A highly hygroscopic composite color-spun yarn and its preparation method

By introducing hydrophilic groups and quaternary ammonium salt structure into the molecular chain of the polyester fiber yarn, combined with the synergistic effect of chitosan, the problem of insufficient hygroscopicity and antibacterial properties of the polyester fiber yarn is solved, and the improvement of high hygroscopicity and excellent antibacterial properties is achieved.

CN118600754BActive Publication Date: 2025-06-27SHIJIAZHUANG PAIGAO TRADING CO LTD
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Patent Information

Application Number
CN202410807009.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-06-21
Publication Date
2025-06-27
Estimated Expiration
2044-06-21

AI Technical Summary

Technical Problem

Polyester fiber yarn has poor hygroscopicity and antibacterial properties, which limits its application in clothing and textiles and other fields.

Method used

By introducing hydrophilic amide bonds, hydroxyl groups and chitosan into the molecular chains of polyester fibers, and using the quaternary ammonium structure to work synergistically with chitosan, the hygroscopicity and antibacterial properties of the fibers are improved.

Benefits of technology

The hygroscopicity and antibacterial properties of polyester fiber yarn are significantly improved, making it more suitable for the production of textile products such as clothing fabrics.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to the technical field of textiles, and discloses a highly hygroscopic composite colored spun yarn and a preparation method thereof. The composite colored spun yarn prepared by the present invention uses polyester fiber as the fiber base, and performs modification treatment on it, improving the hygroscopicity and antibacterial property of the spun yarn; during the synthesis process of the polyester fiber, a modified polyamide salt is introduced as a functional monomer into the molecular chain of the polyester fiber, increasing the content of hydrophilic groups and quaternary ammonium salt structures in the molecular chain, and improving the hygroscopicity and antibacterial property of the fiber; then, through a photo-grafting reaction, the modified chitosan is grafted on the fiber surface, further improving the hygroscopicity and antibacterial property of the fiber. Based on the composite colored spun yarn prepared by the present invention, it can be widely applied to the production of textile products such as clothing fabrics.
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Description

Technical Field

[0001] The present invention relates to the field of textiles, and particularly to a highly hygroscopic composite colored spun yarn and a preparation method thereof. Background Art

[0002] Polyester fiber is one of the three major synthetic fibers in the world. Compared with the other two major synthetic fibers, polyamide fiber and polyacrylonitrile fiber, polyester fiber was industrialized the latest but has the fastest development speed. The polyester fiber we usually refer to mainly refers to polyethylene terephthalate (PET) fiber, which has the highest output and the widest application. With the continuous iteration and update of textile science and technology, and the gradual improvement of people's requirements for life, textile clothing with single performance can no longer meet people's needs, and clothing with special properties has become a popular product among the public, such as moisture absorption and sweat discharge, comfort, antibacterial property, and flame retardancy.

[0003] The yarn formed by spinning polyester fiber has characteristics such as light weight, wear resistance, and softness. However, due to the dense molecular structure of the fiber itself in the polyester fiber yarn and the absence of hydrophilic groups, the moisture absorption of the fiber is poor, and it does not have antibacterial properties, which limits the application of polyester fiber yarn in the fields of clothing textiles, etc. Therefore, it is necessary to improve the moisture absorption and antibacterial properties of polyester fiber by physical, chemical and other methods. The polyester fiber yarn prepared in this application uses a chemical method to introduce hydrophilic amide bonds, hydroxyl groups, and chitosan into the molecular chain of polyester fiber, thereby improving the moisture absorption of the polyester fiber yarn; a quaternary ammonium salt structure is also introduced, and its synergistic effect with chitosan is used to improve the antibacterial property of the polyester fiber yarn. Summary of the Invention

[0004] In order to solve the above technical problems, the present invention provides a highly hygroscopic composite colored spun yarn and a preparation method thereof.

[0005] The object of the present invention can be achieved by the following technical solutions:

[0006] A highly hygroscopic composite colored spun yarn is prepared by mixing and spinning functionalized polyester fibers dyed with two different colors of disperse dyes.

