WO2022148357A1 - Chemical fibre material made of mixed polyester - Google Patents

Abstract

A chemical fibre material made of at least one polyester and at least one other polyester, a preparation method, and an application thereof. The chemical fibre material has desirable physical characteristics such as good dyeing properties and a good hand feel, and is industrially feasible and low cost. The present application also relates to a fabric and/or other product made of the chemical fibre material.

Description

A chemical fiber material made of mixed polyester technical field

The present application relates to a chemical fiber material made of mixed polyester, a preparation method and its application. The chemical fiber material uses at least one polyester and at least another polyester as raw materials, and physically mixes different polyesters before spinning to make a mixed polyester chemical fiber material. The present application also relates to yarns, fabrics and/or other articles made using the above chemical fiber materials.

Background technique

When polyester is used as a textile material, in order to ensure the uniformity of spinning quality, a single-component polyester is usually pursued, and the mixing of different polyesters is avoided as much as possible. Because it is generally accepted that physical mixing of different polyesters adversely affects the uniformity of the fibers, which in turn affects the properties of the manmade fiber material, such as dyeing properties.

Common polyester textile materials, such as polytrimethylene terephthalate (PTT), polyethylene terephthalate (PET), polybutylene terephthalate (PBT), etc., which can be individually , or together with other chemical fiber materials to make yarns, which are widely used in textiles and other end uses.

Some polyester textile materials, such as polytrimethylene terephthalate (PTT), are difficult to dye. Polytrimethylene terephthalate is usually dyed with disperse dyes. Commonly, the dyeing of polytrimethylene terephthalate fibers needs to be carried out under high temperature and high pressure conditions, such as 130°C.

SUMMARY OF THE INVENTION

technical problem

Different textile materials require different process conditions for dyeing. The dyeing of some polyesters, such as polytrimethylene terephthalate, requires higher temperature and pressure conditions. Other common materials, such as wool, are dyed under atmospheric pressure. Therefore, if it is desired to use polytrimethylene terephthalate fibers in fabrics together with other fibers that are dyed under atmospheric conditions, it is difficult to dye them. In particular, when polytrimethylene terephthalate fiber and wool are mixed, sweater factories usually do not have pressurized high-temperature dyeing tanks, and the addition of pressurized equipment will lead to a significant increase in cost.

In addition, in order to meet the higher temperature and pressure conditions required for the dyeing of polytrimethylene terephthalate fibers, the fibers may be damaged during high temperature and high pressure processing, thereby affecting other properties including softness, body bones, etc. . In particular, when polytrimethylene terephthalate fiber is mixed with other fiber materials, such as wool, nylon, etc., the higher temperature and pressure required for the dyeing of polytrimethylene terephthalate fiber will seriously damage other fibers The texture of the material (such as wool, nylon, etc.) causes the softness of the fabric to deteriorate and affects the hand feel.

Therefore, a chemical fiber material, especially an aromatic polyester material, which can be dyed under mild dyeing conditions and has good dyeing performance is desired. It is also desirable that other properties of the chemical fibers, such as strength, skeleton, dimensional stability, etc., are not degraded or perform better.

Technical solutions

The present application provides a chemical fiber material using at least one polyester and at least the other polyester as raw materials, and subjecting the at least one polyester and the at least one other polyester to physical processing before spinning. mix.

Preferably, the at least one polyester is an aromatic polyester; more preferably, the aromatic polyester is a polyalkylene terephthalate; further preferably, the polyalkylene terephthalate The acid ester is polytrimethylene terephthalate.

Preferably, the at least one other polyester is also an aromatic polyester; more preferably, the aromatic polyester is a polyalkylene terephthalate; further preferably, the polyalkylene terephthalate The phthalate is polybutylene terephthalate.

The aromatic polyesters mentioned in this application refer to those polyesters containing aromatic rings in their main chain or side chains, for example, polyethylene terephthalate (PET), polyethylene terephthalate (PET), polyethylene terephthalate (PET), polyethylene terephthalate (PET), Propylene terephthalate (PPT), butylene terephthalate (PBT), polyethylene terephthalate (PHT), etc.

Preferably, the one polyester and the at least one other polyester are physically mixed in a ratio of 1/99 to 99/1; Physically mixed in a ratio of 90/10; more preferably one polyester is physically mixed with said at least one other polyester in a ratio of 20/80 to 80/20; more preferably one polyester is physically mixed with said at least one other polyester The polyesters are physically mixed in a ratio of 30/70 to 70/30; more preferably one polyester is physically mixed with the at least one other polyester in a ratio of 40/60 to 60/40.

Preferably, polytrimethylene terephthalate is physically mixed with the at least one other polyester in a ratio of 1/99 to 99/1; more preferably polytrimethylene terephthalate and the at least one other polyester are mixed with Physically mixed in a ratio of 10/90 to 90/10; more preferably polytrimethylene terephthalate and said at least one other polyester are physically mixed in a ratio of 20/80 to 80/20; more preferably polyparaphenylene Trimethylene terephthalate and the at least one other polyester are physically mixed in a ratio of 30/70 to 70/30; 60/40 ratio physical mix.

Preferably, polytrimethylene terephthalate is physically mixed with the at least one other polyalkylene terephthalate in a ratio of 1/99 to 99/1; At least one other polyalkylene terephthalate is physically mixed in a ratio of 10/90 to 90/10; more preferably polytrimethylene terephthalate and said at least one other polyalkylene terephthalate The acid esters are physically mixed in a ratio of 20/80 to 80/20; more preferably polytrimethylene terephthalate and the at least one other polyalkylene terephthalate are mixed in a ratio of 30/70 to 70/30 The ratio is physically mixed; more preferably the polytrimethylene terephthalate is physically mixed with the at least one other polyalkylene terephthalate in a ratio of 40/60 to 60/40.

Preferably, polytrimethylene terephthalate and polybutylene terephthalate are physically mixed in a ratio of 1/99 to 99/1; more preferably polytrimethylene terephthalate and polybutylene terephthalate Esters are physically mixed in a ratio of 10/90 to 90/10; more preferably polytrimethylene terephthalate and polybutylene terephthalate are physically mixed in a ratio of 20/80 to 80/20; more preferably Physical mixing of polytrimethylene terephthalate and polybutylene terephthalate in a ratio of 30/70 to 70/30; more preferably polytrimethylene terephthalate and polybutylene terephthalate Physically mix in a ratio of 40/60 to 60/40.

