Anti-pilling yarn for wear-resistant fabric and preparation method of anti-pilling yarn
By combining piperazine-modified polylactic acid finishing agent and divinylbenzene-modified acrylic fiber, the problem of yarn damage during friction is solved, and anti-pilling yarn with excellent abrasion resistance and comfort is produced.
Patent Information
- Application Number
- CN202511197388.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-26
- Publication Date
- 2025-11-14
AI Technical Summary
Existing yarns are prone to damage under stress and friction, resulting in pilling and fuzzing, which affects the abrasion resistance and comfort of the fabric.
By combining piperazine-modified polylactic acid finishing agent emulsion with divinylbenzene-modified acrylic fibers, a continuous polymer film is formed on the fiber surface, which enhances the rigidity of the fiber structure and reduces friction and tangling, thus preparing anti-pilling yarn for abrasion-resistant fabrics.
It significantly improves the anti-pilling and anti-fuzzing properties of yarn, extends the service life of fabric, and enhances abrasion resistance and comfort.
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Figure BDA0005565455570000141
Abstract
Description
Technical Field
[0001] This invention relates to the field of yarn, specifically to an anti-pilling yarn for abrasion-resistant fabrics and its preparation method. Background Technology
[0002] During daily wear and use, clothing fabrics are prone to pilling, especially in areas of frequent friction, such as collars, cuffs, and trouser hems. This not only affects the appearance of the clothing but may also reduce the lifespan and comfort of the fabric. Pilling resistance is particularly important for fabrics requiring high abrasion resistance, such as sportswear and casual wear. This invention provides an anti-pilling yarn for abrasion-resistant fabrics. This yarn can significantly improve the abrasion resistance and anti-pilling properties of the fabric while maintaining good softness and comfort. Summary of the Invention
[0003] In order to overcome the above-mentioned technical problems, the present invention aims to provide an anti-pilling yarn for abrasion-resistant fabrics and its preparation method, which solves the problem that existing yarns are easily damaged and pill when subjected to force and friction.
[0004] The objective of this invention can be achieved through the following technical solutions:
[0005] In a first aspect, this application provides an anti-pilling yarn for abrasion-resistant fabrics, comprising the following parts by weight:
[0006] 10-20 parts of piperazine-modified polylactic acid finishing agent emulsion, 50-70 parts of divinylbenzene-modified acrylic fiber, and 30-50 parts of polyester fiber.
[0007] The piperazine-modified polylactic acid finishing agent emulsion is prepared by the following steps:
[0008] Step A1: Add tetramethylcyclotetrasiloxane and 3-piperazinylpropylmethyldimethoxysilane to a four-necked flask equipped with a reflux condenser, thermometer, and stirrer. Stir at a rate of 50-100 r / min. Dissolve potassium hydroxide in deionized water and add it to the flask. Heat to 125-130℃ and maintain the temperature for 3-4 h. Add hexamethyldisiloxane and maintain the temperature for 1-2 h to obtain piperazine-based polysiloxane.
[0009] Step A2: Add lactic acid, diphenyl ether, and stannous chloride to a three-necked flask equipped with a stirrer and thermometer. Use a circulating water vacuum pump to evacuate and maintain a vacuum of 40 Pa. Increase the temperature to 110-120℃ at 300-500 r / min and react for 2-3 h. Increase the temperature to 130-140℃ and react for 3-7 h. Increase the temperature to 150-160℃ and react at 20 Pa for 6-8 h. Remove the diphenyl ether by rotary evaporation, precipitate with ethanol, and filter to obtain polylactic acid prepolymer.
[0010] Step A3: Add polylactic acid prepolymer and acetone to a three-necked flask equipped with a stirrer and thermometer, purge with nitrogen for protection, stir at 50-60 r / min for 10-20 min, heat to 25-50℃, dissolve piperazine-based polysiloxane in tetrahydrofuran and add dropwise to the flask, add dicumyl peroxide, react at 110-120℃ and 2-4 kPa for 2-4 h, cool to 70-85℃, add glacial acetic acid to adjust pH to 6-7, add sodium dodecylbenzenesulfonate and deionized water, emulsify at 1000-1500 r / min for 1 h, remove acetone by vacuum distillation, and obtain piperazine-modified polylactic acid finishing agent emulsion.
[0011] As a further embodiment of the present invention: the ratio of the amounts of octamethylcyclotetrasiloxane, 3-piperazinylpropylmethyldimethoxysilane, potassium hydroxide, deionized water and hexamethyldisiloxane in step A1 is 156-312mL: 6.34-12.68mL: 0.6-1.2g: 5-10mL: 19.63-39.26mL.
[0012] As a further aspect of the present invention: the ratio of lactic acid, diphenyl ether, and stannous chloride used in step A2 is 80-160mL: 120-240mL: 0.5-1.0g.
[0013] As a further aspect of the present invention: the mass fraction of lactic acid in step A2 is 90%.
[0014] As a further aspect of the present invention: the ratio of polylactic acid prepolymer, acetone, piperazine polysiloxane, tetrahydrofuran, dicumyl peroxide, sodium dodecylbenzenesulfonate, and deionized water in step A3 is 85-170g: 150-300mL: 15-30g: 50-100mL: 2-4g: 2-4g: 10-20mL.