[0007] The functionalized polyester fiber is prepared by the following steps:

[0008] Step A1: Add 5-aminoisophthalic acid and dimethylacetamide into a flask, heat to 40 - 50 °C and stir to mix evenly, then cool down to 0 °C, add triethylamine and stir to mix evenly, add 4-dimethylaminobenzoyl chloride slowly into the flask in three portions, stir at low temperature for 1 - 2 h, then transfer the flask to an oil bath, slowly raise the system temperature to 60 - 70 °C, and continue to react for 5.5 - 6.5 h. After the reaction is completed, pour the mixed solution into deionized water at 10 °C, stir for 3 - 5 min, then filter, wash, dry, and recrystallize to obtain Intermediate Product 1;

[0009] Further, in Step A1, the dosage ratio of 5-aminoisophthalic acid, dimethylacetamide, triethylamine, 4-dimethylaminobenzoyl chloride, and deionized water is 0.1 - 0.3 mol : 100 mL : 2 - 7 mL : 0.1 - 0.3 mol : 200 mL;

[0010] Step A2: Add Intermediate Product 1 into a reactor, stir at a constant temperature of 45 °C, and add n-octyl chloride drop by drop using a constant-pressure separating funnel. After the addition is completed, react for 12 h, then let the mixture stand in the separating funnel for 12 h, separate the lower layer liquid, rotary evaporate and freeze-dry for 8 h to obtain the carboxyl-terminal product;

[0011] Further, in Step A2, the molar ratio of Intermediate Product 1 to n-octyl chloride is 1 : 1;

[0012] Step A3: Add 30 wt% pentamethylenediamine solution into a reactor, under nitrogen condition, raise the temperature to 40 - 50 °C, and slowly add adipic acid and the carboxyl-terminal product under stirring condition, continue to react for 2 - 4 h, and control the system pH to 7.2 - 7.6. After the reaction is completed, filter with activated carbon to obtain the modified polyamide salt;

[0013] Further, in Step A3, the molar ratio of pentamethylenediamine, adipic acid, and the carboxyl-terminal product in the 30 wt% pentamethylenediamine solution is 1 : 0.6 - 0.8 : 0.2 - 0.4, and the 30 wt% pentamethylenediamine solution is diluted from 99.5% pentamethylenediamine with demineralized water;

[0014] Step A4: Add terephthalic acid and ethylene glycol into a reactor, add antimony glycolate and triphenyl phosphite and stir evenly. Under nitrogen and stirring conditions, raise the temperature to 220 - 230 °C, continue to react for 2 - 3 h, then add the modified polyamide salt, continue to raise the temperature to 245 - 255 °C, react under vacuum condition for 30 - 50 min, and finally raise the temperature to 260 - 270 °C, continue to react for 2 - 4 h. After the reaction is completed, collect the product, cool down, pelletize, dry, and melt-spin to obtain the modified polyester fiber;

[0015] Further, in step A4, the dosage ratio of terephthalic acid, ethylene glycol, antimony glycolate, triphenyl phosphite and modified polyamide salt is 0.13 - 0.33 mol : 0.17 - 0.51 mol : 0.04 - 0.06 mol : 0.001 - 0.002 mol : 0.004 - 0.016 mol;

[0016] Step A5: Add modified chitosan and benzophenone into a beaker containing ethanol, mix and stir evenly, then adjust the pH to 7 - 8 to obtain an antibacterial solution. Then soak 5 - 10 g of modified polyester fiber in 100 g of the antibacterial solution for 30 min, and then place the soaked polyester fiber under ultraviolet light for irradiation for 4 - 7 min, and then wash with water and dry to obtain functionalized polyester fiber;

[0017] Further, in the antibacterial solution of step A5, the dosage ratio of modified chitosan, benzophenone and ethanol is 2 - 8 g : 2 - 4 g : 100 g.

[0018] The modified chitosan is prepared by the following steps:

[0019] Disperse chitosan in a 2 - 3 wt% sodium hydroxide solution, mix and stir evenly, then refrigerate at -10 °C for 24 h. After thawing, centrifuge and collect the product, and dry the product at 60 °C. Then add the dried chitosan, 1,2 - epoxy - 9 - decene and ethanol into a flask, mix and stir evenly, and heat to 55 - 65 °C, stir and react for 5 - 7 h. After the reaction is completed, centrifuge, wash, and dry at 60 °C for 12 h to obtain modified chitosan;

[0020] Further, the mass ratio of the dried chitosan, 1,2 - epoxy - 9 - decene and ethanol is 1 - 2 : 0.5 - 1 : 35 - 50, and the dosage ratio of chitosan and sodium hydroxide solution is 1 - 3 g : 10 mL.