Preferably polytrimethylene terephthalate and said at least one other polyalkylene terephthalate are 10/90, 30/70, 20/80, 40/60, 50/50, 60/40, Physical mixing in a ratio of 70/30, 80/20 or 90/10; particularly preferably polytrimethylene terephthalate and polybutylene terephthalate in a ratio of 10/90, 30/70, 20/80, 40 /60, 50/50, 60/40, 70/30, 80/20 or 90/10 ratio physical mixing.

The chemical fiber material containing one polyester and at least one other polyester described in this application may also contain other ingredients, including but not limited to a third or more polyesters, other polyester additives, unless they will Detract from the advantages of this application. The additives, such as matting agents (eg titanium dioxide), heat stabilizers, antioxidants, antistatic agents, ultraviolet light absorbers, antibacterial agents, or various pigments, or other functional additives.

On the other hand, the chemical fiber material containing one polyester and at least one other polyester described in this application may contain one aliphatic polyester, such as polylactic acid, and at least one other polyester, such as aromatic Group polyester, thereby improving the properties of chemical fiber materials, such as dyeing properties.

The present application also provides a process for the preparation of a textile material that mixes different polyesters using at least one polyester, such as polytrimethylene terephthalate, with at least one other polyester, such as polybutylene terephthalate Diol esters are used as raw materials to physically mix different polyesters, and the obtained mixed materials are made into chemical fiber materials. Specifically, the obtained mixed material is heated and extruded to obtain a melt of the mixed material. The melt of the mixed material can further be made into a mixed polyester chemical fiber material through a spinning assembly.

The method for obtaining the mixed polyester chemical fiber material of the present application is not particularly limited. For example, the different polyesters can be (1) pre-blended in a separate unit, then heated and extruded, and (2) mixed at the same time as the heating and extrusion.

In a preferred embodiment, the one polyester, eg, polytrimethylene terephthalate, is combined with at least one other polyester, eg, polybutylene terephthalate, in polyester pellets ("polyester pellets"). The "grain" in the text is not intended to limit the shape, and the "grain" includes products called "chips", "flakes", etc.), which are physically mixed in the following way, in the process of conveying different polyester pellets to the silo Perform physical mixing. Thereafter, the mixed material is heated, extruded, and the melt is passed through a spinning assembly, such as a spinneret, to form a mixed polyester chemical fiber material.

In a preferred embodiment, the one polyester, eg, polytrimethylene terephthalate, is physically mixed with at least one other polyester, eg, polybutylene terephthalate, in a manner such that: The different polyester pellets are physically mixed during the transfer from the silo to the feed port of the extruder. The physical mixing can take place before or after the polyester is dried. After that, the mixed material is heated and extruded, and the melt is passed through a spinning assembly to make a mixed polyester chemical fiber material.

In a preferred embodiment, the one polyester, eg, polytrimethylene terephthalate, is physically mixed with at least one other polyester, eg, polybutylene terephthalate, in such a manner that one of The polyester pellets are fed normally, and at least one other polyester pellet is side-fed into the extrusion system for physical mixing. After being heated and extruded, the melt of the mixed material is passed through a spinning assembly to make a mixed polyester chemical fiber material.

The heating and extrusion temperature is usually lower than about 300°C, preferably about 245-260°C.

The mixed polyester chemical fiber material may be long fiber, short fiber and/or other forms of material.

The mixed polyester filaments can be monocomponent filaments of uniform composition, and/or can be combined with other fiber material yarns to form multicomponent composite fibers, such as bicomponent composite filaments. The conjugated fibers may be, for example, side-by-side conjugated fibers, sea-island conjugated fibers, and/or daisy-shaped conjugated fibers. The mixed polyester can be used as an integral part of the fiber to form a composite fiber, such as a side-by-side composite fiber, together with PET.

The mixed polyester staple fiber material can be made into yarns alone and/or blended with other fiber materials to make yarns.

The mixed polyester chemical fiber material can be further made into fabrics and/or other products.

In a preferred embodiment, the mixed polyester chemical fiber material containing polytrimethylene terephthalate and at least one other polyalkylene terephthalate is short fiber, which is further combined with wool or other fibers such as Cotton, viscose, nylon, acrylic, etc. are blended to make fabrics.

In a preferred embodiment, the mixed polyester chemical fiber material containing polytrimethylene terephthalate and at least one other polyalkylene terephthalate is made into fully drawn yarn (FDY), or Partially oriented yarn (POY), or stretch textured yarn (DTY), or other forms of yarn, and further chemical fiber materials are co-spun with other materials to form composite fibers. In a preferred embodiment, the full-drawn yarn containing mixed polyester chemical fibers and the stretch-textured yarn of polyethylene terephthalate are made into a bicomponent composite length in a ratio of 50/50. Silk.

The present application also relates to fabrics and/or other articles containing the aforementioned textile materials. Fabrics can be knitted, woven and non-woven.

The present application also relates to a method for dyeing textile materials, the method comprising adding at least one polyester by physical mixing as a raw material to at least one polyester, the at least one polyester and the at least one other polyester The polyester is physically mixed to obtain a mixed material, the melt of the mixed material is made into a textile material, and then the textile material is dyed at a temperature lower than 130° C. under normal pressure. Preferably, the dyeing treatment can be performed at 90°C-100°C, for example, 95°C, using the method of the present application.

In a preferred embodiment, the method for dyeing textile materials comprises adding at least one further polyester as a raw material by physical mixing in polytrimethylene terephthalate. Preferably the at least one other polyester is a polyalkylene terephthalate, more preferably it is a polybutylene terephthalate.

beneficial effect

One advantage of the present application is that, although the chemical fiber material described in the present application is physically mixed with different polyesters, surprisingly, it can still obtain a melt with a good degree of uniformity, and can produce uniform fibers with Good workability.

The chemical fiber material described in this application has lower raw material cost and processing cost, can be dyed at lower temperature and normal pressure, and has better color after dyeing, stronger tinting strength and better color fastness.

Another advantage of the present application is that the chemical fiber material and the textile material comprising the chemical fiber material described in the present application also have excellent physical properties, such as good softness and smoothness, good body bones, and dimensional stability. Good performance, and not easy to pilling.

