Windproof and breathable composite fabric and its application

Abstract

The invention discloses a windproof and breathable composite fabric and application thereof, and is used to solve the technical problem in the prior art that the windproof and breathable performance, wear resistance, antistatic performance and wash resistance of polyester fiber fabrics need to be further improved. The invention is processed by the following steps: placing a blank in a pretreatment solution for pretreatment to obtain a pretreated grey cloth; using a modified quaternary ammonium salt as a crosslinking agent to promote crosslinking of a polyurethane prepolymer co-blocked with modified polysiloxane and polyethylene glycol to prepare an epoxy-terminated modified polyurethane; and dispersing and mixing the modified polyurethane with tetrabutyl titanate in an alkaline emulsion to prepare a finishing solution for padding and modification of the pretreated grey cloth. This not only effectively improves the windproof and moisture permeability performance of the composite fabric, but also improves its antistatic performance and wear resistance and pilling resistance.

Description

Technical Field

[0001] The present invention relates to the technical field of fabric processing, and in particular to a windproof and breathable composite fabric and application thereof. Background Art

[0002] Down jackets and cotton jackets are essential winter clothing. They are popular among people because they are comfortable and light to wear and can provide people with the best warmth. Polyester fiber fabrics are wrinkle-resistant, heat-resistant, chemical-resistant and easy to clean and maintain, and are widely used in clothing processing.

[0003] Polyester fiber fabrics in the prior art are prone to pilling and static electricity during use, and have poor moisture permeability. In order to improve the relevant properties of polyester fiber fabrics, the fabrics are usually subjected to padding modification to form a padding modification layer on the fabric fibers. However, conventional padding modification is to form a physical coating on the fabric fibers through simple physical padding. The padding modification layer is easily destroyed, resulting in a gradual decrease in its antistatic and anti-pilling properties. In addition, the padding modification forms a modified film layer on the fabric layer, which increases the coarseness of the fibers, reduces the size of the gaps between the fabric fibers, and further reduces the moisture permeability of the polyester fiber fabric.

[0004] In view of the technical defects in this aspect, a solution is now proposed. Summary of the Invention

[0005] The purpose of the present invention is to provide a windproof and breathable composite fabric and its application, which is used to solve the technical problem in the prior art that the windproof and breathable performance, wear resistance, antistatic performance and washability of polyester fiber fabrics need to be further improved.

[0006] The purpose of the present invention can be achieved by the following technical solution: A windproof and breathable composite fabric is obtained by processing the following steps:

[0007] S1, placing the blank in a pretreatment solution for pretreatment to obtain a pretreated grey cloth;

[0008] S2. Under inert gas protection, polyethylene glycol, hydroxyl-terminated polysiloxane, a catalyst and butanone are mixed, the reaction system temperature is raised to 70-78° C., isophorone diisocyanate is added to the reaction system, and the reaction is kept warm for 90-120 min to obtain a polyurethane prepolymer, a modified quaternary ammonium salt is added to the reaction system, and the reaction is kept warm for 70-90 min, 2-(oxirane-2-yl)ethanol-1-ol is added to the reaction system, and the reaction is kept warm for 60-80 min, and post-processed to obtain a modified polyurethane;

[0009] The synthetic reaction formula of modified polyurethane is:

[0010]

[0011]

[0012] Where:

[0013] ;

[0014] ;

[0015] .

[0016] The synthetic reaction mechanism of modified polyurethane is:

[0017] During the reaction process, hydroxyl groups on polyethylene glycol and hydroxyl-terminated polysiloxane molecular chains are used as active reaction groups to condense with isocyanate groups on isophorone diisocyanate molecules. By controlling the molar ratio of isocyanate groups to hydroxyl groups, a polyurethane prepolymer having isocyanate-terminated polyethylene glycol and hydroxyl-terminated polysiloxane co-blocked segments is prepared. Then, polyvalent hydroxyl groups on modified quaternary ammonium salt molecules are used as active sites to promote crosslinking of polyurethane prepolymer molecular chains. 2-(oxirane-2-yl)ethane-1-ol is used as a capping agent, and the hydroxyl groups on its molecules are used as active groups to condense with isocyanate groups on crosslinked polyurethane prepolymer molecules to form epoxy modifications, thereby preparing a modified polyurethane.

[0018] S3, mixing the modified polyurethane, tetrabutyl titanate and emulsion, and emulsifying at high speed for 60-80 minutes to obtain a finishing liquid;

[0019] S4, immersing the modified grey fabric in a finishing liquid, and adopting a double-immersion and double-rolling finishing method to obtain a composite fabric.

[0020] Furthermore, in step S1, the pretreatment method is: adding the grey cloth to a pretreatment solution at a temperature of 60-70°C, ultrasonically dispersing for 30-50 minutes, and adding 3-aminopropyltriethoxysilane solution to the pretreatment solution under ultrasonic dispersion. After the addition is completed, the pretreatment solution is kept warm for 60-80 minutes, and post-treated to obtain the pretreated grey cloth.