[0021] In the modified chitosan, chitosan is first treated with a sodium hydroxide solution for alkali treatment to expose more hydroxyl groups, and then the hydroxyl groups react with the epoxy groups in 1,2 - epoxy - 9 - decene, thereby introducing double bonds into chitosan to obtain modified chitosan.

[0022] A preparation method of a highly hygroscopic composite color - spun yarn includes the following steps:

[0023] Step S1: Immerse the functionalized polyester fiber in two different - colored disperse dye solutions respectively, heat up to 80 - 100 °C at a rate of 1 °C / min, keep warm for 50 - 80 min, then rinse with cold water and dry for standby;

[0024] Step S2: Mix and spin the two different - colored functionalized polyester fibers obtained in step S1 in a mass ratio of 1:1 to obtain the composite color - spun yarn.

[0025] Advantages of the present invention:

[0026] The composite color spinning yarn prepared by the present invention uses polyester fiber as the fiber base and modifies it to improve the hygroscopicity and antibacterial properties of the spinning yarn. During the synthesis of polyester fiber, a modified polyamide salt is introduced into the molecular chain of polyester fiber as a functional monomer, increasing the content of hydrophilic groups and quaternary ammonium salt structures in the molecular chain, and improving the hygroscopicity and antibacterial properties of the fiber. Then, through a photo-grafting reaction, the modified chitosan is grafted onto the fiber surface, further improving the hygroscopicity and antibacterial properties of the fiber. The composite color spinning yarn prepared based on the present invention can be widely used in the production of textile products such as clothing fabrics.

[0027] In the functionalized polyester fiber, the amino group in 5-aminoisophthalic acid reacts with the acyl chloride group in 4-dimethylaminobenzoyl chloride to form an intermediate product 1 containing a tertiary amine structure. The nucleophilic substitution reaction between the tertiary amine in the intermediate product 1 and the chlorine atom in n-octyl chloride is used to generate an end-carboxyl product containing a quaternary ammonium salt structure. Then, the end-carboxyl product and adipic acid are used as the dibasic acids for synthesizing polyamide at the same time, and they react with pentamethylenediamine to form a modified polyamide salt. The modified polyamide salt is used as a modifier in the synthesis of polyester fiber to generate a modified polyester fiber containing an amide structure. Finally, by means of photo-grafting, the modified chitosan is grafted into the modified polyester fiber to obtain the functionalized polyester fiber. The functionalized polyester fiber is dyed and then spun to obtain a composite color spinning yarn with excellent antibacterial properties and high hygroscopicity. This is because the functionalized polyester fiber introduces an amide bond, a hydrophilic group, into the main chain structure, which can promote the diffusion of water molecules into the fiber interior. The combination of chemical bonds and hydrophilic groups improves the moisture absorption capacity of the fiber. At the same time, the introduction of the modified polyamide salt weakens the crystallization ability of the polyester fiber, making it easier for water molecules to diffuse into the fiber macromolecules, further improving the hygroscopicity of the polyester fiber. Grafting the modified chitosan onto the modified polyester fiber further improves the moisture absorption performance of the polyester fiber. This is because chitosan itself contains a large number of strongly polar groups (such as hydroxyl groups, amino groups, etc.), and these groups have high hygroscopicity, which can effectively improve the hygroscopicity of the polyester fiber. The ring-opening reaction between the hydroxyl group in chitosan and the epoxy group in 1,2-epoxy-9-decene not only generates a hydrophilic ether bond but also generates a hydroxyl group, further improving the hygroscopicity of the polyester fiber. A quaternary ammonium salt structure with antibacterial ability and chitosan are also introduced into the functionalized polyester fiber, and they work synergistically to improve the antibacterial properties of the fiber, thereby making the spinning yarn have certain antibacterial properties. In addition, the amide groups introduced into the functionalized polyester fiber also disrupt the regularity of the main chain of the polyester fiber molecule, reducing the crystallinity of the polyester fiber. As a result, the dye molecules of disperse dyes are more likely to diffuse into the fiber interior, improving the color fastness of the polyester fiber. Specific embodiments