The dyeing of the chemical fiber material described in the present application can be completed at a relatively low temperature and normal pressure, without the use of pressurized equipment, lower requirements for equipment, great cost savings, and better safety.

While not wishing to be bound by any theory, it is believed that the physical mixing of the different polyester materials can affect the crystallinity of the polyester materials to achieve superior dyeing results under milder conditions.

At the same time, the chemical fiber material of the present application has a relatively low oligomer content, which can improve the problem of excessive cyclic dimers caused by polytrimethylene terephthalate alone and pollute processing equipment, and has good processing performance. feasibility.

In addition, the present application only needs to perform simple physical mixing of different polyester particles during spinning production, and additional melt blending processing steps for different polyesters may not be performed outside spinning, which is further beneficial to the simplification of the process and the cost of It reduces and avoids the damage to textile materials caused by the high temperature and high pressure dyeing process.

Description of drawings

FIG. 1 is the dyeing result of the fabric of the mixed polyester chemical fiber material of the present application in Example 2. FIG.

FIG. 2 is the dyeing result of the fabric of the PBT/PTT mixed polyester chemical fiber material in Example 3. FIG.

FIG. 3 is the dyeing result of the yarn socks of the PBT/PTT mixed polyester chemical fiber material in Example 3. FIG.

Detailed ways

In the absence of the contrary, "polytrimethylene terephthalate" (PTT) is meant to include homopolymers and copolymers containing at least 70 mole percent repeating units of trimethylene terephthalate and containing at least 70 mole percent Polymer composition of polymers or copolyesters. Preferred polytrimethylene terephthalates contain at least 85 mole %, more preferably at least 90 mole %, still more preferably at least 95 mole % or at least 98 mole %, and most preferably about 100 mole % repeats of trimethylene terephthalate unit. The 1,3-propanediol used in the manufacture of PTT is preferably biochemically obtained from renewable sources. Commercially available polytrimethylene terephthalate resins include, but are not limited to, DuPont's

The intrinsic viscosity of the polytrimethylene terephthalate used in this application is preferably in the range of 0.7-1.3 dL/g.

Intrinsic viscosity (IV) is a measure of polymer molecular weight and can be measured according to ASTM D 5225. Intrinsic viscosity generally increases as the molecular weight of the polymer increases, but also depends on the type of polymer, its shape or conformation, and the solvent used for the measurement.

Where not indicated to the contrary, "polyethylene terephthalate" (PET) is meant to include both homopolymers and copolymers containing at least 70 mole % repeating units of ethylene terephthalate and containing at least Polymer composition of 70 mole % homopolymer or copolyester. Preferred polyethylene terephthalates contain at least 85 mole %, more preferably at least 90 mole %, still more preferably at least 95 mole % or at least 98 mole %, most preferably about 100 mole % ethylene terephthalate Diol ester repeating unit.

Where not indicated to the contrary, "polybutylene terephthalate" (PBT) is meant to include homopolymers and copolymers containing at least 70 mole % repeating units of butylene terephthalate and containing at least Polymer composition of 70 mole % homopolymer or copolyester. Preferred polybutylene terephthalates contain at least 85 mole %, more preferably at least 90 mole %, still more preferably at least 95 mole % or at least 98 mole %, most preferably about 100 mole % butyl terephthalate Diol ester repeating unit.

For convenience, where "PTT", "PBT" or "PET" is mentioned in the text, it refers to polytrimethylene terephthalate, polybutylene terephthalate, or polyethylene terephthalate, respectively alcohol ester.

The manufacture of polyesters, such as polytrimethylene terephthalate, polybutylene terephthalate or polyethylene terephthalate, is well known to those skilled in the art and is omitted in this specification for the sake of brevity. to further describe.

The term "yarn" refers to a continuous bundle of twisted threads of natural or synthetic material (eg, wool, nylon, or polyester) used for weaving or weaving. Yarns such as fully drawn yarns (FDY), partially oriented yarns (POY), shaped yarns (SAY), stretch textured yarns (DTY), air textured yarns (ATY), composite fibers and blended yarns, etc.

All percentages, parts, ratios, etc. are by weight unless otherwise indicated.

Preparation of chemical fiber materials

Unless otherwise indicated, the samples and controls in the Examples were prepared as follows.

The preparation of spinning includes mixing at least one polyester pellet, such as PTT polyester chip, and at least one other polyester particle, such as PBT polyester chip, in different ratios, such as 10/90, 20/80, 30/ 70, 40/60, 50/50, 60/40, 70/40, 80/20 and 90/10, put into the feed port of the screw extruder after physical mixing. After the material is sheared and melted in the extruder, a mixed polyester melt, such as a PTT/PBT mixed polyester melt, is obtained, and the mixed polyester melt is transported to the spinning assembly by a pump.

The mixed polyester melt can be passed through the spinning pack alone, bundled into strands to make long fibers, or cut into short fibers.

Blended polyester melts can also be co-formed with melts of other polyester fiber materials to form composite fibers. At this time, at least two extruders are used. For example, in one of the extruders, using the above method, at least one polyester pellet, such as PTT polyester chips, and at least one other polyester pellets, such as PBT polyester chips, in different proportions, through After physical mixing, it is put into the feed port of the screw extruder. After the material is melted by shearing in the extruder, a uniformly mixed polyester melt, such as a PTT/PBT mixed polyester melt, is obtained. In another extruder, use another or more polyester pellets, such as PET polyester chips, and put them into the feed port of the screw extruder. After the material is sheared and melted in the extruder, a uniform Polyester melts, such as PET polyester melts. The resulting mixed polyester melt and the single polyester melt are further co-passed through a spin pack to form composite fibers, such as bicomponent composite filaments.

The controls were prepared in essentially the same way as described above, with the difference that the mixed polyester melts were prepared using different types of polyesters that were physically mixed in the feed, while the controls were prepared using only one polyester alone. For example, PTT polyester chips are used alone and put into the feed port of the screw extruder. After the single polyester material is sheared and melted in the extruder, a polyester melt of the reference substance is obtained, and the polyester melt of the reference substance is transported to the spinning assembly by a pump.