[0021] Furthermore, the grey cloth is a polyester fiber cloth, and the usage ratio of the grey cloth, the pretreatment solution and the 3-aminopropyltriethoxysilane solution is 5g:70mL:5g, the pretreatment solution is composed of sodium hydroxide, purified water, sodium lauryl sulfate and 30wt% hydrogen peroxide in the ratio of 8-10g:100mL:3g:15-20mL, and the 3-aminopropyltriethoxysilane solution is composed of 3-aminopropyltriethoxysilane and anhydrous ethanol in the ratio of 1g:3mL. The post-treatment includes: after the treatment is completed, removing the grey cloth from the solution, washing it with purified water to neutrality and then drying it to obtain the pretreated grey cloth.

[0022] Furthermore, in step S2, the amount ratio of the polyethylene glycol, hydroxyl-terminated polysiloxane, catalyst and butanone is 10g:3g:0.1g:30mL, and during the preparation of the polyurethane prepolymer, the molar ratio of the hydroxyl group to the isocyanate group is 1:1.1, the catalyst is dibutyltin dilaurate, and the weight ratio of the polyethylene glycol, modified quaternary ammonium salt and 2-(oxirane-2-yl)ethanol-1-ol is 10:1.2-1.5:4. The post-treatment includes: after the reaction is completed, the reaction system is kept warm at 70-78°C, and low-boiling substances are removed under reduced pressure to obtain a modified polyurethane.

[0023] Furthermore, in step S3, the modified polyurethane, tetrabutyl titanate and emulsion are used in a ratio of 10-20 g:0.8-1.2 g:40-60 mL, and the emulsion is composed of deionized water, hexadecyltrimethylammonium chloride, emulsifier AEO-4, Tween-80 and sodium carbonate in a ratio of 100 mL:2 g:1 g:1 g:15 g.

[0024] Furthermore, in step S4, the two-immersion and two-rolling finishing operation includes: transporting the modified grey cloth to an immersion tank filled with a finishing liquid, dipping for 5-7 minutes, rolling out excess finishing liquid at a rolling rate of 30-40%, immersing the grey cloth in the finishing liquid again, dipping for 3-5 minutes, rolling out excess finishing liquid at a rolling rate of 75-85%, and obtaining a padded grey cloth, transferring the padded grey cloth to a heat setting machine at a temperature of 80-90°C for pre-drying for 3-5 minutes, and then transferring it to a dryer at a temperature of 140-150°C for drying to obtain a composite fabric crude product, and rubbing the composite fabric crude product with purified water and drying it to obtain a composite fabric.

[0025] Furthermore, the preparation method of hydroxyl-terminated polysiloxane is as follows: octamethylcyclotetrasiloxane, modified pyrimidine and xylene are mixed, a catalyst is added to the reaction system, the temperature of the reaction system is increased to 105-115°C, the reaction is kept warm for 3-4 hours, 1,3-bis(3-hydroxypropyl)-1,1,3,3-tetramethyldisiloxane is added to the reaction system, the reaction is kept warm for 4-6 hours, and post-processed to obtain hydroxyl-terminated polysiloxane.

[0026] The synthetic reaction formula of hydroxyl-terminated polysiloxane is:

[0027]

[0028] Where:

[0029]

[0030] The synthesis reaction mechanism of hydroxyl-terminated polysiloxane is:

[0031] During the reaction, under the action of high temperature and catalyst, octamethylcyclotetrasiloxane is partially hydrolyzed to form a polysiloxane chain modified with silanol. At the same time, the siloxane bonds on the modified pyrimidine molecules are hydrolyzed to form silanol groups. The silanol groups condense to form silicon-oxygen-silicon bonds, thereby preparing a long polysiloxane chain modified with 2,6-dichloropyrimidine molecules. 1,3-bis(3-hydroxypropyl)-1,1,3,3-tetramethyldisiloxane molecules serve as end-capping agents. After hydrolysis, the silanol groups formed condense with the polysiloxane molecular chains to form hydroxyl modifications, thereby preparing a hydroxyl-terminated polysiloxane.

[0032] Furthermore, the amount ratio of the octamethylcyclotetrasiloxane, modified pyrimidine, xylene, catalyst and 1,3-bis(3-hydroxypropyl)-1,1,3,3-tetramethyldisiloxane is 7g:2g:50mL:5mL:1g, the catalyst is a 10wt% formic acid aqueous solution, and the post-treatment includes: after the reaction is completed, the temperature of the reaction system is lowered to room temperature, sodium hydroxide solution is added to the reaction system, the pH of the system is adjusted to 7, the liquid is allowed to stand, the organic phase is washed with purified water three times, and the xylene is evaporated under reduced pressure to obtain a hydroxyl-terminated polysiloxane.

[0033] Furthermore, the preparation method of the modified pyrimidine is as follows: under the protection of inert gas, 4-amino-2,6-dichloropyrimidine and tetrahydrofuran are mixed, the temperature of the reaction system is increased to 50-60°C, 3-isocyanatopropylmethyldiethoxysilane is added to the reaction system, the reaction is kept warm for 60-90 minutes, and post-processed to obtain the modified pyrimidine.

[0034] The synthetic reaction formula of modified pyrimidine is:

[0035]

[0036] The synthetic reaction mechanism of modified pyrimidine is:

[0037] During the reaction, the amino group on the 4-amino-2,6-dichloropyrimidine molecule undergoes a condensation reaction with the isocyanate group on the 3-isocyanatepropylmethyldiethoxysilane molecule, and the methyldiethoxysilane is modified on the 2,6-dichloropyrimidine molecule to prepare a modified pyrimidine;

[0038] The mass spectrometry data of modified pyrimidine are: m / z:380.0838 (100.0%), 382.0809 (63.9%),

[0039] 381.0872(14.1%),384.0779(10.2%),383.0842(9.0%),381.0834(5.1%),382.0807(3.3%),383.0804(3.2%),384.0777(2.1%),381.0809(1.5%),385.0813(1.4%).