[0015] As a further aspect of the present invention: the divinylbenzene modified acrylic fiber is prepared by the following steps:
[0016] Step B1: Acrylonitrile, methyl acrylate, N,N-dimethylformamide, and polyethylene glycol are added to a four-necked flask equipped with a stirrer, thermometer, reflux condenser, and nitrogen gas delivery tube. Nitrogen gas is introduced for protection, and the mixture is stirred at 200-300 r / min for 20-30 min. The temperature is raised to 50-60℃, divinylbenzene is added, and the mixture is stirred for 10-20 min. Azobisisobutyronitrile is added, and the mixture is heated to 63-67℃ and reacted for 3-4 h. The temperature is lowered to 24-26℃, hydroquinone is added, and the mixture is rotary evaporated. After filtration, the mixture is washed 2-4 times with ethanol and placed in a drying oven to be vacuum dried at 40-50℃ for 22-24 h to obtain divinylbenzene-modified polyacrylonitrile.
[0017] Step B2: Add divinylbenzene-modified polyacrylonitrile and N,N-dimethylformamide to a reactor equipped with a thermometer, let it stand at 40°C for 30 minutes, and then let the solution enter the N,N-dimethylacetamide coagulation bath through the spinneret. The fibers formed by spinning enter the first drawing bath at 60°C, and then enter the second drawing bath at 100°C to obtain divinylbenzene-modified acrylic fibers.
[0018] As a further embodiment of the present invention: the ratio of acrylonitrile, methyl acrylate, N,N-dimethylformamide, polyethylene glycol, divinylbenzene, azobisisobutyronitrile, and hydroquinone used in step B1 is 75-150mL: 9-18mL: 200-400mL: 6-12mL: 15-30mL: 0.9-1.8g: 0.15-0.3g.
[0019] As a further aspect of the present invention: the polyethylene glycol mentioned in step B1 is of type PEG-200.
[0020] As a further aspect of the present invention: the ratio of divinylbenzene-modified polyacrylonitrile and N,N-dimethylformamide used in step B2 is 20-40g:60-120mL.
[0021] As a further aspect of the present invention: the mass fraction of the N,N-dimethylacetamide coagulation bath in step B2 is 50%.
[0022] As a further aspect of the present invention: the spinneret cap in step B2 has a specification of Ф200×0.075mm.
[0023] Secondly, this application provides a method for preparing anti-pilling yarn for abrasion-resistant fabrics, comprising the following steps:
[0024] Step 1: Weigh out 10-20 parts of piperazine-modified polylactic acid finishing agent emulsion, 50-70 parts of divinylbenzene-modified acrylic fiber, and 30-50 parts of polyester fiber according to the weight ratio, and set aside.
[0025] Step 2: Blend divinylbenzene modified acrylic fiber and polyester fiber to obtain blended fiber;
[0026] Step 3: Prepare a finishing solution by mixing piperazine-modified polylactic acid finishing agent emulsion at a concentration of 60 g / L. Immerse the yarn in the finishing solution at a bath ratio of 1:30-50 and perform finishing using a two-dip, two-nip method, controlling the tie weight at 80%. After finishing, pre-dry the yarn at 90℃ for 60 seconds, then bake it at 140-170℃ for 60-180 seconds. After baking, wash the yarn 3-5 times and dry it to make abrasion-resistant, anti-pilling yarn for fabrics.
[0027] The beneficial effects of this invention are:
[0028] This invention discloses an anti-pilling yarn for wear-resistant fabrics and its preparation method. Piperazine groups are introduced into polylactic acid to obtain a finishing agent emulsion, which can form a continuous and dense polymer film on the fiber surface, thereby effectively reducing friction and tangling between fibers and reducing the tendency of pilling. Divinylbenzene is introduced into polyacrylonitrile to enhance the structural rigidity of acrylic fibers, reduce deformation and breakage under stress, thereby improving the anti-pilling performance and extending the service life of the fabric.
[0029] To prepare an anti-pilling yarn for abrasion-resistant fabrics, a piperazine-modified polylactic acid finishing agent emulsion is first prepared. Tetramethylcyclotetrasiloxane undergoes Si-O bond cleavage under potassium hydroxide catalysis to form active chain ends. The piperazine group of 3-piperazinylpropylmethyldimethoxysilane reacts with the active chain ends to introduce a piperazine group. Hexamethyldisiloxane is used as a capping agent to monochromatically terminate chain growth at the active chain ends, yielding piperazine-based polysiloxane. Lactic acid undergoes a dehydration condensation reaction to obtain a polylactic acid prepolymer. The piperazine-based polysiloxane reacts with the polylactic acid prepolymer, and the alkylene oxide in the piperazine group... The amino groups form hydrogen bonds with the ester and hydroxyl groups in the polylactic acid (PLA) prepolymer, and can also react chemically with the carboxyl groups, thereby introducing piperazine groups into the PLA segments. These piperazine segments reduce inter-fiber friction, decrease fiber breakage and separation, and inhibit pilling. The film formed by the PLA prepolymer segments adheres to and encapsulates the fibers, preventing fuzz from becoming free and entangled, thus inhibiting pilling. The grafted structure enhances the bonding force between the finishing agent and the fiber, ensuring a long-lasting effect. This endows the piperazine-modified PLA finishing agent emulsion with the ability to achieve its effects through a process