[0028] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0029] Example 1

[0030] The modified chitosan is prepared by the following steps:

[0031] Disperse 1 g of chitosan in 10 mL of 2 wt% sodium hydroxide solution, stir and mix evenly, then refrigerate at -10°C for 24 h. After thawing, centrifuge, collect the product, and dry the product at 60°C. Then add 1 g of the dried chitosan, 0.5 g of 1,2-epoxy-9-decene, and 35 g of ethanol into a flask, mix and stir evenly, heat to 55°C, stir and react for 5 h. After the reaction is completed, centrifuge, wash, and dry at 60°C for 12 h to obtain the modified chitosan.

[0032] The functionalized polyester fiber is prepared by the following steps:

[0033] Step A1: Add 0.1 mol of 5-aminophthalic acid and 100 mL of dimethylacetamide into a flask, heat to 40°C and stir to mix evenly. Then cool to 0°C, add 2 mL of triethylamine and stir to mix evenly. Slowly add 0.1 mol of 4-dimethylaminobenzoyl chloride into the flask in three portions, and stir at low temperature for 1 h. Then transfer the flask to an oil bath, slowly raise the system temperature to 60°C, and continue to react for 5.5 h. After the reaction is completed, pour the mixed solution into 200 mL of deionized water at 10°C, stir for 3 min, then filter, wash, dry, and recrystallize to obtain Intermediate Product 1;

[0034] Step A2: Add 0.1 mol of Intermediate Product 1 into a reactor, stir at a constant temperature of 45°C, and gradually add 0.1 mol of n-octyl chloride dropwise using a constant pressure dropping funnel. After the dropping is completed, react for 12 h. Then let the mixture stand in a separating funnel for 12 h, separate the lower layer liquid, rotary evaporate, and freeze-dry for 8 h to obtain the carboxyl-terminated product;

[0035] Step A3: Add 30 wt% pentamethylenediamine solution into the reactor. Under nitrogen condition, heat up to 40 °C, and slowly add adipic acid and the carboxyl-terminated product under stirring condition. Continue the reaction for 2 h, and control the pH of the system to 7.2. After the reaction is completed, filter with activated carbon to obtain the modified polyamide salt. The molar ratio of pentamethylenediamine, adipic acid and the carboxyl-terminated product in the 30 wt% pentamethylenediamine solution is 1:0.8:0.2. The 30 wt% pentamethylenediamine solution is diluted with demineralized water from 99.5% pentamethylenediamine;

[0036] Step A4: Add 0.13 mol of terephthalic acid and 0.17 mol of ethylene glycol into the reactor, then add 0.04 mol of antimony glycolate and 0.001 mol of triphenyl phosphite and stir evenly. Under nitrogen and stirring conditions, raise the temperature to 220 °C and continue the reaction for 2 h. Then add 0.004 mol of the modified polyamide salt, continue to raise the temperature to 245 °C, and react for 30 min under vacuum condition. Finally, raise the temperature to 260 °C and continue the reaction for 2 h. After the reaction is completed, collect the product, cool down, pelletize, dry, and melt-spin to obtain the modified polyester fiber;

[0037] Step A5: Add 2 g of modified chitosan and 2 g of benzophenone into a beaker containing 100 g of ethanol and mix and stir evenly. Then adjust the pH to 7 to obtain the antibacterial solution. Then soak 5 g of the modified polyester fiber in 100 g of the antibacterial solution for 30 min. Subsequently, place the soaked polyester fiber under ultraviolet light for irradiation for 4 min, then wash with water and dry to obtain the functionalized polyester fiber.