[0040] Furthermore, the amount ratio of the 4-amino-2,6-dichloropyrimidine and 3-isocyanatopropylmethyldiethoxysilane is 1 mol:1 mol, and the amount ratio of the 4-amino-2,6-dichloropyrimidine and tetrahydrofuran is 1 g:7 mL. The post-treatment includes: after the reaction is completed, distilling off the tetrahydrofuran under reduced pressure to obtain modified pyrimidine.

[0041] Furthermore, the preparation method of the modified quaternary ammonium salt is as follows: under the protection of inert gas, 1,4-dichlorobenzyl, triethanolamine and tetrahydrofuran are mixed, the temperature of the reaction system is increased to the system reflux, the reaction is kept warm for 6-8 hours, and post-processed to obtain the modified quaternary ammonium salt.

[0042] The synthetic reaction formula of modified quaternary ammonium salt is:

[0043]

[0044] The synthetic reaction mechanism of modified quaternary ammonium salt is:

[0045] During the reaction, 1,4-dichlorobenzyl, as a halogenated hydrocarbon, contains a chlorine atom on its molecule that can be attacked by a nucleophilic reagent. Ethanolamine, as a nucleophilic reagent, has a lone pair of electrons on its nitrogen atom that is nucleophilic. Tetrahydrofuran, as a solvent, provides a polar environment conducive to the reaction. Under high temperature, benzyl chloride undergoes a nucleophilic substitution reaction with the nitrogen atom to form a quaternary ammonium salt, thereby preparing a modified quaternary ammonium salt.

[0046] The mass spectrometry data of the modified quaternary ammonium salt are: m / z: 472.2107 (100.0%), 474.2077 (63.9%),

[0047] 473.2140(21.6%),475.2111(13.8%),476.2048(10.2%),474.2174(2.2%),477.2081(2.2%),476.2145(1.4%),474.2149(1.2%).

[0048] Furthermore, the ratio of 1,4-dichlorobenzyl to triethanolamine is 1 mol:2 mol, and the ratio of 1,4-dichlorobenzyl to tetrahydrofuran is 1 g:10 mL. The post-treatment includes: after the reaction is completed, distilling off tetrahydrofuran under reduced pressure to obtain a modified quaternary ammonium salt.

[0049] The present invention also provides an application of a windproof and breathable composite fabric, and applies the windproof and breathable composite fabric to clothing processing.

[0050] The present invention has the following beneficial effects:

[0051] 1. The windproof and breathable composite fabric of the present invention is prepared by soaking a polyester fiber cloth in a pretreatment solution. In the pretreatment solution, sodium hydroxide serves as an alkaline reagent, which helps to activate the surface of the polyester fiber cloth, partially hydrolyzes the ester bonds on the fiber surface, and increases the surface roughness and polarity. Hydrogen peroxide has oxidizing properties and can remove impurities and some oil stains on the fabric surface, further clean the fabric surface and induce weak oxidation on the fiber surface, thereby increasing reactive sites. The polyester fiber cloth is then modified with 3-aminopropyltriethoxysilane to introduce a large number of amino active sites into the polyester fiber cloth to prepare a pretreated grey cloth. After the grey cloth is finished with a finishing liquid, the epoxy groups on the finishing liquid molecules undergo ring-opening condensation with the amino groups to form a stable padding finishing layer on the polyester fiber fabric, making it more washable and improving the windproof and moisture-permeable, antistatic, wear-resistant and anti-pilling properties of the composite fabric.

[0052] 2. The windproof and breathable composite fabric of the present invention is obtained by introducing a polyurethane prepolymer co-blocked with hydroxyl-terminated polysiloxane modified with 2,6-dichloropyrimidine and polyethylene glycol on the modified polyurethane molecule. The polysiloxane chain segment has low surface energy and good flexibility, and can form a continuous thin film on the fiber surface of the fabric. Polyethylene glycol is a hydrophilic polymer. The hydroxyl groups on its chain segment can form hydrogen bonds with water molecules, thereby improving the moisture absorption and moisture permeability of the modified polyurethane. The 2,6-dichloropyrimidine modified on the hydroxyl-terminated polysiloxane molecular chain contains two chlorine atoms with high electronegativity and a pyrimidine ring in its molecular structure. The electronegativity of the chlorine atom attracts the surrounding electron cloud, thereby changing the charge distribution of the polyurethane prepolymer, resulting in stronger interaction forces between the polyurethane prepolymer chain segments, such as van der Waals forces and dipole-dipole interactions, further enhancing the intermolecular interaction forces, making the film layer formed by the finishing agent impregnated on the polyester fiber fabric more compact, thereby improving the fabric's windproof and moisture permeability and wear and anti-pilling properties.