of "lubrication and friction reduction - film formation and fiber fixation - boundary..." The "surface anchoring" triple synergistic effect significantly improves the anti-pilling and anti-fuzzing properties of yarns. Divinylbenzene-modified acrylic fibers are prepared by reacting acrylonitrile, methyl acrylate, and divinylbenzene. The cyano group in acrylonitrile is a strong electron-withdrawing group, which reduces the electron cloud density of the double bond and results in high reactivity. The ester group in methyl acrylate is a moderate electron-withdrawing group, with a lower electron cloud density in the double bond than acrylonitrile, resulting in slightly lower reactivity. Divinylbenzene contains a benzene ring and conjugated double bonds. The benzene ring in divinylbenzene reacts first with the cyano group, and then the remaining conjugated double bonds in the molecule react with the ester group. By connecting two linear chains with divinylbenzene to form a bridging structure, a three-dimensional network structure is obtained. Crosslinking restricts the slippage and free movement of molecular chains, enhances the rigidity of the acrylic fiber structure, and reduces slippage and breakage of the fiber under stress, thus reducing the probability of fuzz formation. By enhancing the structural strength of the fiber itself and optimizing the surface treatment process, the yarn is less prone to damage under stress and friction, thereby extending the service life of the fabric, reducing pilling and fuzzing, and greatly improving the durability and user experience of the fabric. Detailed Implementation
[0030] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0031] Example 1:
[0032] This embodiment describes a method for preparing anti-pilling yarn for abrasion-resistant fabrics, including the following steps:
[0033] Step S1: Add 156 mL of tetramethylcyclotetrasiloxane and 6.34 mL of 3-piperazinylpropylmethyldimethoxysilane to a four-necked flask equipped with a reflux condenser, thermometer, and stirrer. Stir at 50 r / min. Dissolve 0.6 g of potassium hydroxide in 5 mL of deionized water and add it to the flask. Heat to 125 °C and maintain the temperature for 3 h. Add 19.63 mL of hexamethyldisiloxane and maintain the temperature for 1 h to obtain piperazine-based polysiloxane.
[0034] Step S2: Add 80 mL of lactic acid, 120 mL of diphenyl ether and 0.5 g of stannous chloride to a three-necked flask equipped with a stirrer and thermometer. Use a circulating water vacuum pump to evacuate and maintain a vacuum of 40 Pa. Heat to 110 °C at 300 r / min and react for 2 h, then heat to 130 °C and react for 3 h, then heat to 150 °C and react at 20 Pa for 6 h. Remove diphenyl ether by rotary evaporation, precipitate with ethanol, and filter to obtain polylactic acid prepolymer.
[0035] Step S3: Add 85g of polylactic acid prepolymer and 150mL of acetone to a three-necked flask equipped with a stirrer and thermometer. Purge with nitrogen for protection and stir at 50r / min for 10min. Heat to 25℃. Dissolve 15g of piperazine-based polysiloxane in 50mL of tetrahydrofuran and add it dropwise to the flask. Add 2g of dicumyl peroxide and react at 110℃ and 2kPa for 2h. Cool to 70℃, add glacial acetic acid to adjust the pH to 6, add 2g of sodium dodecylbenzenesulfonate and 10mL of deionized water, and emulsify at 1000r / min for 1h. Remove acetone by vacuum distillation to obtain piperazine-modified polylactic acid finishing agent emulsion.
[0036] Step S4: Add 75 mL acrylonitrile, 9 mL methyl acrylate, 200 mL N,N-dimethylformamide, and 6 mL polyethylene glycol to a four-necked flask equipped with a stirrer, thermometer, reflux condenser, and nitrogen delivery tube. Purge with nitrogen for protection and stir at 200 r / min for 20 min. Heat to 50 °C, add 15 mL divinylbenzene and stir for 10 min. Add 0.9 g azobisisobutyronitrile and heat to 63 °C for 3 h. Cool to 24 °C and add 0.15 g hydroquinone. Rotary evaporate, filter, wash twice with ethanol, and place in a drying oven to vacuum dry at 40 °C for 22 h to obtain divinylbenzene-modified polyacrylonitrile.
[0037] Step S5: Add 20g of divinylbenzene-modified polyacrylonitrile and 60mL of N,N-dimethylformamide to a reaction vessel equipped with a thermometer, let it stand at 40℃ for 30min, and then put the solution into a 50% N,N-dimethylacetamide coagulation bath through a spinneret. The fibers formed by spinning enter the first drawing tank at a temperature of 60℃, and then enter the second drawing bath at a temperature of 100℃ to obtain divinylbenzene-modified acrylic fibers.
[0038] Step S6: Weigh out 10 parts by weight of piperazine-modified polylactic acid finishing agent emulsion, 50 parts by weight of divinylbenzene-modified acrylic fiber and 30 parts by weight of polyester fiber, and set aside.
[0039] Step S7: Blend divinylbenzene modified acrylic fiber and polyester fiber to obtain blended fiber;
[0040] Step S8: Prepare a finishing solution by mixing piperazine-modified polylactic acid finishing agent emulsion at a ratio of 60 g / L. Immerse the yarn in the finishing solution at a bath ratio of 1:30 and perform finishing by two dips and two nips, with the tie weight controlled at 80%. After finishing, pre-dry the yarn at 90°C for 60 seconds, then bake it at 140°C for 60 seconds. After baking, wash the yarn three times and dry it to make abrasion-resistant fabric anti-pilling yarn.