The reference polyester melt can be passed through the spinning pack alone, bundled into a sliver to make long fibers, or cut into short fibers. The polyester melt of the reference substance can also be made into a composite fiber with the melt of other polyester fiber materials by the above method.

Representation of basic features

Unless otherwise indicated, the corresponding parameters of the samples and controls in the examples were determined as follows.

The breaking strength ("Tenacity@break/cN/dtex"), elongation at break ("Elongation@break/%") and Young's Modulus (Young's Modulus/cN) of the samples were tested by GB/T14344-2008 method .

The fiber boiling shrinkage % test is carried out by the following method. Take a certain length of fiber, knot it at the beginning and end, and measure the length by hanging the tension. Then put it into boiling water at 95-100 °C for 30 minutes, take it out and dry it, and then measure the length again. Calculate the shrinkage, that is, the fiber boiling shrinkage %.

Shrinkage (%) was measured using the AATCC 135 method.

The ASTMD3107 method was used to measure the elongation of the sample under stress ("Fabric stretch/%"); after the fabric was dyed, the ASTMD3107 method was used to measure its elasticity after dyeing (Stretch after dyeing/%).

The degree of curl was measured by the following method. Wind the sample and control substance, take off the wire that has been wound, and tie the ends. Then add an initial load of 7.5g (for example for 5550dtex filament) on the bottom of the filament, measure the initial length Cb, accurate to 1mm. Lightly add a heavy load of 500g to the initial load, and after balancing for 45 seconds, measure the length Lb, accurate to 1mm. The heavy load was removed, the strands were hung on a rack, and the rack was placed in a 121°C oven to dry for 30 minutes. The filaments were taken out from the oven and cooled to room temperature, and then placed in a constant temperature and humidity environment (temperature 21° C., humidity 65%) for 2 hours. Then measure its length Ca, accurate to 1mm. Then lightly add a heavy load, and measure the length La after balancing for 45 seconds, accurate to 1mm. Remove the heavy load and measure the length Cc after equilibrating for 10 minutes, accurate to 1mm.

The above measured values were put into the following formula to calculate the shrinkage %CS, the curling ratio %CCb before heating, and the curling ratio %CCa after heating.

Shrinkage %CS=(Lb-La)/La*100%;

The crimp ratio % includes CCb=(Lb-Cb)/Lb*100% (before heating) and CCa=(La-Ca)/La*100% (after heating).

Characterization of anti-pilling properties

Unless otherwise specified, the method of GB/T 4802.3 ICI 7200/14400 was used to evaluate the anti-pilling properties of the samples and controls in the examples.

Characterization of dyeing properties

The color depth ("Color Shade") adopts the human eye observation evaluation method.

The evaluation of color fastness ("Color fastness") adopts AATCC 8/ATTCC 61 method to measure color change, degree of staining, dry rubbing fastness and wet rubbing fastness, respectively.

The % staining intensity ("Dyeing Str") of the samples and to the photographs in the examples was measured using a spectrophotometer. According to the Kubelka-Munk equation, K/S=(1-Rλ) ² /2Rλ, where K is the constant that dyed fabrics absorb light; S is the constant that dyed fabrics scatter light; R is the reflectance of dyed fabrics, expressed in relative proportions. The larger the K/S value, the darker the color; the smaller the K/S value, the lighter the color.

The L, a, b values of the dyed samples were measured using the instrument LabScan XE Spectrophotometer.

The examples given below are only to illustrate the present application and are not intended to be limiting. Although suitable methods and materials are described herein, methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present application. All parts, percentages, etc. are by weight unless otherwise indicated.

Example:

Example 1: Preparation and physical property test of PBT/PTT mixed polyester chemical fiber

1.1 Preparation and performance characterization of monocomponent filaments of uniform composition

Polytrimethylene terephthalate (commercially available trade name

Intrinsic viscosity of 1.02) chips and polybutylene terephthalate chips (intrinsic viscosity of 1.10) were physically mixed in different proportions, and the mixed polyester chips were put into the extruder from the feed port. The extruder is a single-screw extruder, which is divided into three temperature zones. The mixed polyester raw materials are heated and sheared in the extruder, melted and then passed through the spinning assembly and extruded from the spinneret. The first drawing roll and the second drawing roll are drawn and finally wound to form a fully drawn yarn (FDY) sample.

The polytrimethylene terephthalate chips alone were used as the raw material and put into the extruder, as the control polytrimethylene terephthalate fully drawn yarn. The polybutylene terephthalate chips alone were used as the raw material and put into the extruder, as the control polybutylene terephthalate fully drawn yarn. The fully drawn yarn specifications are all 75D/72f (the yarn thickness is 75 denier, and the number of spinneret holes is 72). The process parameters of samples and reference substances are shown in Table 1.

Table 1 Process parameters of single-component filament samples and reference materials with different PBT/PTT ratios

It was observed that fully drawn yarn (FDY) samples with uniform evenness were obtained.

Further, the properties of the above-mentioned fully drawn yarns were analyzed, and the results obtained are shown in Table 2.

Table 2 Properties of single-component filament samples and controls with different PBT/PTT ratios

The partially fully drawn yarn (FDY) samples obtained above and the control were further knitted into socks, and the socks were dyed. Dyeing adopts the condition of keeping 100℃ for 45min. The specific heating, cooling and post-processing procedures go through the following steps: at room temperature, at a rate of 1℃/min, heat up to 40℃ and hold for 10min, and then continue to increase the temperature at a rate of 1℃/min. to 70°C and hold for 10min, and finally heated to 100°C for 45min at a rate of 1°C/min, then cooled to 80°C at 2-3°C/min, treated with 1g/L soda ash for 10min at 80°C, and then After treatment with 1g/L neutral washing solution for 10min, and finally washing with water at room temperature for 5min to complete the dyeing. The dye used Zhejiang Deou Chemical Manufacturing Co., Ltd., disperse brilliant blue E-4R, 1.2% concentration through the same dyeing process, the color depth obtained by some experimental samples and control samples was measured, the results are shown in Table 3.

Table 3 Dyeing properties of single-component filament samples and controls containing different PBT/PTT ratios

The above color depth results show that the mixed polyester chemical fiber material has better dyeing effect, the color depth value is higher, and when different polyesters are mixed in a large proportion, that is, when the mixing ratio is close to 50/50, the effect of dyeing deepening is more obvious. At this time, the dyeing effect is better than the dyeing effect when different polyesters are mixed in a small proportion, that is, when the mixing ratio is far from 50/50.