[0053] 3. The windproof and breathable composite fabric of the present invention is prepared by adding tetrabutyl titanate to a finishing liquid. Under an alkaline emulsification environment, the tetrabutyl titanate is hydrolyzed to form cross-linked bonds with active groups such as imino groups and hydroxyl groups on modified polyurethane molecules, thereby forming titanium doping on the modified polyurethane and enhancing the conductivity of the padding layer. The modified quaternary ammonium salt is used as a cross-linking agent. The quaternary ammonium salt molecules have cationic properties and can form a charge conduction layer on the fiber surface. When the fabric is subjected to friction or contact, the static charge generated can be quickly dissipated through this charge conduction layer, thereby improving the antistatic properties of the composite fabric. The polyvalent hydroxyl groups on the modified quaternary ammonium salt molecules serve as reactive sites, thereby increasing the cross-linking points between polyurethane prepolymer molecular chains and making the film structure more stable. The windproof and moisture-permeable effects as well as the wear and anti-pilling properties are improved. Moreover, the polysiloxane chain segment has a low friction coefficient and good lubricity, and can form a lubricating layer on the surface of the fiber fabric to reduce friction and wear between fibers, thereby improving the wear and anti-pilling properties of the fiber fabric. By adding sodium carbonate to the emulsion, an alkaline environment is provided for the emulsion. When the pretreated grey fabric is padding-modified, the alkaline environment can promote the reaction between the epoxy groups on the modified polyurethane molecules and the active sites on the pretreated grey fabric molecules, thereby improving the padding modification effect and water-washing resistance of the modified grey fabric by the finishing liquid. At the same time, sodium carbonate, as a porogen, is removed by water washing, which can increase the porosity of the padding film layer and further improve the overall performance of the composite fabric. DETAILED DESCRIPTION

[0054] The technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0055] The polyethylene glycol used in this application is PEG-1000.

[0056] Example 1

[0057] This embodiment provides a method for preparing a windproof and breathable composite fabric, comprising the following steps:

[0058] S1. Preparation of pretreated grey cloth

[0059] Sodium hydroxide, purified water, sodium lauryl sulfate, and 30 wt% hydrogen peroxide were mixed in a ratio of 8 g:100 mL:3 g:15 mL to obtain a pretreatment solution for later use.

[0060] 3-Aminopropyltriethoxysilane and anhydrous ethanol were mixed at a ratio of 1 g:3 mL to obtain a 3-aminopropyltriethoxysilane solution for later use.

[0061] Weigh: 7000 mL of the pretreatment solution was placed in a beaker, the temperature of the beaker was raised to 60 ° C, 500 g of polyester fiber cloth was added to the beaker, and the polyester fiber cloth was completely immersed in the pretreatment solution. Ultrasonic dispersion was performed for 30 minutes. Under the ultrasonic dispersion state, 500 g of 3-aminopropyltriethoxysilane solution was added dropwise to the beaker. After the addition was completed, the heat treatment was carried out for 60 minutes. The grey cloth was removed from the beaker, washed with purified water until it was neutral, and then dried to obtain the pretreated grey cloth.

[0062] S2. Preparation of hydroxyl-terminated polysiloxane

[0063] Weigh: 16.4 g of 4-amino-2,6-dichloropyrimidine and 115 mL of tetrahydrofuran are added to a three-necked flask protected by nitrogen and stirred. The temperature of the three-necked flask is raised to 50°C. 21.7 g of 3-isocyanatopropylmethyldiethoxysilane is added to the three-necked flask and the reaction is kept warm for 60 minutes. The three-necked flask is kept warm at 50°C and low-boiling substances are evaporated under reduced pressure to obtain modified pyrimidine;

[0064] Weigh: 70 g of octamethylcyclotetrasiloxane, 20 g of modified pyrimidine and 500 mL of xylene are added to a three-necked flask and stirred. 50 mL of 10 wt% formic acid aqueous solution is added to the three-necked flask, the temperature of the three-necked flask is raised to 105 ° C, and the reaction is kept warm for 3 hours. 1,3-bis(3-hydroxypropyl)-1,1,3,3-tetramethyldisiloxane 10 g is added to the three-necked flask, and the reaction is kept warm for 4 hours. The temperature of the three-necked flask is lowered to room temperature, and 0.1 mol / L sodium hydroxide solution is added to the three-necked flask to adjust the pH of the system to 7. The liquid is separated by standing. The organic phase is washed 3 times with purified water and dried with anhydrous sodium sulfate for 2 hours. The organic phase is transferred to a rotary evaporator with a water bath temperature of 70 ° C, and low boiling points are evaporated under reduced pressure to obtain a hydroxyl-terminated polysiloxane.

[0065] S3. Preparation of modified quaternary ammonium salt

[0066] Weigh 17.5 g of 1,4-benzyl chloride, 29.8 g of triethanolamine, and 175 mL of tetrahydrofuran into a three-necked flask and stir. Raise the temperature of the three-necked flask to reflux and keep the reaction for 6 hours. Then lower the temperature of the three-necked flask to 50° C. and remove low-boiling substances by distillation under reduced pressure to obtain a modified quaternary ammonium salt.

[0067] S4. Preparation of modified polyurethane

[0068] Weigh: 50 g of polyethylene glycol, 15 g of hydroxyl-terminated polysiloxane, 0.5 g of dibutyltin dilaurate and 150 mL of butanone are added to a nitrogen-protected three-necked flask with stirring, the temperature of the three-necked flask is raised to 70° C., isophorone diisocyanate is weighed according to a molar ratio of hydroxyl to isocyanate group of 1:1.1, and added to the three-necked flask, and the reaction is kept warm for 90 min. 6 g of modified quaternary ammonium salt is added to the three-necked flask, and the reaction is kept warm for 70 min. 20 g of 2-(oxirane-2-yl)ethanol-1-ol is added to the three-necked flask, and the reaction is kept warm for 60 min. The three-necked flask is kept warm at 70° C., and low-boiling substances are removed by distillation under reduced pressure to obtain a modified polyurethane.