[0041] Example 2:
[0042] This embodiment describes a method for preparing anti-pilling yarn for abrasion-resistant fabrics, including the following steps:
[0043] Step S1: Add 234 mL of tetramethylcyclotetrasiloxane and 9.51 mL of 3-piperazinylpropylmethyldimethoxysilane to a four-necked flask equipped with a reflux condenser, thermometer, and stirrer. Stir at 75 r / min. Dissolve 0.9 g of potassium hydroxide in 7 mL of deionized water and add it to the flask. Heat to 127 °C and maintain the temperature for 3.5 h. Add 29.45 mL of hexamethyldisiloxane and maintain the temperature for 1.5 h to obtain piperazine-based polysiloxane.
[0044] Step S2: Add 120 mL of lactic acid, 180 mL of diphenyl ether, and 0.75 g of stannous chloride to a three-necked flask equipped with a stirrer and thermometer. Use a circulating water vacuum pump to evacuate and maintain a vacuum of 40 Pa. Heat to 115 °C at 400 r / min and react for 2.5 h, then heat to 135 °C and react for 5 h, then heat to 155 °C and react at 20 Pa for 7 h. Remove diphenyl ether by rotary evaporation, precipitate with ethanol, and filter to obtain polylactic acid prepolymer.
[0045] Step S3: Add 127.5g of polylactic acid prepolymer and 225mL of acetone to a three-necked flask equipped with a stirrer and thermometer. Purge with nitrogen for protection and stir at 55r / min for 15min. Heat to 37℃. Dissolve 22.5g of piperazine-based polysiloxane in 75mL of tetrahydrofuran and add it dropwise to the flask. Add 3g of dicumyl peroxide and react at 115℃ and 3kPa for 3h. Cool to 77℃, add glacial acetic acid to adjust the pH to 6, add 3g of sodium dodecylbenzenesulfonate and 15mL of deionized water, and emulsify at 1250r / min for 1h. Remove acetone by vacuum distillation to obtain piperazine-modified polylactic acid finishing agent emulsion.
[0046] Step S4: Add 112 mL of acrylonitrile, 13 mL of methyl acrylate, 300 mL of N,N-dimethylformamide, and 9 mL of polyethylene glycol to a four-necked flask equipped with a stirrer, thermometer, reflux condenser, and nitrogen delivery tube. Purge with nitrogen for protection and stir at 250 r / min for 25 min. Heat to 55 °C, add 22 mL of divinylbenzene and stir for 15 min. Add 1.35 g of azobisisobutyronitrile (AIBN), heat to 65 °C and react for 3.5 h. Cool to 25 °C, add 0.225 g of hydroquinone, rotary evaporate, filter, wash three times with ethanol, and place in a drying oven to vacuum dry at 45 °C for 23 h to obtain divinylbenzene-modified polyacrylonitrile.
[0047] Step S5: Add 30g of divinylbenzene-modified polyacrylonitrile and 90mL of N,N-dimethylformamide to a reaction vessel equipped with a thermometer, let it stand at 40℃ for 30min, and then put the solution into a 50% N,N-dimethylacetamide coagulation bath through a spinneret. The fibers formed by spinning enter the first drawing tank at a temperature of 60℃, and then enter the second drawing bath at a temperature of 100℃ to obtain divinylbenzene-modified acrylic fibers.
[0048] Step S6: Weigh out 15 parts of piperazine-modified polylactic acid finishing agent emulsion, 60 parts of divinylbenzene-modified acrylic fiber, and 40 parts of polyester fiber according to the weight ratio, and set aside.
[0049] Step S7: Blend divinylbenzene modified acrylic fiber and polyester fiber to obtain blended fiber;
[0050] Step S8: Prepare a finishing solution by mixing piperazine-modified polylactic acid finishing agent emulsion at a ratio of 60 g / L. Immerse the yarn in the finishing solution at a bath ratio of 1:40 and perform finishing by two dips and two nips, with the tie weight controlled at 80%. After finishing, pre-dry the yarn at 90°C for 60 seconds, then bake it at 155°C for 120 seconds. After baking, wash the yarn 4 times and dry it to make abrasion-resistant fabric with anti-pilling yarn.
[0051] Example 3:
[0052] This embodiment describes a method for preparing anti-pilling yarn for abrasion-resistant fabrics, including the following steps:
[0053] Step S1: Add 312 mL of tetramethylcyclotetrasiloxane and 12.68 mL of 3-piperazinylpropylmethyldimethoxysilane to a four-necked flask equipped with a reflux condenser, thermometer, and stirrer. Stir at 100 r / min. Dissolve 1.2 g of potassium hydroxide in 10 mL of deionized water and add it to the flask. Heat to 130 °C and maintain the temperature for 4 h. Add 39.26 mL of hexamethyldisiloxane and maintain the temperature for 2 h to obtain piperazine-based polysiloxane.
[0054] Step S2: Add 160 mL of lactic acid, 240 mL of diphenyl ether and 1.0 g of stannous chloride to a three-necked flask equipped with a stirrer and thermometer. Use a circulating water vacuum pump to evacuate and maintain a vacuum of 40 Pa. Heat to 120 °C at 500 r / min and react for 3 h, then heat to 140 °C and react for 7 h, then heat to 160 °C and react at 20 Pa for 8 h. Remove diphenyl ether by rotary evaporation, precipitate with ethanol, and filter to obtain polylactic acid prepolymer.