[0038] Example 2

[0039] The modified chitosan is prepared by the following steps:

[0040] Disperse 2 g of chitosan in 10 mL of 2.5 wt% sodium hydroxide solution and mix and stir evenly. Then refrigerate at -10 °C for 24 h. After thawing, centrifuge and collect the product, and dry the product at 60 °C. Then add 1.5 g of the dried chitosan, 0.75 g of 1,2-epoxy-9-decene and 42 g of ethanol into the flask, mix and stir evenly, and heat to 60 °C and stir and react for 6 h. After the reaction is completed, centrifuge, wash, and dry at 60 °C for 12 h to obtain the modified chitosan.

[0041] The functionalized polyester fiber is prepared by the following steps:

[0042] Step A1: Add 0.2 mol of 5-aminoisophthalic acid and 100 mL of dimethylacetamide into a flask, heat to 45 °C and stir to mix evenly, then cool down to 0 °C, add 5 mL of triethylamine and stir to mix evenly. Then, slowly add 0.2 mol of 4-dimethylaminobenzoyl chloride into the flask in three portions, and stir at low temperature for 1.5 h. Then, transfer the flask to an oil bath, slowly raise the system temperature to 65 °C, and continue the reaction for 6 h. After the reaction is completed, pour the mixed solution into 200 mL of deionized water at 10 °C, stir for 4 min, then filter, wash, dry, and recrystallize to obtain Intermediate Product 1;

[0043] Step A2: Add 0.1 mol of Intermediate Product 1 into a reactor, stir at a constant temperature of 45 °C, and gradually add 0.1 mol of n-octyl chloride dropwise using a constant-pressure dropping funnel. After the addition is completed, react for 12 h, then let the mixture stand in a separating funnel for 12 h, separate the lower layer liquid, rotary evaporate and freeze-dry for 8 h to obtain the carboxyl-terminal product;

[0044] Step A3: Add 30 wt% pentamethylenediamine solution into a reactor, under nitrogen conditions, raise the temperature to 45 °C, and slowly add adipic acid and the carboxyl-terminal product under stirring conditions, continue the reaction for 3 h, and control the system pH to 7.4. After the reaction is completed, filter with activated carbon to obtain the modified polyamide salt. The molar ratio of pentamethylenediamine, adipic acid, and the carboxyl-terminal product in the 30 wt% pentamethylenediamine solution is 1:0.7:0.3, and the 30 wt% pentamethylenediamine solution is diluted with demineralized water from 99.5% pentamethylenediamine;

[0045] Step A4: Add 0.23 mol of terephthalic acid and 0.34 mol of ethylene glycol into a reactor, add 0.05 mol of antimony glycolate and 0.0015 mol of triphenyl phosphite, stir evenly. Under nitrogen and stirring conditions, raise the temperature to 225 °C, continue the reaction for 2.5 h, then add 0.01 mol of the modified polyamide salt, continue to raise the temperature to 250 °C, react under vacuum conditions for 40 min, and finally raise the temperature to 265 °C, continue the reaction for 3 h. After the reaction is completed, collect the product, cool down, pelletize, dry, and melt-spin to obtain the modified polyester fiber;

[0046] Step A5: Add 5 g of modified chitosan and 3 g of benzophenone into a beaker containing 100 g of ethanol, mix and stir evenly, then adjust the pH to 7.5 to obtain an antibacterial solution. Then, soak 7.5 g of the modified polyester fiber in 100 g of the antibacterial solution for 30 min, then place the soaked polyester fiber under ultraviolet light for irradiation for 5 min, and then wash with water and dry to obtain the functionalized polyester fiber.

[0047] Example 3

[0048] The modified chitosan is prepared by the following steps:

[0049] Disperse 3 g of chitosan in 10 mL of 3 wt% sodium hydroxide solution, stir and mix evenly, then refrigerate at -10 °C for 24 h. After thawing, centrifuge, collect the product, and dry the product at 60 °C. Then add 2 g of the dried chitosan, 1 g of 1,2-epoxy-9-decene, and 50 g of ethanol into a flask, mix and stir evenly, heat to 65 °C, and stir and react for 7 h. After the reaction is completed, centrifuge, wash, and dry at 60 °C for 12 h to obtain the modified chitosan.