[0069] S5. Preparation of finishing liquid

[0070] Deionized water, hexadecyltrimethylammonium chloride, emulsifier AEO-4, Tween-80, and sodium carbonate were mixed uniformly in the ratio of 100 mL: 2 g: 1 g: 1 g: 15 g to obtain an emulsion, which was set aside.

[0071] The modified polyurethane, tetrabutyl titanate and emulsion were placed in a high-speed dispersant at a ratio of 10 g:0.8 g:40 mL, the stirring speed was set to 900 r / min, and the emulsification was carried out with high-speed stirring for 60 minutes to obtain a finishing liquid.

[0072] S6. Preparation of composite fabric

[0073] The modified grey fabric is transported to an impregnation tank filled with finishing liquid, and after impregnation for 5 minutes, the excess finishing liquid is squeezed out at a squeezing rate of 30% to obtain a once-impregnated fabric;

[0074] The once-impregnated cloth is immersed in the finishing liquid again for 3 minutes, and the excess finishing liquid is squeezed out at a rolling rate of 75% to obtain a second-impregnated cloth;

[0075] The padding fabric was transferred to a heat setting machine at 80°C for pre-drying for 3 minutes, and then transferred to a dryer at 140°C for drying to obtain a crude composite fabric;

[0076] The crude composite fabric product is washed with purified water and then air-dried to obtain the composite fabric.

[0077] Example 2

[0078] This embodiment provides a method for preparing a windproof and breathable composite fabric, comprising the following steps:

[0079] S1. Preparation of pretreated grey cloth

[0080] Sodium hydroxide, purified water, sodium lauryl sulfate, and 30 wt% hydrogen peroxide were mixed in a ratio of 9 g:100 mL:3 g:17 mL to obtain a pretreatment solution for later use.

[0081] 3-Aminopropyltriethoxysilane and anhydrous ethanol were mixed at a ratio of 1 g:3 mL to obtain a 3-aminopropyltriethoxysilane solution for later use.

[0082] Weigh: 7000 mL of the pretreatment solution was placed in a beaker, the temperature of the beaker was raised to 65 ° C, 500 g of polyester fiber cloth was added to the beaker, and the polyester fiber cloth was completely immersed in the pretreatment solution. Ultrasonic dispersion was performed for 40 minutes. Under the ultrasonic dispersion state, 500 g of 3-aminopropyltriethoxysilane solution was added dropwise to the beaker. After the addition was completed, the heat treatment was carried out for 70 minutes. The grey cloth was removed from the beaker, washed with purified water until it was neutral, and then dried to obtain a pretreated grey cloth.

[0083] S2. Preparation of hydroxyl-terminated polysiloxane

[0084] Weigh: 16.4 g of 4-amino-2,6-dichloropyrimidine and 115 mL of tetrahydrofuran are added to a three-necked flask protected by nitrogen and stirred. The temperature of the three-necked flask is raised to 55°C. 21.7 g of 3-isocyanatopropylmethyldiethoxysilane is added to the three-necked flask and the reaction is kept warm for 75 minutes. The three-necked flask is kept warm at 55°C and low-boiling substances are evaporated under reduced pressure to obtain modified pyrimidine;

[0085] Weigh: 70 g of octamethylcyclotetrasiloxane, 20 g of modified pyrimidine and 500 mL of xylene are added to a three-necked flask and stirred. 50 mL of 10 wt% formic acid aqueous solution is added to the three-necked flask, the temperature of the three-necked flask is raised to 110 ° C, and the reaction is kept warm for 3.5 hours. 1,3-bis(3-hydroxypropyl)-1,1,3,3-tetramethyldisiloxane 10 g is added to the three-necked flask, and the reaction is kept warm for 5 hours. The temperature of the three-necked flask is lowered to room temperature, and 0.15 mol / L sodium hydroxide solution is added to the three-necked flask to adjust the pH of the system to 7. The liquid is separated after standing. The organic phase is washed 3 times with purified water and dried with anhydrous sodium sulfate for 2.5 hours. The organic phase is transferred to a rotary evaporator with a water bath temperature of 75 ° C, and low boiling points are evaporated under reduced pressure to obtain a hydroxyl-terminated polysiloxane.

[0086] S3. Preparation of modified quaternary ammonium salt

[0087] Weigh 17.5 g of 1,4-benzyl chloride, 29.8 g of triethanolamine, and 175 mL of tetrahydrofuran into a three-necked flask and stir. Raise the temperature of the flask to reflux and keep the reaction for 7 hours. Then lower the temperature of the flask to 53°C and remove low-boiling substances under reduced pressure to obtain a modified quaternary ammonium salt.