[0055] Step S3: Add 170g of polylactic acid prepolymer and 300mL of acetone to a three-necked flask equipped with a stirrer and thermometer. Purge with nitrogen for protection and stir at 60r / min for 20min. Heat to 50℃. Dissolve 30g of piperazine-based polysiloxane in 100mL of tetrahydrofuran and add it dropwise to the flask. Add 4g of dicumyl peroxide and react at 120℃ and 4kPa for 4h. Cool to 85℃, add glacial acetic acid to adjust the pH to 7, add 4g of sodium dodecylbenzenesulfonate and 20mL of deionized water, and emulsify at 1500r / min for 1h. Remove acetone by vacuum distillation to obtain piperazine-modified polylactic acid finishing agent emulsion.
[0056] Step S4: Add 150 mL of acrylonitrile, 18 mL of methyl acrylate, 400 mL of N,N-dimethylformamide, and 12 mL of polyethylene glycol to a four-necked flask equipped with a stirrer, thermometer, reflux condenser, and nitrogen delivery tube. Purge with nitrogen for protection and stir at 300 r / min for 30 min. Heat to 60 °C, add 30 mL of divinylbenzene and stir for 20 min. Add 1.8 g of azobisisobutyronitrile (AIBN), heat to 67 °C and react for 4 h. Cool to 26 °C, add 0.3 g of hydroquinone, rotary evaporate, filter, wash 4 times with ethanol, and place in a drying oven to vacuum dry at 50 °C for 24 h to obtain divinylbenzene-modified polyacrylonitrile.
[0057] Step S5: Add 40g of divinylbenzene-modified polyacrylonitrile and 120mL of N,N-dimethylformamide to a reaction vessel equipped with a thermometer. Let it stand at 40℃ for 30min. Then, put the solution into a 50% N,N-dimethylacetamide coagulation bath through a spinneret. The fibers formed by spinning enter the first drawing bath at 60℃ and then enter the second drawing bath at 100℃ to obtain divinylbenzene-modified acrylic fibers.
[0058] Step S6: Weigh out 20 parts by weight of piperazine-modified polylactic acid finishing agent emulsion, 70 parts by weight of divinylbenzene-modified acrylic fiber and 50 parts by weight of polyester fiber, and set aside.
[0059] Step S7: Blend divinylbenzene modified acrylic fiber and polyester fiber to obtain blended fiber;
[0060] Step S8: Prepare a finishing solution by mixing piperazine-modified polylactic acid finishing agent emulsion at a ratio of 60 g / L. Immerse the yarn in the finishing solution at a bath ratio of 1:50 and perform finishing by two dips and two nips, with the tie weight controlled at 80%. After finishing, pre-dry the yarn at 90°C for 60 seconds, then bake it at 170°C for 180 seconds. After baking, wash the yarn 5 times and dry it to make abrasion-resistant fabric anti-pilling yarn.
[0061] Comparative Example 1:
[0062] This comparative example illustrates a method for preparing an anti-pilling yarn for abrasion-resistant fabrics, comprising the following steps:
[0063] Step S1: Add 160 mL of lactic acid, 240 mL of diphenyl ether and 1.0 g of stannous chloride to a three-necked flask equipped with a stirrer and thermometer. Use a circulating water vacuum pump to evacuate and maintain a vacuum of 40 Pa. Heat to 120 °C at 500 r / min and react for 3 h, then heat to 140 °C and react for 7 h, then heat to 160 °C and react at 20 Pa for 8 h. Remove diphenyl ether by rotary evaporation, precipitate with ethanol, and filter to obtain polylactic acid prepolymer.
[0064] Step S2: Add 170g of polylactic acid prepolymer and 300mL of acetone to a three-necked flask equipped with a stirrer and thermometer, purge with nitrogen for protection, stir at 60r / min for 20min, heat to 50℃, add 4g of sodium dodecylbenzenesulfonate and 20mL of deionized water, emulsify at 1500r / min for 1h, remove acetone by vacuum distillation to obtain polylactic acid finishing agent emulsion;
[0065] Step S3: Add 150 mL of acrylonitrile, 18 mL of methyl acrylate, 400 mL of N,N-dimethylformamide, and 12 mL of polyethylene glycol to a four-necked flask equipped with a stirrer, thermometer, reflux condenser, and nitrogen delivery tube. Purge with nitrogen for protection and stir at 300 r / min for 30 min. Heat to 60 °C, add 30 mL of divinylbenzene and stir for 20 min. Add 1.8 g of azobisisobutyronitrile (AIBN), heat to 67 °C and react for 4 h. Cool to 26 °C, add 0.3 g of hydroquinone, rotary evaporate, filter, wash 4 times with ethanol, and place in a drying oven to vacuum dry at 50 °C for 24 h to obtain divinylbenzene-modified polyacrylonitrile.
[0066] Step S4: Add 40g of divinylbenzene-modified polyacrylonitrile and 120mL of N,N-dimethylformamide to a reaction vessel equipped with a thermometer, let it stand at 40℃ for 30min, and then put the solution into a 50% N,N-dimethylacetamide coagulation bath through a spinneret. The fibers formed by spinning enter the first drawing bath at a temperature of 60℃, and then enter the second drawing bath at a temperature of 100℃ to obtain divinylbenzene-modified acrylic fibers.
[0067] Step S5: Weigh out 20 parts of polylactic acid finishing agent emulsion, 70 parts of divinylbenzene modified acrylic fiber and 50 parts of polyester fiber according to the weight ratio, and set aside.