[0050] The functionalized polyester fiber is prepared by the following steps:

[0051] Step A1: Add 0.3 mol of 5-aminophthalic acid and 100 mL of dimethylacetamide into a flask, heat to 50 °C, stir and mix evenly, then cool down to 0 °C, add 7 mL of triethylamine and stir and mix evenly, and slowly add 0.3 mol of 4-dimethylaminobenzoyl chloride into the flask in three portions, stir at low temperature for 2 h, then transfer the flask to an oil bath, slowly raise the system temperature to 70 °C, and continue to react for 6.5 h. After the reaction is completed, pour the mixed solution into 200 mL of deionized water at 10 °C, stir for 5 min, then filter, wash, dry, and recrystallize to obtain Intermediate Product 1;

[0052] Step A2: Add 0.1 mol of Intermediate Product 1 into a reactor, stir at a constant temperature of 45 °C, and gradually add 0.1 mol of n-octyl chloride dropwise using a constant pressure separating funnel. After the addition is completed, react for 12 h, then let the mixture stand in the separating funnel for 12 h, separate the lower layer liquid, rotary evaporate, and freeze-dry for 8 h to obtain the carboxyl-terminated product;

[0053] Step A3: Add 30 wt% pentanediamine solution into a reactor, under nitrogen conditions, raise the temperature to 50 °C, and slowly add adipic acid and the carboxyl-terminated product under stirring conditions, continue to react for 4 h, and control the system pH to 7.6. After the reaction is completed, filter with activated carbon to obtain the modified polyamide salt. The molar ratio of pentanediamine, adipic acid, and the carboxyl-terminated product in the 30 wt% pentanediamine solution is 1:0.6:0.4, and the 30 wt% pentanediamine solution is diluted with demineralized water from 99.5% pentanediamine;

[0054] Step A4: Add 0.33 mol of terephthalic acid and 0.51 mol of ethylene glycol into the reactor, then add 0.06 mol of antimony glycolate and 0.002 mol of triphenyl phosphite, stir evenly. Under the conditions of nitrogen and stirring, raise the temperature to 230 °C, continuously react for 3 h, then add 0.016 mol of modified polyamide salt, continue to raise the temperature to 255 °C, react under vacuum conditions for 50 min, and finally raise the temperature to 270 °C, continuously react for 4 h. After the reaction is completed, collect the product, cool down, pelletize, dry, and perform melt spinning to obtain the modified polyester fiber;

[0055] Step A5: Add 8 g of modified chitosan and 4 g of benzophenone into a beaker containing 100 g of ethanol, mix and stir evenly, then adjust the pH to 8 to obtain the antibacterial solution. Then soak 10 g of the modified polyester fiber in 100 g of the antibacterial solution for 30 min, and then place the soaked polyester fiber under ultraviolet light for irradiation for 7 min, and then wash with water and dry to obtain the functionalized polyester fiber.

[0056] Example 4

[0057] A preparation method of a highly hygroscopic composite color spinning yarn includes the following steps:

[0058] Step S1: Immerse the functionalized polyester fiber prepared in Example 1 in the disperse dye solutions of disperse orange and disperse yellow respectively, raise the temperature to 80 °C at a rate of 1 °C / min, keep warm for 50 min, then rinse with cold water and dry for standby;

[0059] Step S2: Mix and spin the orange and yellow functionalized polyester fibers obtained in Step S1 at a mass ratio of 1:1 to obtain the composite color spinning yarn.

[0060] Example 5

[0061] A preparation method of a highly hygroscopic composite color spinning yarn includes the following steps:

[0062] Step S1: Immerse the functionalized polyester fiber prepared in Example 2 in the disperse dye solutions of disperse orange and disperse yellow respectively, raise the temperature to 90 °C at a rate of 1 °C / min, keep warm for 70 min, then rinse with cold water and dry for standby;

[0063] Step S2: Mix and spin the orange and yellow functionalized polyester fibers obtained in Step S1 at a mass ratio of 1:1 to obtain the composite color spinning yarn.

[0064] Example 6

[0065] A preparation method of a highly hygroscopic composite color spinning yarn includes the following steps:

[0066] Step S1: Immerse the functionalized polyester fibers prepared in Example 3 in the disperse dye baths of disperse orange and disperse yellow respectively, heat up to 100 °C at a rate of 1 °C / min, keep warm for 80 min, then rinse with cold water and dry for standby;

[0067] Step S2: Mix and spin the orange and yellow functionalized polyester fibers obtained in Step S1 in a mass ratio of 1:1 to obtain the composite color spun yarn.