1.2 Preparation and performance characterization of bicomponent composite filament

Similar to the preparation method described in section 1.1 of Example 1, polytrimethylene terephthalate (commercially available trade name

Intrinsic viscosity of 1.02) chips and polybutylene terephthalate chips (intrinsic viscosity of 1.10) were physically mixed in different proportions, and the mixed polyester chips were put into the extruder from the feed port. The extruder is a single-screw extruder, which is divided into three temperature zones. The mixed polyester raw materials are heated, sheared and melted in the extruder.

The difference is that the resulting mixed polyester melt is coextruded with a PET melt that has been heated, sheared and melted in another extruder, then passed through a spin pack and extruded from a spinneret. According to this method, the mixed polyester and PET in a ratio of 50/50 are made into two-component composite filaments. The bicomponent composite filaments are fully drawn yarn (FDY) samples.

The polytrimethylene terephthalate chips were used alone as the raw material to be put into the extruder, and the fully drawn yarn samples of PTT and PET bicomponent composite filaments with a ratio of 50/50 were prepared according to the above method as a control. The polybutylene terephthalate chips were used alone as the raw material to be put into the extruder, and a fully drawn yarn sample of PBT and PET bicomponent composite filaments in a ratio of 50/50 was prepared as a control according to the above method. The bicomponent composite filament was a fully drawn yarn (FDY) reference.

The parameters shown in Table 4 were used for the fully drawn yarn samples of the above-mentioned bicomponent composite filaments and the reference, and the specifications were both 75D/36f.

The process parameters of table 4 bicomponent composite filament sample and reference substance

Further, the properties of the above two-component composite filament samples were analyzed, and the results obtained are shown in Table 5.

Table 5 Properties of bicomponent composite filament samples and controls

1.3 Preparation and performance characterization of woven fabrics

The bicomponent composite filaments obtained above (experimental sample 1-2-1, experimental sample 1-2-2, experimental sample 1-2-3 and experimental sample 1-2-4) and PET yarn were woven together into woven cloth.

The weaving method of the fabric: the warp direction adopts the PET stretched textured yarn with the specification of 75D/72f, and the weft direction adopts the bicomponent composite filament with the specification of 75D/36f obtained above and the PET with the specification of 150D/288f to stretch Textured yarn, the ratio of the two is 3:1.

In contrast, polytrimethylene terephthalate chips were used alone as raw materials to be put into the extruder, and the two-component composite filaments of PTT and PET were made according to the above method, wherein the ratio of PET to PTT was 60/40. Then, using the same fabric weaving method as above, the obtained fully drawn yarns of the bicomponent composite filaments were mixed and woven to make a woven fabric, which was used as a control woven fabric.

The physical properties of the obtained fabric were analyzed, and the results are shown in Table 6.

Table 6 Two-component composite filament samples and physical properties of fabrics made from photos

1.4 Dyeing elasticity of bicomponent composite filament yarn fabrics

Part of the 75D bicomponent composite filament samples obtained above (experimental sample 1-2-2 and experimental sample 1-2-4) and control substances (control sample 1-2-5 and control sample 1-2-6) were used as weft yarn. Another 150D PET stretch-textured yarn was selected as the warp yarn, and the above-mentioned warp and weft yarns were woven with different weaving densities to obtain fabric samples with different tightness. is 3/2RH Twill.

The obtained fabric samples were dyed and their elasticity after dyeing was measured, as shown in Table 7 below.

Table 7 Elasticity after dyeing

Based on the above experimental results, it can be found that the mixed polyester chemical fiber material of the present application can obtain uniform materials and uniform fibers even though physical mixing of different kinds of polyesters is carried out for feeding. Its technological parameters such as spinning speed are acceptable in industry and are comparable to those of existing common textile materials. The mixed polyester chemical fiber material of the present application can achieve a good dyeing effect, and at the same time, its physical properties such as strength, elasticity, and shrinkage characteristics are also acceptable.

Example 2: Samples and properties of PTT mixed with different polyesters

Referring to the method in Example 1, PTT/PBT mixed polyester chemical fibers and PTT/PET mixed polyester chemical fibers were obtained. The chemical fiber using PTT alone was used as a control. The yarns of the above three kinds of chemical fiber materials are prepared by the same processing technology, and are further made into fabrics. Fabric specifications are 40s (40).

The obtained fabric was dyed, and the dyeing was carried out at a temperature of 90° C., and the procedures of heating, cooling and post-treatment were referred to the steps in Example 1. The dye is 3% Navy Blue. The dyed fabric is obtained by finishing after dyeing. The dyeing effect is shown in Figure 1.

For the above-mentioned PTT/PBT mixed polyester chemical fiber, PTT/PBT mixed polyester chemical fiber, and the control using PTT alone, the breaking strength, elongation at break, shrinkage of boiling width, pilling rating, and dyeing strength were measured. The results are as follows shown in Table 8.

Table 8 Properties of different polyester blend samples

sample	Experimental sample 2-1	Experimental sample 2-2	Control 2-3
Fiber composition	PTT/PBT ratio 50/50	PTT/PET ratio 50/50	PTT alone
Breaking Strength (cN/Tex)	13.3	21.6	16
Elongation at break%	33	28.7	49.2
Fiber Boiling %	11.7	15.1	8.7
pilling pilling rating	2	3	2-3
Dyeing Intensity %	100%	70%	18%

To sum up, it can be seen that adding a certain proportion of other polyesters in pure PTT in the form of physical mixing can significantly improve the dyeing strength. The better performance is acceptable in industry and has extremely high feasibility.

In particular, the incorporation of PBT into PTT resulted in relatively better depth of dyeing compared to the incorporation of PET into PTT.

Example 3: Dyeing properties of mixed polyester chemical fibers

3.1 The dyeing color of the mixed polyester chemical fiber material in this application

The mixed polyester chemical fiber material with the PBT/PTT mixing ratio of 40/60 is prepared with reference to the process in Example 1, and the obtained mixed polyester chemical fiber material is spun to make single-component yarn, warp knitted socks and socks. Dyeing in a cylinder to obtain dyed samples of mixed polyester chemical fiber materials.