[0068] Step S6: Blend divinylbenzene modified acrylic fiber and polyester fiber to obtain blended fiber;
[0069] Step S7: Prepare a finishing solution by mixing polylactic acid finishing agent emulsion at a ratio of 60g / L. Immerse the yarn in the finishing solution at a bath ratio of 1:50 and perform finishing by two dips and two nips, with the tie weight controlled at 80%. After finishing, pre-dry the yarn at 90℃ for 60s, then bake it at 170℃ for 180s. After baking, wash the yarn 5 times and dry it to make abrasion-resistant fabric with anti-pilling yarn.
[0070] Comparative Example 2:
[0071] This comparative example illustrates a method for preparing an anti-pilling yarn for abrasion-resistant fabrics, comprising the following steps:
[0072] Step S1: Add 312 mL of tetramethylcyclotetrasiloxane and 12.68 mL of 3-piperazinylpropylmethyldimethoxysilane to a four-necked flask equipped with a reflux condenser, thermometer, and stirrer. Stir at 100 r / min. Dissolve 1.2 g of potassium hydroxide in 10 mL of deionized water and add it to the flask. Heat to 130 °C and maintain the temperature for 4 h. Add 39.26 mL of hexamethyldisiloxane and maintain the temperature for 2 h to obtain piperazine-based polysiloxane.
[0073] Step S2: Add 160 mL of lactic acid, 240 mL of diphenyl ether and 1.0 g of stannous chloride to a three-necked flask equipped with a stirrer and thermometer. Use a circulating water vacuum pump to evacuate and maintain a vacuum of 40 Pa. Heat to 120 °C at 500 r / min and react for 3 h, then heat to 140 °C and react for 7 h, then heat to 160 °C and react at 20 Pa for 8 h. Remove diphenyl ether by rotary evaporation, precipitate with ethanol, and filter to obtain polylactic acid prepolymer.
[0074] Step S3: Add 170g of polylactic acid prepolymer and 300mL of acetone to a three-necked flask equipped with a stirrer and thermometer. Purge with nitrogen for protection and stir at 60r / min for 20min. Heat to 50℃. Dissolve 30g of piperazine-based polysiloxane in 100mL of tetrahydrofuran and add it dropwise to the flask. Add 4g of dicumyl peroxide and react at 120℃ and 4kPa for 4h. Cool to 85℃, add glacial acetic acid to adjust the pH to 7, add 4g of sodium dodecylbenzenesulfonate and 20mL of deionized water, and emulsify at 1500r / min for 1h. Remove acetone by vacuum distillation to obtain piperazine-modified polylactic acid finishing agent emulsion.
[0075] Step S4: Add 150 mL of acrylonitrile, 400 mL of N,N-dimethylformamide and 12 mL of polyethylene glycol to a four-necked flask equipped with a stirrer, thermometer, reflux condenser and nitrogen delivery tube. Purge with nitrogen for protection and stir at 300 r / min for 30 min. Heat to 60 °C, add 1.8 g of azobisisobutyronitrile, heat to 67 °C and react for 4 h. Cool to 26 °C, add 0.3 g of hydroquinone, rotary evaporate, filter and wash 4 times with ethanol. Place in a drying oven and vacuum dry at 50 °C for 24 h to obtain polyacrylonitrile.
[0076] Step S5: Add 40g of polyacrylonitrile and 120mL of N,N-dimethylformamide to a reaction vessel equipped with a thermometer, let it stand at 40℃ for 30min, and then put the solution into a 50% N,N-dimethylacetamide coagulation bath through a spinneret. The fibers formed by spinning enter the first drawing tank at a temperature of 60℃, and then enter the second drawing tank at a temperature of 100℃ to obtain acrylic fibers.
[0077] Step S6: Weigh out 20 parts by weight of piperazine-modified polylactic acid finishing agent emulsion, 70 parts by weight of acrylic fiber and 50 parts by weight of polyester fiber, and set aside.
[0078] Step S7: Blend acrylic fiber and polyester fiber to obtain blended fiber;
[0079] Step S8: Prepare a finishing solution by mixing piperazine-modified polylactic acid finishing agent emulsion at a ratio of 60 g / L. Immerse the yarn in the finishing solution at a bath ratio of 1:50 and perform finishing by two dips and two nips, with the tie weight controlled at 80%. After finishing, pre-dry the yarn at 90°C for 60 seconds, then bake it at 170°C for 180 seconds. After baking, wash the yarn 5 times and dry it to make abrasion-resistant fabric anti-pilling yarn.
[0080] Comparative Example 3:
[0081] This comparative example illustrates a method for preparing an anti-pilling yarn for abrasion-resistant fabrics, comprising the following steps:
[0082] Step S1: Add 160 mL of lactic acid, 240 mL of diphenyl ether and 1.0 g of stannous chloride to a three-necked flask equipped with a stirrer and thermometer. Use a circulating water vacuum pump to evacuate and maintain a vacuum of 40 Pa. Heat to 120 °C at 500 r / min and react for 3 h, then heat to 140 °C and react for 7 h, then heat to 160 °C and react at 20 Pa for 8 h. Remove diphenyl ether by rotary evaporation, precipitate with ethanol, and filter to obtain polylactic acid prepolymer.