[0088] S4. Preparation of modified polyurethane

[0089] Weigh: 50 g of polyethylene glycol, 15 g of hydroxyl-terminated polysiloxane, 0.5 g of dibutyltin dilaurate and 150 mL of butanone are added to a nitrogen-protected three-necked flask with stirring, the temperature of the three-necked flask is raised to 74 ° C, isophorone diisocyanate is weighed according to the molar ratio of hydroxyl group to isocyanate group of 1:1.1, and is added to the three-necked flask, and the reaction is kept warm for 105 min. 7.0 g of modified quaternary ammonium salt is added to the three-necked flask, and the reaction is kept warm for 80 min. 20 g of 2-(oxirane-2-yl)ethanol-1-ol is added to the three-necked flask, and the reaction is kept warm for 70 min. The three-necked flask is heated at 704 ° C, and low boiling points are removed by distillation under reduced pressure to obtain a modified polyurethane.

[0090] S5. Preparation of finishing liquid

[0091] Deionized water, hexadecyltrimethylammonium chloride, emulsifier AEO-4, Tween-80, and sodium carbonate were mixed uniformly in the ratio of 100 mL: 2 g: 1 g: 1 g: 15 g to obtain an emulsion, which was set aside.

[0092] The modified polyurethane, tetrabutyl titanate and emulsion were placed in a high-speed dispersant at a ratio of 15 g:1.0 g:50 mL, the stirring speed was set to 1050 r / min, and the emulsification was carried out with high-speed stirring for 70 minutes to obtain a finishing liquid.

[0093] S6. Preparation of composite fabric

[0094] The modified grey fabric is transported to an impregnation tank filled with finishing liquid, and after impregnation for 6 minutes, the excess finishing liquid is squeezed out at a squeezing rate of 35% to obtain a once-impregnated fabric;

[0095] The once-impregnated cloth is immersed in the finishing liquid again for 4 minutes, and the excess finishing liquid is squeezed out at a squeezing rate of 80% to obtain a second-impregnated cloth;

[0096] The padding fabric was transferred to a heat setting machine at 85°C for pre-drying for 4 minutes, and then transferred to a dryer at 145°C for drying to obtain a crude composite fabric;

[0097] The crude composite fabric product is washed with purified water and then air-dried to obtain the composite fabric.

[0098] Example 3

[0099] This embodiment provides a method for preparing a windproof and breathable composite fabric, comprising the following steps:

[0100] S1. Preparation of pretreated grey cloth

[0101] Sodium hydroxide, purified water, sodium lauryl sulfate, and 30 wt% hydrogen peroxide were mixed in a ratio of 10 g:100 mL:3 g:20 mL to obtain a pretreatment solution for later use.

[0102] 3-Aminopropyltriethoxysilane and anhydrous ethanol were mixed at a ratio of 1 g:3 mL to obtain a 3-aminopropyltriethoxysilane solution for later use.

[0103] Weigh: 7000 mL of the pretreatment solution was placed in a beaker, the temperature of the beaker was raised to 70°C, 500 g of polyester fiber cloth was added to the beaker, and the polyester fiber cloth was completely immersed in the pretreatment solution. Ultrasonic dispersion was performed for 50 minutes. Under ultrasonic dispersion, 500 g of 3-aminopropyltriethoxysilane solution was added dropwise to the beaker. After the addition was completed, the heat treatment was carried out for 80 minutes. The grey cloth was removed from the beaker, washed with purified water until it was neutral, and then dried to obtain a pretreated grey cloth.

[0104] S2. Preparation of hydroxyl-terminated polysiloxane

[0105] Weigh: 16.4 g of 4-amino-2,6-dichloropyrimidine and 115 mL of tetrahydrofuran are added to a nitrogen-protected three-necked flask and stirred. The temperature of the three-necked flask is raised to 60°C. 21.7 g of 3-isocyanatepropylmethyldiethoxysilane is added to the three-necked flask and the reaction is kept warm for 90 minutes. The three-necked flask is kept warm at 60°C and low-boiling substances are evaporated under reduced pressure to obtain modified pyrimidine;

[0106] Weigh: 70 g of octamethylcyclotetrasiloxane, 20 g of modified pyrimidine and 500 mL of xylene are added to a three-necked flask and stirred. 50 mL of 10 wt% formic acid aqueous solution is added to the three-necked flask, the temperature of the three-necked flask is raised to 115 ° C, and the reaction is kept warm for 4 hours. 1,3-bis(3-hydroxypropyl)-1,1,3,3-tetramethyldisiloxane 10 g is added to the three-necked flask, and the reaction is kept warm for 6 hours. The temperature of the three-necked flask is lowered to room temperature, and 0.2 mol / L sodium hydroxide solution is added to the three-necked flask to adjust the pH of the system to 7. The liquid is separated by standing. The organic phase is washed 3 times with purified water and dried with anhydrous sodium sulfate for 3 hours. The organic phase is transferred to a rotary evaporator with a water bath temperature of 80 ° C, and low boiling points are removed under reduced pressure to obtain a hydroxyl-terminated polysiloxane.

[0107] S3. Preparation of modified quaternary ammonium salt

[0108] Weigh: 17.5 g of 1,4-benzyl chloride, 29.8 g of triethanolamine and 175 mL of tetrahydrofuran are added into a three-necked flask and stirred. The temperature of the three-necked flask is raised to reflux and kept warm for 8 hours. The temperature of the three-necked flask is lowered to 55°C, and low-boiling substances are evaporated under reduced pressure to obtain a modified quaternary ammonium salt.