Socks were dyed at 95°C for 45min. Refer to the steps in Example 1 for the heating, cooling and post-processing procedures. The dye concentration is 2%.

The same process was used, but instead of using a PBT/PTT blend polyester, PBT and PTT alone were used as controls. Through the same spinning, hosiery and hosiery dyeing process, pure PBT dyeing control substance and pure PTT dyeing control substance were obtained.

The L, a and b values were measured for the dyed samples and controls, and the results are shown in Table 9.

Table 9 Dyeing color

To sum up, it can be found that compared with the pure PBT control and pure PTT control, the dyed samples of mixed polyester chemical fibers have achieved better dyeing color. Hybrid polyester dyed samples have lower L values in any of the above colors; in some colors, mixed polyester dyed samples have higher a-values, and in some colors, mixed polyester dyed samples have higher b value.

3.2 The dyeing results of the mixed polyester chemical fiber material in this application under different dyeing processes

Referring to the method in Example 1, the woven fabrics of experimental sample 1-3-1, experimental sample 1-3-2, experimental sample 1-3-3 and experimental sample 1-3-4 were prepared; high-pressure dyeing was performed to obtain High pressure dyeing sample 3-2-1, high pressure dyeing sample 3-2-2, high pressure dyeing sample 3-2-3 and high pressure dyeing sample 3-2-4.

The high-pressure dyeing method is as follows: the dye is added at 60°C, then the temperature is increased to 98°C at a rate of 1.5°C/min, maintained for 15min, and then the temperature is further increased to 135°C at a rate of 0.7°C/min and maintained for 45min, and finally The dyeing was completed by cooling to 80°C at a rate of 2°C/min.

The control sample 1-2-5 bicomponent composite filament and the control sample 1-2-6 bicomponent composite filament were used to make woven fabrics in the same way, and high-pressure dyeing was carried out under the same conditions to obtain PBT respectively. High pressure staining control and PTT high pressure staining control.

The obtained high-pressure dyeing samples of mixed polyester chemical fibers, PBT high-pressure dyeing reference substance and PTT high-pressure dyeing reference substance, the color depth results are shown in Table 10. The dyeing effect is shown in Figure 2.

Table 10 Color depth of high pressure dyeing

Referring to the method in Example 1, the mixed polyester chemical fiber materials with the ratios of PBT and PTT of 80/20 and 60/40 were prepared respectively. The obtained mixed polyester chemical fiber material is then spun into a bicomponent composite filament with PET yarn in a ratio of 50/50.

PBT and PTT were used alone and spun together with PET in a 50/50 ratio to make bicomponent composite filaments as a control.

The above two-component composite filament yarn samples and controls were knitted, woven into hosiery, and then dyed by hosiery, and the obtained samples and controls were dyed at normal pressure. The dyeing method is the same as that of the sock dyeing method in Example 1. The results obtained are shown in Figure 3, and the color depths are shown in Table 11.

Table 11 Color depth of atmospheric dyeing

Mixed polyester chemical fiber composition (PBT-PTT)	0/100	60/40	80/20	100/0
Two-component composite filament composition (PET/PBT-PTT)	50 (0/50)	50/(30/20)	50/(40/10)	50/5 (0/0)
color depth	2.5	4.5	4.0	3.5

To sum up, under the condition of normal pressure (100°C), good dyeing can be obtained by mixing polyester chemical fiber material, without dyeing under high pressure (135°C); while the control product cannot obtain good dyeing under normal temperature and pressure.

In addition, the above results show that the mixed polyester chemical fiber material exhibits better dyeing effect and higher color depth regardless of whether it is dyed under normal pressure or under high pressure. At the same time, when the two are mixed in a larger proportion close to the average, the strengthening effect of the dyeing effect is better than the mixing of the two in an uneven smaller proportion. For example, a 50/50 mix is significantly better than 40/60; a 40/60 mix is significantly better than 30/70 or 70/30.

It is believed that the physical mixing of PTT and PBT followed by charging can affect the crystallization of the entire melt system, and when the degree of stable crystallization is reduced, it is easier to dye, and under relatively mild conditions, such as normal pressure or lower temperature, i.e. Can form a good dyeing effect. When the two are mixed in a larger proportion, the stable crystallization will be reduced to a greater extent than that in a small proportion. Therefore, when the two are mixed in a larger proportion, the dyeing effect will be better.

In the field of textile dyeing, when using disperse dyes for dyeing, the dyeing temperature below 100 ℃ is used, and no pressure is required. However, if the chemical fiber material requires higher dyeing temperatures, pressurized equipment is required. High temperature and high pressure not only increase the complexity of the process, but also increase the cost, and also bring adverse effects on the properties of the fiber. Therefore, the dyeing effect of the mixed polyester chemical fiber at lower temperature and normal pressure is significantly better than that of the control group, which can solve the dyeing difficulty of textile materials. At the same time, since a good dyeing effect is obtained, it is not necessary to experience the dyeing conditions of high temperature and high pressure, so other properties of the textile material can also be prevented from being damaged due to the high temperature and high pressure.

3.3 The color fastness of the mixed polyester chemical fiber material in this application

A mixed polyester chemical fiber material with a PBT/PTT ratio of 50/50 prepared by the method in Example 1 was used. The melt of mixed polyester chemical fiber material is made into staple fiber. In a ratio of 70/30, bamboo fiber staple fibers and the above-mentioned PBT/PTT mixed polyester staple fibers were blended to form a blended yarn sample (hereinafter referred to as "70/30 bamboo fiber/polyester blended yarn").

Using pure PTT yarn as a control, the same bamboo fiber staple fiber and pure PTT yarn were blended in a 70/30 ratio to make a blended yarn sample (hereinafter referred to as "70/30 bamboo fiber/PTT yarn blended yarn") .

The above-mentioned 70/30 bamboo fiber/polyester blended yarn and 70/30 bamboo fiber/PTT yarn blended yarn are woven into knitted fabrics (hereinafter referred to as "70/30 bamboo fiber/polyester blended") in the same way. Blended Yarn Knitted Fabric" and "70/30 Bamboo Fiber/PTT Blended Yarn Knitted Fabric"), both specifications are 30s (30 counts).