[0083] Step S2: Add 170g of polylactic acid prepolymer and 300mL of acetone to a three-necked flask equipped with a stirrer and thermometer, purge with nitrogen for protection, stir at 60r / min for 20min, heat to 50℃, add 4g of sodium dodecylbenzenesulfonate and 20mL of deionized water, emulsify at 1500r / min for 1h, remove acetone by vacuum distillation to obtain polylactic acid finishing agent emulsion;
[0084] Step S3: Add 150 mL of acrylonitrile, 400 mL of N,N-dimethylformamide and 12 mL of polyethylene glycol to a four-necked flask equipped with a stirrer, thermometer, reflux condenser and nitrogen delivery tube. Purge with nitrogen and stir at 300 r / min for 30 min. Heat to 60 °C, add 1.8 g of azobisisobutyronitrile, heat to 67 °C and react for 4 h. Cool to 26 °C, add 0.3 g of hydroquinone, rotary evaporate, filter and wash 4 times with ethanol. Place in a drying oven and vacuum dry at 50 °C for 24 h to obtain polyacrylonitrile.
[0085] Step S4: Add 40g of polyacrylonitrile and 120mL of N,N-dimethylformamide to a reaction vessel equipped with a thermometer, let it stand at 40℃ for 30min, and then put the solution into a 50% N,N-dimethylacetamide coagulation bath through a spinneret. The fibers formed by spinning enter the first drawing tank at a temperature of 60℃, and then enter the second drawing bath at a temperature of 100℃ to obtain acrylic fibers.
[0086] Step S5: Weigh out 20 parts of polylactic acid finishing agent emulsion, 70 parts of acrylic fiber and 50 parts of polyester fiber according to the weight ratio, and set aside.
[0087] Step S6: Blend acrylic fiber and polyester fiber to obtain blended fiber;
[0088] Step S7: Prepare a finishing solution by mixing polylactic acid finishing agent emulsion at a ratio of 60g / L. Immerse the yarn in the finishing solution at a bath ratio of 1:50 and perform finishing by two dips and two nips, with the tie weight controlled at 80%. After finishing, pre-dry the yarn at 90℃ for 60s, then bake it at 170℃ for 180s. After baking, wash the yarn 5 times and dry it to make abrasion-resistant fabric with anti-pilling yarn.
[0089] Performance testing
[0090] The anti-pilling yarns of Examples 1-3 and Comparative Examples 1-3 were woven into fabrics using a rapier loom. The fabrics were tested according to GB / T 4802.3-2008 "Textiles - Determination of Pilling Properties - Part 3: Pilling Box Method" to obtain the anti-pilling grade; the fabrics were tested according to GB / T 3917.3-2025 "Textiles - Tear Properties - Part 3: Determination of Tear Strength of Trapezoidal Specimens" to obtain the tear performance; the fabrics were tested according to GB / T 3923.1-1997 "Textiles - Tensile Properties - Part 1: Determination of Breaking Strength and Elongation at Break" to obtain the breaking strength; the fabrics were tested according to FZ / T01054-2012 "Experimental Method for Surface Friction Properties of Fabrics" to obtain the kinetic friction coefficient; and the fabrics were tested according to GB / T The bending stiffness of fabrics is obtained by testing them according to 18318.1-2009 "Determination of bending properties of textiles - Part 1: Inclined plane method".
[0091]
[0092] Referring to the table above, based on the comparison between Examples 1-3 and Comparative Examples 1-3, it can be seen that the yarn obtained by blending divinylbenzene modified acrylic fiber with polyester after adding piperazine-modified polylactic acid finishing agent emulsion has good anti-pilling and anti-fuzzing properties.
[0093] Based on the comparison between Example 3 and Comparative Example 1, it can be seen that the anti-pilling grade of the yarn obtained by blending divinylbenzene modified acrylic fiber with polyester with piperazine-modified polylactic acid finishing agent emulsion is higher than that of the yarn obtained by blending divinylbenzene modified acrylic fiber with polyester with polylactic acid finishing agent emulsion. This indicates that the fabric made from the yarn obtained by blending divinylbenzene modified acrylic fiber with polyester with piperazine-modified polylactic acid finishing agent emulsion has good abrasion resistance.
[0094] Based on the comparison between Example 3 and Comparative Example 2, it can be seen that the anti-pilling grade of the yarn obtained by blending divinylbenzene modified acrylic fiber with polyester with piperazine-modified polylactic acid finishing agent emulsion is higher than that of the yarn obtained by blending acrylic fiber with polyester with piperazine-modified polylactic acid finishing agent emulsion. This indicates that the fabric made from the yarn obtained by blending divinylbenzene modified acrylic fiber with polyester with piperazine-modified polylactic acid finishing agent emulsion has good abrasion resistance.
[0095] Based on the comparison between Example 3 and Comparative Example 3, it can be seen that the anti-pilling grade of the yarn obtained by blending divinylbenzene modified acrylic fiber with polyester with piperazine-modified polylactic acid finishing agent emulsion is higher than that of the yarn obtained by blending acrylic fiber with polyester with polylactic acid finishing agent emulsion. This indicates that the fabric made from the yarn obtained by blending divinylbenzene modified acrylic fiber with polyester with piperazine-modified polylactic acid finishing agent emulsion has good abrasion resistance.
[0096] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.
[0097] The above description is merely an example and illustration of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described or use similar methods to replace them, as long as they do not deviate from the invention or exceed the scope defined in this application, they should all fall within the protection scope of the present invention.