[0068] Comparative Example 1

[0069] This comparative example is a kind of composite color spun yarn. The difference from Example 6 is that the polyester fibers prepared by the following steps are used to replace the functionalized polyester fibers prepared in Example 3, and the rest are the same;

[0070] Add 8 g of the modified chitosan prepared in Example 3 and 4 g of benzophenone into a beaker containing 100 g of ethanol, mix and stir evenly, then adjust the pH to 8 to obtain the antibacterial solution. Then soak 10 g of polyester fibers in 100 g of the antibacterial solution for 30 min, and then place the soaked polyester fibers under ultraviolet light for irradiation for 7 min, and then wash with water and dry to obtain the polyester fibers.

[0071] Comparative Example 2

[0072] This comparative example is a kind of composite color spun yarn. The difference from Example 6 is that the modified polyester fibers prepared in Example 3 are used to replace the functionalized polyester fibers prepared in Example 3, and the rest are the same.

[0073] Perform performance tests on the composite color spun yarns prepared in Examples 4 - 6 and Comparative Examples 1 - 2:

[0074] Antibacterial performance test: Weave the composite color spun yarns prepared in Examples 4 - 6 and Comparative Examples 1 - 2 into fabrics, and use the method disclosed in the industry standard FZ / T 73023 - 2006 to conduct antibacterial tests after washing 100 times;

[0075] Moisture regain test: Conduct moisture regain tests according to GB / T6503 - 2017 "Test Method for Moisture Regain of Chemical Fibers". Test conditions: After placing in a constant temperature and humidity (25 °C, 60% RH) environment for 48 h, weigh a certain mass of fibers and place them in an oven for weighing and record as G (g). After drying for 1 h, weigh once every 10 min until the mass remains constant and record as G0 (g). The calculation formula for moisture regain W is as follows: W = (G - G0) / G0 × 100%;

[0076] Color fastness test: Refer to GB / T 3920—2008 "Textiles - Tests for color fastness - Color fastness to rubbing" for testing;

[0077] The test results are shown in the following table:

[0078]

[0079] As can be seen from the above table, after the antibacterial test of the color-spun yarn prepared by the present invention, the antibacterial rate against Escherichia coli is 97.6%-98.6%, and the antibacterial rate against Staphylococcus aureus is 96.1%-97.2%, indicating that the color-spun yarn has excellent antibacterial properties; after the moisture regain test, the moisture regain is 167%-192%, indicating that the color-spun yarn has high hygroscopicity; it also has excellent color fastness.

[0080] The above content is only an example and illustration of the concept of the present invention. Those skilled in the art of this technology can make various modifications or supplements or use similar methods to replace the specific embodiments described, as long as they do not deviate from the scope defined by the concept of the invention, they shall fall within the protection scope of the present invention.

Claims

1. A highly hygroscopic composite colored spun yarn, characterized in that: It is made by dyeing functional polyester fibers with two different colors of disperse dyes and then mixing and spinning them; The functionalized polyester fiber is prepared by the following steps: Step A1, add 5-aminoisophthalic acid and dimethylacetamide to a flask, heat to 40-50°C and stir to mix evenly, then cool to 0°C, add triethylamine and stir to mix evenly, then slowly add 4-dimethylaminobenzoyl chloride to the flask three times, and stir at low temperature for 1-2h, then transfer the flask to an oil bath, slowly increase the system temperature to 60-70°C, and continue the reaction for 5.5-6.5h. After the reaction is completed, pour the mixed solution into 10°C deionized water and stir for 3-5min, then filter, wash, dry and recrystallize to obtain intermediate 1; Step A2, adding the intermediate product 1 to a reactor, stirring at a constant temperature of 45° C., and adding n-octyl chloride dropwise using a constant pressure separatory funnel. After the addition is completed, react for 12 hours, and then let the mixture stand in the separatory funnel for 12 hours, separate the lower layer of liquid, and rotary evaporate and freeze-dry for 8 hours to obtain a carboxyl-terminated product; Step A3, adding 30wt% pentamethylenediamine solution into the reactor, raising the temperature to 40-50°C under nitrogen, and slowly adding adipic acid and the carboxyl-terminated product under stirring, continuing the reaction for 2-4h, and controlling the pH of the system to 7.2-7.