[0109] S4. Preparation of modified polyurethane

[0110] Weigh: 50 g of polyethylene glycol, 15 g of hydroxyl-terminated polysiloxane, 0.5 g of dibutyltin dilaurate and 150 mL of butanone are added to a nitrogen-protected three-necked flask with stirring, the temperature of the three-necked flask is raised to 78 ° C, isophorone diisocyanate is weighed according to the molar ratio of hydroxyl group to isocyanate group of 1:1.1, and is added to the three-necked flask, and the reaction is kept warm for 120 min. 7.5 g of modified quaternary ammonium salt is added to the three-necked flask, and the reaction is kept warm for 90 min. 20 g of 2-(oxirane-2-yl)ethanol-1-ol is added to the three-necked flask, and the reaction is kept warm for 80 min. The three-necked flask is kept warm at 78 ° C, and low-boiling substances are distilled off under reduced pressure to obtain a modified polyurethane.

[0111] S5. Preparation of finishing liquid

[0112] Deionized water, hexadecyltrimethylammonium chloride, emulsifier AEO-4, Tween-80, and sodium carbonate were mixed uniformly in the ratio of 100 mL: 2 g: 1 g: 1 g: 15 g to obtain an emulsion, which was set aside.

[0113] The modified polyurethane, tetrabutyl titanate and emulsion were placed in a high-speed dispersant at a ratio of 20 g:1.2 g:60 mL, the stirring speed was set to 1200 r / min, and the emulsification was carried out with high-speed stirring for 80 minutes to obtain a finishing liquid.

[0114] S6. Preparation of composite fabric

[0115] The modified grey fabric is transported to an impregnation tank filled with finishing liquid, and after impregnation for 7 minutes, the excess finishing liquid is squeezed out at a squeezing rate of 40% to obtain a once-impregnated fabric;

[0116] The once-impregnated cloth is immersed in the finishing liquid again for 5 minutes, and the excess finishing liquid is squeezed out at a rolling rate of 85% to obtain a second-impregnated cloth;

[0117] The padding fabric was transferred to a heat setting machine at a temperature of 90°C for pre-drying for 5 minutes, and then transferred to a dryer at a temperature of 150°C for drying to obtain a crude composite fabric;

[0118] The crude composite fabric product is washed with purified water and then air-dried to obtain the composite fabric.

[0119] Comparative Example 1

[0120] The difference between this comparative example and Example 3 is that in step S1, when preparing the pretreated grey cloth, no 3-aminopropyltriethoxysilane solution is added.

[0121] Comparative Example 2

[0122] The difference between this comparative example and Example 3 is that in step S2, when preparing the hydroxyl-terminated polysiloxane, no modified pyrimidine is added.

[0123] Comparative Example 3

[0124] The difference between this comparative example and Example 3 is that step S3 is eliminated, and the modified quaternary ammonium salt in step S4 is replaced by an equimolar amount of triethanolamine in step S3.

[0125] Comparative Example 4

[0126] The difference between this comparative example and Example 3 is that in step S5, no sodium carbonate is added to the emulsion.

[0127] Performance testing:

[0128] The air permeability and moisture permeability of the composite fabric samples prepared in Examples 1-3 and Comparative Examples 1-4 were measured with reference to Standard FZ / T01149-2019 “Evaluation of Windproof and Moisture Permeability of Textiles”;

[0129] The antistatic properties of the composite fabric samples prepared in Examples 1-3 and Comparative Examples 1-4 were measured with reference to the standard GB / T12703.1-2021 “Test method for electrostatic properties of textiles - Part 1: Corona charging method”;

[0130] The number of friction pilling of the composite fabric samples prepared in Examples 1-3 and Comparative Examples 1-4 was measured under a chuck pressure of 590 cN in accordance with the standard GB / T4802.1-2008 "Determination of the pilling properties of textile fabrics - Part 1: Circular locus method";

[0131] The composite fabric samples prepared in Examples 1-3 and Comparative Examples 1-4 were washed, and various properties of the samples after washing 80 times were measured according to the above standards. The specific test results are shown in Table 1 below.

[0132] Table 1-Performance test data of the sample

[0133]

[0134] Data Analysis:

[0135] Comparing and analyzing the data in Table 1 above, the air permeability of the composite fabric prepared by the present invention is reduced to 8.4 mm / s, and the moisture permeability reaches 5930 g / (m 2· 24h), the number of friction pilling reached 180 times, and, after being washed 80 times, the air permeability retention rate reached 95.45%, the moisture permeability retention rate reached 98.02%, and the number of friction pilling reached 98.87%. It had good antistatic performance before and after washing, and various performance parameters were better than those of the comparative example. This shows that the present invention uses a modified quaternary ammonium salt as a cross-linking agent to promote the crosslinking of a polyurethane prepolymer co-blocked with modified polysiloxane and polyethylene glycol to prepare an epoxy-terminated modified polyurethane, and disperses and mixes the modified polyurethane with tetrabutyl titanate in an alkaline emulsion to perform padding modification on the pretreated grey cloth, thereby effectively improving not only the windproof and moisture permeability of the composite fabric, but also its antistatic performance and wear resistance and anti-pilling performance.