Claims
1. A pilling-resistant yarn for abrasion-resistant fabrics, characterized in that, Includes the following components by weight: 10-20 parts of piperazine-modified polylactic acid finishing agent emulsion, 50-70 parts of divinylbenzene-modified acrylic fiber, and 30-50 parts of polyester fiber; The piperazine-modified polylactic acid finishing agent emulsion is prepared by the following steps: Step A1: Add tetramethylcyclotetrasiloxane and 3-piperazinylpropylmethyldimethoxysilane to a flask and stir. Dissolve potassium hydroxide in deionized water and add it to the flask. Heat the mixture and maintain the temperature for the reaction. Add hexamethyldisiloxane and maintain the temperature for the reaction to obtain piperazine polysiloxane. Step A2: Add lactic acid, diphenyl ether and stannous chloride to a flask, use a circulating water vacuum pump to evacuate and maintain the vacuum level, heat the reaction at 300-500 r / min, heat the reaction at 20 Pa, remove the diphenyl ether by rotary evaporation, precipitate with ethanol, and filter to obtain polylactic acid prepolymer. Step A3: Add polylactic acid prepolymer and acetone to a flask, purge with nitrogen and stir, heat, dissolve piperazine-based polysiloxane in tetrahydrofuran and add dropwise to the flask, add dicumyl peroxide to react, cool, add glacial acetic acid to adjust pH, add sodium dodecylbenzenesulfonate and deionized water to emulsify, remove acetone by vacuum distillation, and obtain piperazine-modified polylactic acid finishing agent emulsion.
2. The anti-pilling yarn for abrasion-resistant fabrics according to claim 1, characterized in that, The ratio of octamethylcyclotetrasiloxane, 3-piperazinylpropylmethyldimethoxysilane, potassium hydroxide, deionized water, and hexamethyldisiloxane used in step A1 is 156-312 mL : 6.34-12.68 mL : 0.6-1.2 g : 5-10 mL : 19.63-39.26 mL.
3. The anti-pilling yarn for abrasion-resistant fabrics according to claim 1, characterized in that, In step A2, the ratio of lactic acid, diphenyl ether, and stannous chloride is 80-160 mL : 120-240 mL : 0.5-1.0 g; the mass fraction of the lactic acid is 90%.
4. The anti-pilling yarn for abrasion-resistant fabrics according to claim 1, characterized in that, The ratio of polylactic acid prepolymer, acetone, piperazine polysiloxane, tetrahydrofuran, dicumyl peroxide, sodium dodecylbenzenesulfonate, and deionized water in step A3 is 85-170g: 150-300mL: 15-30g: 50-100mL: 2-4g: 2-4g: 10-20mL.
5. The anti-pilling yarn for abrasion-resistant fabrics according to claim 1, characterized in that, The divinylbenzene-modified acrylic fiber is prepared by the following steps: Step B1: Acrylonitrile, methyl acrylate, N,N-dimethylformamide and polyethylene glycol are added to a flask, nitrogen gas is introduced for protection and stirring is performed, divinylbenzene is added and stirred, azobisisobutyronitrile is added and heated to react, hydroquinone is added after cooling, rotary evaporation is performed, the mixture is filtered, washed with ethanol, and dried under vacuum to obtain divinylbenzene modified polyacrylonitrile. Step B2: Add divinylbenzene-modified polyacrylonitrile and N,N-dimethylformamide to a reactor equipped with a thermometer, let it stand at 40°C for 30 minutes, and then let the solution enter the N,N-dimethylacetamide coagulation bath through the spinneret. The fibers formed by spinning enter the first drawing bath at 60°C, and then enter the second drawing bath at 100°C to obtain divinylbenzene-modified acrylic fibers.
6. The anti-pilling yarn for abrasion-resistant fabric according to claim 5, characterized in that, In step B1, the ratio of acrylonitrile, methyl acrylate, N,N-dimethylformamide, polyethylene glycol, divinylbenzene, azobisisobutyronitrile, and hydroquinone is 75-150 mL: 9-18 mL: 200-400 mL: 6-12 mL: 15-30 mL: 0.9-1.8 g: 0.15-0.3 g; the polyethylene glycol is PEG-200.
7. The anti-pilling yarn for abrasion-resistant fabric according to claim 5, characterized in that, In step B2, the ratio of divinylbenzene-modified polyacrylonitrile to N,N-dimethylformamide is 20-40g:60-120mL.
8. The anti-pilling yarn for abrasion-resistant fabric according to claim 5, characterized in that, The mass fraction of the N,N-dimethylacetamide coagulation bath mentioned in step B2 is 50%.
9. The anti-pilling yarn for abrasion-resistant fabric according to claim 5, characterized in that, The spinneret cap described in step B2 has a specification of Ф200×0.075mm.
10. A process for preparing anti-pilling yarn for abrasion-resistant fabrics, characterized in that, Includes the following steps: Step 1: Weigh out 10-20 parts of piperazine-modified polylactic acid finishing agent emulsion, 50-70 parts of divinylbenzene-modified acrylic fiber, and 30-50 parts of polyester fiber according to the weight ratio, and set aside. Step 2: Blend divinylbenzene modified acrylic fiber and polyester fiber to obtain blended fiber; Step 3: Prepare a finishing solution by mixing piperazine-modified polylactic acid finishing agent emulsion at a concentration of 60 g / L. Immerse the yarn in the finishing solution at a bath ratio of 1:30-50 and perform finishing using a two-dip, two-nip method, controlling the tie weight at 80%. After finishing, pre-dry the yarn at 90℃ for 60 seconds, then bake it at 140-170℃ for 60-180 seconds. After baking, wash the yarn 3-5 times and dry it to make abrasion-resistant, anti-pilling yarn for fabrics.