The obtained knitted fabric was dyed at 110° C. and 100° C. respectively, and the steps in Example 1 were referred to for the heating, cooling and post-treatment procedures. The color fastness of the dyed knitted fabrics was evaluated using the AATCC 8/ATTCC 61 method, and the results are shown in Table 12 below.

Table 12 Color fastness

The above results show that the textile material made of the mixed polyester chemical fiber material of the present application has good color fastness, which is basically equivalent to the color fastness of the existing PTT textile material.

It is generally required in the art that the color change of the textile material is >= 4, and the degree of staining is >= 3. It can be seen from this that the color fastness of the textile material of the present application can meet the requirements.

Example 4: Properties of Hybrid Polyester Chemical Fiber Blended Fabric

Blended textile materials are common in the art, and different textile materials have different handfeel. Different textile materials, such as wool with excellent hand, acrylic with bulky but rough hand, nylon with waxy feel, and the mixed polyester chemical fiber material of the present application, were used to make blended yarns, and their properties were evaluated. Compared with the aforementioned existing fabric materials, such as wool, acrylic and nylon, the mixed polyester chemical fiber material has a moderate hand feeling.

4.1 Preparation of blended fabrics

A mixed polyester chemical fiber material with a PBT/PTT ratio of 50/50 prepared by the method in Example 1 was used. The melt of the mixed polyester chemical fiber material is made into short fibers (hereinafter referred to as "mixed polyester fibers").

The blended yarns were prepared according to the yarn compositions in Table 13, and the blended yarns were further made into blended fabrics, all with a common count of 42Nm.

Table 13 Yarn composition of blended fabrics

blended fabric	Blended Yarn Composition
Sample 4-1-1	50% wool, 50% PBT/PTT blended polyester (50/50 blend of PBT and PTT)
Control substance 4-1-2	50% wool, 25% acrylic, 25% nylon
Control 4-1-3	50% wool, 50% PET

4.2 Hand feel of blended fabrics

The hand of the above-mentioned blended fabric was analyzed. The blended fabric samples and controls were analyzed for toughness, smoothness, and softness using the AATCC 202 standard test method, and the results are shown in Tables 14 to 16 below.

Table 14 Toughness of blended fabrics

The above toughness results show that the blended fabric sample 4-1-1 is more tough. The blended polyester chemical fiber material of the present application can bring better toughness value to the blended fabric.

According to the minimum requirements of ASTM, using 5 samples, based on the D.F value and the 0.050 significance level, the key value Tc=2.306, it is considered that:

Blended fabric sample 4-1-1 has a statistically significant difference in toughness from blended fabric control 4-1-2 as T=5.886>Tc.

The blended fabric control 4-1-3 of blended fabric sample 4-1-1 had a statistically significant difference in toughness because T=5.652>Tc.

There was no statistically significant difference in toughness between the blended fabric control 4-1-2 and the blended fabric control 4-1-3 because T=0.445<Tc.

Table 15 Softness of blended fabrics

The above softness results show that the blended fabric sample 4-1-1 has higher softness and is softer. The blended polyester chemical fiber material of the present application can bring better softness to the blended fabric.

According to the minimum requirements of ASTM, using 5 samples, based on the D.F value and the 0.050 significance level, the key value Tc=2.306, it is considered that:

There was a statistically significant difference in softness between the blended fabric sample 4-1-1 and the blended fabric control 4-1-2, as T=4.887>Tc.

The blended fabric control 4-1-3 of blended fabric sample 4-1-1 had a statistically significant difference in softness as T=4.788>Tc.

There was no statistically significant difference in softness between the blended fabric control 4-1-2 and the blended fabric control 4-1-3 because T=0.138<Tc.

Table 16 Smoothness of blended fabrics

The above softness results show that the blended fabric sample 4-1-1 has higher smoothness and is smoother. The blended polyester chemical fiber material of the application can bring better smoothness to the blended fabric.

According to the minimum requirements of ASTM, using 5 samples, based on the D.F value and the 0.050 significance level, the key value Tc=2.306, it is considered that:

The blended fabric sample 4-1-1 has a statistically significant difference in smoothness from the blended fabric control 4-1-2 because T=4.086>Tc.

The blended fabric control 4-1-3 of blended fabric sample 4-1-1 had a statistically significant difference in smoothness as T=3.604>Tc.

There was no statistically significant difference in smoothness between the blended fabric control 4-1-2 and the blended fabric control 4-1-3 because T=0.160<Tc.

Based on the above results, it can be found that, compared with the existing textile materials, the hybrid polyester chemical fiber material of the present application achieves better toughness, smoothness, softness, and better hand feeling.

4.3 Anti-fuzzing properties of blended fabrics

The anti-fuzzing properties of the blended fabric sample 4-1-1, the blended fabric reference 4-1-2 and the blended fabric reference 4-1-3 in this example were evaluated. Under the same conditions, the blended fabric sample 4-1-1, the blended fabric reference 4-1-2 and the blended fabric reference 4-1-3 were respectively made into fabric pieces and garment fabrics, and the obtained fabric pieces and garments were respectively The anti-pilling and anti-pilling properties were evaluated, and the pilling and pilling rating values were measured under different inversion numbers. The results are shown in Table 17.

Table 17 Pilling and pilling ratings of blended fabrics

The pilling characteristics of the blended fabric sample 4-1-1 were comparable to the two controls. To sum up, it can be seen that the mixed polyester chemical fiber material of the present application has good anti-pilling and pilling characteristics, which is comparable to the anti-pilling and pilling characteristics of existing common textile materials, and is acceptable.

4.4 Dimensional stability of blended fabrics

The method of AATCC 135 was used to evaluate the dimensional stability of the fabric sheets of the blended fabric sample 4-1-1, the blended fabric reference 4-1-2 and the blended fabric reference 4-1-3 in this example, under the following conditions The shrinkage rate was measured, and the results are shown in Table 18.

Table 18 Dimensional stability

A 70/30 bamboo fiber/polyester blended yarn knitted fabric was prepared by the method in Example 3, and its dimensional stability was evaluated. The method of AATCC 135 is used to measure the shrinkage (fabric shrinkage%) of 70/30 bamboo fiber/polyester blended yarn knitted fabric, and ISO 3005:1978 is used to evaluate the air permeability of 70/30 bamboo fiber/polyester blended yarn knitted fabric The dimensional shrinkage (fabric shrinkage %) after free-steaming is shown in Table 19.