[0136] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to specific embodiments. Obviously, many modifications and variations are possible based on the contents of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A windproof and breathable composite fabric, characterized in that: The windproof and breathable composite fabric is obtained by processing the following steps: S1, placing a blank in a pretreatment solution, and adding a 3-aminopropyltriethoxysilane solution dropwise to the pretreatment solution for pretreatment to obtain a pretreated grey cloth, wherein the grey cloth is a polyester fiber cloth; S2. Under inert gas protection, polyethylene glycol, hydroxyl-terminated polysiloxane, a catalyst and butanone are mixed, the reaction system temperature is raised to 70-78° C., isophorone diisocyanate is added to the reaction system, and the reaction is kept warm for 90-120 min to obtain a polyurethane prepolymer, a modified quaternary ammonium salt is added to the reaction system, and the reaction is kept warm for 70-90 min, 2-(oxirane-2-yl)ethanol-1-ol is added to the reaction system, and the reaction is kept warm for 60-80 min, and post-processed to obtain a modified polyurethane; S3, mixing the modified polyurethane, tetrabutyl titanate and the emulsion containing sodium carbonate, and emulsifying at high speed for 60-80 minutes to obtain a finishing solution; S4, immersing the pretreated grey fabric in a finishing solution, and performing two-immersion and two-rolling finishing to obtain a composite fabric; The preparation method of hydroxyl-terminated polysiloxane comprises: mixing octamethylcyclotetrasiloxane, modified pyrimidine and xylene, adding a catalyst to the reaction system, raising the temperature of the reaction system to 105-115° C., keeping the temperature for reaction for 3-4 hours, adding 1,3-bis(3-hydroxypropyl)-1,1,3,3-tetramethyldisiloxane to the reaction system, keeping the temperature for reaction for 4-6 hours, and post-treating to obtain hydroxyl-terminated polysiloxane; The preparation method of the modified pyrimidine comprises: mixing 4-amino-2,6-dichloropyrimidine and tetrahydrofuran under inert gas protection, raising the temperature of the reaction system to 50-60°C, adding 3-isocyanatopropylmethyldiethoxysilane to the reaction system, keeping the temperature for reaction for 60-90 minutes, and post-treating to obtain the modified pyrimidine; The preparation method of the modified quaternary ammonium salt is as follows: under the protection of inert gas, 1,4-dichlorobenzyl, triethanolamine and tetrahydrofuran are mixed, the temperature of the reaction system is increased to the system reflux, the reaction is kept warm for 6-8 hours, and post-processed to obtain the modified quaternary ammonium salt.

2. The windproof and breathable composite fabric according to claim 1, characterized in that: In step S1, the pretreatment method is: adding the grey cloth to a pretreatment solution with a temperature of 60-70°C, ultrasonically dispersing for 30-50 minutes, and adding 3-aminopropyltriethoxysilane solution to the pretreatment solution under ultrasonic dispersion. After the addition is completed, heat preservation treatment is performed for 60-80 minutes, and post-treatment is performed to obtain the pretreated grey cloth.

3. The windproof and breathable composite fabric according to claim 2, characterized in that: The amount ratio of the grey cloth, pretreatment solution and 3-aminopropyltriethoxysilane solution is 5g:70mL:5g, the pretreatment solution is composed of sodium hydroxide, purified water, sodium lauryl sulfate and 30wt% hydrogen peroxide in the ratio of 8-10g:100mL:3g:15-20mL, and the 3-aminopropyltriethoxysilane solution is composed of 3-aminopropyltriethoxysilane and anhydrous ethanol in the ratio of 1g:3mL.

4. The windproof and breathable composite fabric according to claim 1, characterized in that: In step S2, the amount ratio of the polyethylene glycol, hydroxyl-terminated polysiloxane, catalyst and butanone is 10g:3g:0.1g:30mL, in the preparation process of the polyurethane prepolymer, the molar ratio of the hydroxyl group to the isocyanate group is 1:1.1, the catalyst is dibutyltin dilaurate, and the weight ratio of the polyethylene glycol, modified quaternary ammonium salt and 2-(oxirane-2-yl)ethanol-1-ol is 10:1.2-1.5:4; in step S3, the amount ratio of the modified polyurethane, tetrabutyl titanate and emulsion is 10-20g:0.8-1.2g:40-60mL, and the emulsion is composed of deionized water, hexadecyltrimethylammonium chloride, emulsifier AEO-4, Tween-80 and sodium carbonate in a ratio of 100mL:2g:1g:1g:15g.

5. The windproof and breathable composite fabric according to claim 1, characterized in that: The usage ratio of the octamethylcyclotetrasiloxane, modified pyrimidine, xylene, catalyst and 1,3-bis(3-hydroxypropyl)-1,1,3,3-tetramethyldisiloxane is 7g:2g:50mL:5mL:1g, and the catalyst is a 10wt% formic acid aqueous solution.

6. The windproof and breathable composite fabric according to claim 1, characterized in that: The usage ratio of the 4-amino-2,6-dichloropyrimidine and 3-isocyanatepropylmethyldiethoxysilane is 1 mol:1 mol, and the usage ratio of the 4-amino-2,6-dichloropyrimidine and tetrahydrofuran is 1 g:7 mL.

7. The windproof and breathable composite fabric according to claim 1, characterized in that: The usage ratio of the 1,4-dichlorobenzyl and triethanolamine is 1 mol:2 mol.

8. An application of a windproof and breathable composite fabric, characterized in that: The windproof and breathable composite fabric according to any one of claims 1 to 7 is used in clothing processing.

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