6. After the reaction is completed, filtering with activated carbon to obtain a modified polyamide salt; Step A4, adding terephthalic acid and ethylene glycol to a reactor, then adding ethylene glycol antimony and triphenyl phosphite and stirring evenly, raising the temperature to 220-230° C. under nitrogen and stirring conditions, continuing the reaction for 2-3 hours, then adding modified polyamide salt, continuing to raise the temperature to 245-255° C., reacting under vacuum conditions for 30-50 minutes, and finally raising the temperature to 260-270° C., continuing the reaction for 2-4 hours, after the reaction is completed, collecting the product, cooling, pelletizing, drying, and melt spinning to obtain modified polyester fiber; Step A5, adding modified chitosan and benzophenone into a beaker containing ethanol, mixing and stirring evenly, then adjusting the pH to 7-8 to obtain an antibacterial solution, and then soaking 5-10 g of modified polyester fiber in 100 g of the antibacterial solution for 30 min, then irradiating the soaked polyester fiber under ultraviolet light for 4-7 min, and then washing and drying to obtain functionalized polyester fiber; The modified chitosan is prepared by the following steps: Disperse chitosan in 2-3wt% sodium hydroxide solution, stir and mix evenly, then refrigerate at -10°C for 24h, centrifuge after thawing, collect the product, and dry the product at 60°C, then add the dried chitosan, 1,2-epoxy-9-decene and ethanol into a flask, mix and stir evenly, heat to 55-65°C, stir and react for 5-7h, after the reaction is completed, centrifuge, wash, and dry at 60°C for 12h to obtain modified chitosan.

2. A highly hygroscopic composite colored spun yarn according to claim 1, characterized in that: In step A1, the usage ratio of 5-aminoisophthalic acid, dimethylacetamide, triethylamine, 4-dimethylaminobenzoyl chloride and deionized water is 0.1-0.3 mol: 100 mL: 2-7 mL: 0.1-0.3 mol: 200 mL.

3. A highly hygroscopic composite colored spun yarn according to claim 1, characterized in that: The molar ratio of the intermediate product 1 and n-octyl chloride in step A2 is 1:

1.

4. A highly hygroscopic composite colored spun yarn according to claim 1, characterized in that: The molar ratio of pentamethylenediamine, adipic acid and the carboxyl-terminated product in the 30 wt % pentamethylenediamine solution in step A3 is 1:0.6-0.8:0.2-0.

4. The 30 wt % pentamethylenediamine solution is prepared by diluting 99.5 wt % pentamethylenediamine with desalted water.

5. A highly hygroscopic composite colored spun yarn according to claim 1, characterized in that: In step A4, the usage ratio of terephthalic acid, ethylene glycol, ethylene glycol antimony, triphenyl phosphite and modified polyamide salt is 0.13-0.33 mol: 0.17-0.51 mol: 0.04-0.06 mol: 0.001-0.002 mol: 0.004-0.016 mol.

6. A highly hygroscopic composite colored spun yarn according to claim 1, characterized in that: The dosage ratio of modified chitosan, benzophenone and ethanol in the antibacterial solution of step A5 is 2-8g:2-4g:100g.

7. A highly hygroscopic composite colored spun yarn according to claim 1, characterized in that: The mass ratio of the dried chitosan, 1,2-epoxy-9-decene and ethanol is 1-2:0.5-1:35-50, and the dosage ratio of the chitosan and the sodium hydroxide solution is 1-3g:10mL.

8. The method for preparing a highly hygroscopic composite colored spun yarn according to claim 1, characterized in that: The following steps are involved: Step S1, immersing the functionalized polyester fiber in two disperse dye solutions of different colors respectively, heating the temperature to 80-100° C. at a rate of 1° C. / min, keeping the temperature for 50-80 min, rinsing with cold water and drying for later use; Step S2, mixing and spinning the two functionalized polyester fibers of different colors obtained in step S1 at a mass ratio of 1:1 to obtain composite color yarn.

Citation Information

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