Table 19 Dimensional stability

70/30 bamboo fiber/polyester blended yarn and 70/30 bamboo fiber/PTT yarn blended yarn were prepared by the method in Example 3, and their shrinkage properties were evaluated. 70/30 bamboo fiber/polyester blended yarn and 70/30 bamboo fiber/PTT yarn blended yarn are made into woven pieces, the specification of the woven piece is 44s/2 (44 counts/2 strands), respectively at 100 ℃ Treat under two dyeing conditions of 30min and 100°C for 45min, and then measure the shrinkage after washing with water (flat-laying and sun-drying).

Table 20 Shrinkage Properties

The above shrinkage results can all meet the industrial requirements, and compared with the existing textile materials, the hybrid polyester chemical fiber material of the present application can achieve less shrinkage. Therefore, the mixed polyester chemical fiber of the present application has good dimensional stability and has extremely high industrial feasibility.

Example 5: Oligomer content of mixed polyester chemical fiber material

According to the method in Example 1, PTT and PBT were mixed with polyester chemical fiber material in a ratio of 60/40, and the oligomer content in the mixed polyester chemical fiber was measured by NMR nuclear magnetic resonance method, and the control of using PTT resin alone The content of oligomers contained in the samples and the control samples using PBT resin alone were compared, and the results are shown in Table 21.

Table 21 Oligomer Content

fiber material	Oligomer content (wt%)
100% PTT resin reference	2.5
100% PBT resin reference	0.7
Hybrid polyester sample with PTT/PBT ratio of 60/40	1.8

It can be seen from the results in Table 21 that the mixed polyester chemical fiber material of the present application has a relatively low oligomer content. Oligomers tend to migrate to the surface during processing, which can cause equipment contamination. Therefore, the lower oligomer content of the mixed polyester chemical fiber of the present application will help to improve the problem of equipment pollution during processing and improve the processing feasibility.

Based on the above results, it can be seen that the mixed polyester chemical fiber material of the present application has better coloring properties, it can be dyed at lower temperature and normal pressure, the obtained color is excellent, and the color fastness is good. At the same time, other characteristic indexes are also acceptable in industry.

The mixed polyester chemical fiber material of the present application has better process performance, good industrial feasibility, and can save material cost. It can be directly used in the processing technology of existing textile materials, can be compatible with existing processing equipment of other textile materials, and can save processing costs. The hybrid polyester chemical fiber material of the present application also achieves good technical effects in terms of body bones, hand feel, softness, smoothness, dimensional stability and the like.

The mixed polyester chemical fiber material of the present application does not need to be under high temperature and high pressure to achieve good dyeing effect, so when it is blended with other textile materials, especially when blended with other textile materials with mild dyeing conditions, high temperature and high pressure dyeing can be avoided The process damages the textile fibers, which in turn is beneficial for the blended materials to obtain good physical properties.

The mixed chemical fiber material of the present application has good application prospects, it has good compatibility with other existing textile materials, such as wool, and can be processed into fabrics together with other existing textile materials to obtain Good compounding properties.

The above-described embodiments of the present application are for the purpose of illustration. It is not intended to be exhaustive, nor is it intended to limit the application to the strict forms disclosed. It will be apparent to those skilled in the art that many changes and modifications to the described embodiments can be made in light of the disclosure herein.

Claims (23)

1. A chemical fiber material using at least one polyester and at least one other polyester as raw materials, the at least one polyester and the at least one other polyester are physically mixed before spinning.
2. The chemical fiber material according to claim 1, wherein the one kind of polyester and the other kind of polyester are physically mixed in a ratio of 1/99 to 99/1.
3. The chemical fiber material of claim 2, wherein the at least one polyester is an aromatic polyester.
4. The chemical fiber material of claim 3, wherein the at least one other polyester is an aromatic polyester.
5. The chemical fiber material according to claim 4, wherein the aromatic polyester is a polyalkylene terephthalate.
6. The chemical fiber material of claim 5, wherein the polyalkylene terephthalate is polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate and /or polyethylene terephthalate.
7. The chemical fiber material of claim 2, wherein the at least one polyester is polytrimethylene terephthalate, the at least one other polyester is polybutylene terephthalate, and the polyterephthalate Trimethylene terephthalate and the polybutylene terephthalate are physically mixed in a ratio of 40/60 to 60/40.
8. A yarn comprising the chemical fiber material of claim 1.
9. A yarn according to claim 8, which is a monocomponent filament of uniform composition.
10. A yarn according to claim 8, which is a bicomponent composite filament.
11. A yarn according to claim 8, wherein the chemical fiber material is short fiber.
12. A yarn according to claim 11, which is a blended yarn, which further comprises other fiber materials.
13. A yarn according to claim 12, wherein the other fiber materials are wool fibers, nylon fibers, cotton fibers, acrylic fibers and/or viscose fibers.
14. A fabric and/or other article comprising the chemical fiber material of claim 1.
15. A preparation method of a textile material, which uses at least one polyester and at least another polyester as raw materials, physically mixes different polyesters, and uses the resulting mixed material to make a textile material.
16. The preparation method of claim 15, further comprising heating and extruding the mixed material obtained by the physical mixing to obtain a melt of the mixed material, and making the melt into the chemical fiber material.
17. The preparation method of claim 16, further comprising passing the melt through a spinning pack to form the chemical fiber material.
18. 18. The method of preparation of claim 17, wherein the different polyesters are not subjected to additional melt blending prior to passing the melt through the spin pack.
19. A textile material prepared by the method of claim 18.
20. A fabric and/or other article comprising the textile material of claim 19.
21. A method for dyeing textile materials, the method comprising adding at least one polyester as a raw material by physical mixing in at least one polyester, the at least one polyester and the at least one other polyester being Physical mixing to obtain a mixed material, the melt of the mixed material is made into a textile material, and then the textile material is dyed under normal pressure and/or at a temperature below 130°C.
22. The method for dyeing textile materials according to claim 21, wherein the dyeing treatment is carried out at 100°C.
23. The method for dyeing textile materials according to claim 22, wherein the dyeing treatment is carried out at 90°C.

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