food items are served hot or hot.

Thus, given the mechanical properties exemplified above, containers embodying elements of aspects of the invention also need to accommodate packaging of the container from the kitchen. Accordingly, as shown in Figure 14A, aspects of the invention can include a lid for the container, the lid also being made from the materials exemplified in this application. Additionally, the lid and the container may include a locking mechanism to allow secure transport of the container and meal. As shown in Figure 14A, a tongue element at the outer end of the container at the end of its curved end can enter the opening created by the edge of the lid. In this embodiment, the end of the lid may include a tip that may be curved toward the container, thus creating an opening instead of leaving the container. The tip may include sufficient length to press against the curved end of the container to allow the tongue element to engage the upper edge of the lid opening. Since the material has the tensile strength described above, the engagement of the tip and the curved end, and the tongue and the upper edge of the lid, will keep the lid in place during transport and heating/reheating. strong enough to keep the

In another embodiment, as shown in FIG. 14B, the tongue can be inserted into a tight opening by the edge of the lid such that there is a friction fit between the container and the lid.

In yet another embodiment, the outer surface of the lid and the bottom of the container may include complementary features. For example, as shown in Figure 14C, the meal containers should be stackable. To prevent or reduce slipping of the container from the underlying lid, the lid may include a lowered central portion or recess, with contoured or recessed curved edges to provide relief from the lowered edge. connecting the central portion and the surface of the lid. Similarly, the feet of the container are center lowered such that each of the feet (e.g., four) mates with the four corners of the lowered portion and the contoured/recessed curved ends. It can be positioned inside the part.

Additionally, the feet protrude from the bottom of the container, as shown in FIG. 14D. In one embodiment, the foot is configured to create an additional air flow by creating a space between the container and the lid in a stacked state, so that heat or steam can be dissipated. , can flow between the container and the lid. In one aspect, such features can further maintain the wet tensile strength of the container.

Overall, aspects of the present invention overcome the drawbacks of previous approaches in which toxic chemicals (eg, fluoropolymers and their derivatives) are added. Aspects of the present invention also overcome the shortcomings of previous approaches that use pulp as the base layer or layers. It should be understood that pulp fibers range in diameter from 10 to 50 micrometers (μm). In contrast, aspects of the present invention are finer in size (eg, in the range of less than 1 μm).

The descriptions above are intended to be illustrative, not limiting. Many variations of the embodiments may become apparent to those of skill in the art upon reviewing this disclosure. The scope of embodiments should, therefore, be determined not with reference to the above description, but instead should be determined with reference to the pending claims, along with their full scope or equivalents. be.

One or more features from any embodiment may be combined with one or more features of any other embodiment without departing from the scope of the disclosure. References to "a", "an" or "above, this, the", unless specifically indicated to the contrary, include "one or more ” is intended to mean. The use of "and/or" is intended to represent the most inclusive meaning of the term unless specifically indicated to the contrary.

While this disclosure can be embodied in many different forms, the drawings and discussion limit the disclosure to the embodiments in which it is an exemplification of one or more inventive principles and any one embodiment is exemplified. is presented with the understanding that it is not intended to be

The present disclosure provides a solution to the above long-desired need. In particular, aspects of the present invention overcome difficulties that rely on the existing practice of using chemical formulations to provide enhanced properties of cellulosic materials.

Additional advantages and modifications of the above-described systems and methods may readily occur to those skilled in the art.

Therefore, the disclosure, in its broader aspects, is not limited to the specific details, representative systems and methods, and illustrative examples shown and described above. Various modifications and variations may be made to the above specifications without departing from the scope or spirit of the disclosure, which is intended to come within the scope of the following claims and their equivalents. As a condition, it is intended to cover all such modifications and variations.

Claims (22)

An apparatus for producing biodegradable material, said apparatus comprising:
A first unit for receiving a first material, wherein said first unit includes a fiber catcher for capturing some of the fibers in said first material. 1 unit;
a second unit for interlocking some of said fibers;
a third unit for interlocking a second material and some of said fibers, said second material and some of said fibers forming a third material; and said third material. a water removal unit for reducing the moisture content in
equipment, including 2. The apparatus of claim 1, further comprising a former for forming said third material after said water removal unit, wherein said former applies heat and pressure to said third material. 2. The apparatus of claim 1, wherein said first material comprises a pulp suspension. 2. The apparatus of claim 1, wherein the second material comprises fibrillated cellulose slush after grinding. 2. The apparatus of claim 1, wherein said third unit includes a container for holding said second material. 6. The apparatus of claim 5, wherein said third unit includes a heating element. 7. The apparatus of claim 6, wherein said heating element is configured to maintain a temperature of said second material of at least about 40<0>C. 7. The apparatus of claim 6, wherein the heating element is configured to warm the temperature of the second material to at least about 40<0>C when the surface material engages the first material. 4. The third material is generally free of chemical additives adapted to improve tensile strength, enhanced oil barrier, gas and/or liquid impermeability, tensile modulus, or tensile index. 1. The device according to claim 1. The third material is
an oxygen transmission rate of about 8000 cm ³ m ⁻² 24 h ⁻¹ or less; a water vapor transmission rate of 3000 g m ⁻² 24 h ⁻¹ or less;
dry tensile strength of about 30 MPa or greater;
a dry tensile modulus of about 4 GPa or greater, and a dry tensile index of about 45 Nm g ⁻¹ or greater;
2. The apparatus of claim 1, comprising the property of The third material is
wet tensile strength of about 5 MPa or greater;
a wet tensile modulus of about 0.4 MPa or greater, and a wet tensile index of about 5 Nm g ⁻¹ or greater;
2. The device of claim 1, comprising the additional property of 2. The device of claim 1, wherein the third material comprises fibrillated cellulose of different diameters having a weight ratio of 1:100 or 1:50. 2. The device of claim 1, wherein said third material comprises fibrillated cellulose having a diameter of about 1-10000 nanometers (nm). Clause 1, wherein the third material comprises fibrillated cellulose having about 0.1-1000 microns, about 10-500 microns, about 1-25 microns, or about 0.2-100 microns. The apparatus described in . 3. The apparatus of claim 1, wherein said third material constitutes a flat sheet. 3. The apparatus of claim 1, wherein the third material constitutes a container for edible items. 2. The device of claim 1, wherein said third material constitutes a fibrillated mixture. 2. The apparatus of claim 1, wherein the third material constitutes a film having a thickness of approximately 0.01-3.0 millimeters (mm). 16. The apparatus of claim 15, wherein said flat sheet comprises a length ranging from 0.01 mm to 10000 mm. An apparatus for producing biodegradable material, said apparatus comprising:
a second unit for engaging a second material;
a third unit for vacuum intermeshing said second material to form a third material; and a water removal unit for reducing moisture content in said third material;
equipment, including A method for producing a biodegradable material, said method comprising:
engaging the second material;
vacuum mating the second material to form a third material; and reducing the moisture content in the third material.
A method that encompasses A method for producing a biodegradable material, said method comprising:
receiving a first material in a fiber trap for trapping some of the fibers in said first material;
engaging the second material;
vacuum mating the second material to form a third material; and reducing the moisture content in the third material.
A method that encompasses

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