Wear-resistant light thermal fabric and preparation method thereof

Abstract

The invention discloses a wear-resistant light warm-keeping fabric and a preparation method thereof, belongs to the technical field of fabric processing, and aims to solve the technical problem that wear resistance and light weight of a warm-keeping fabric in the prior art need to be further improved. The preparation method comprises the following steps: spinning modified acrylic fibers to obtain a light wear-resistant fabric; after a wool modified material is prepared and activated, wool fibers are modified to overcome the defects of poor wear resistance, poor high temperature resistance and the like, and carbon-carbon double bonds are introduced to the surfaces of the wool fibers, so that the modified wool fibers are used as a skeleton to hybridize an organic chain segment structure in the synthesis process of composite polyacrylonitrile, and the mechanical property of the composite polyacrylonitrile is improved; the process of electrostatic spinning is promoted through the electrical conductivity of the wool modified material, finally, the hollow acrylic fibers of a hollow porous structure are prepared, and the light wear-resistant fabric is obtained through spinning.

Description

Technical Field

[0001] The invention relates to the technical field of fabric processing, and in particular to a wear-resistant, lightweight, warm-keeping fabric and a preparation method thereof. Background Art

[0002] The progress of lightweight, wear-resistant and warm fabrics is reflected in the development of the fabric field. Although traditional thermal insulation materials are warm, they are heavy and not durable enough. With the gradual development of technology, the use of synthetic materials such as polyester and nylon, coupled with the integration of nanotechnology and microporous technology, modern fabrics have become light and tough, with excellent thermal insulation performance. These materials are particularly critical in outdoor sports equipment. They can adapt to extreme climates while maintaining breathability and moisture management, greatly improving service life and wearing comfort. This versatility of the fabric ensures warmth in low temperature environments while coping with the heat and moisture generated by activities, making it an outstanding achievement of modern textile technology.

[0003] Prior art CN103774440A discloses a lightweight, elastic, wear-resistant nylon fabric, comprising a base fabric layer and at least one coating layer, wherein the base fabric layer is a nylon fabric interwoven with warp yarns and weft yarns, with a warp elastic elongation of 16-30%, a weft elastic elongation of 15-32%, and a warp and weft elastic recovery rate of more than 95%. A coating layer is coated on the base fabric layer, and the coating slurry is composed of the following components in parts by mass: 45-65 parts of polyurethane modified polyester resin, 15-30 parts of polyurethane resin, 6-10 parts of silane coupling agent, 7-15 parts of cross-linking agent, 5-8 parts of titanium dioxide and 12-18 parts of toluene; the lightweight, elastic, wear-resistant nylon fabric provided by the above patent content is light, dense, smooth, elastic, and has excellent wear resistance after coating treatment, and is very suitable as a lightweight outdoor product with certain requirements for elasticity and wear resistance.

[0004] However, the above patent content is to achieve the purpose of improving the wear resistance of the material by combining the base fabric layer and the coating by using isocyanate cross-linking agents. However, this solution lacks performance improvement treatment of the nylon fiber used, such as improving its structure to enhance its lightness, improving its process components to enhance its wear resistance, etc., resulting in the lightness and wear resistance of the material to be further improved, and the activity of isocyanate cross-linking agents is too high, and they are easily deactivated during the cross-linking process, so that the bonding strength between the base fabric layer and the coating needs to be further improved, and the wear resistance of the material is significantly improved.

[0005] In view of the technical defects in this aspect, a solution is now proposed. Summary of the invention

[0006] The object of the present invention is to provide a wear-resistant and lightweight thermal insulation fabric and a preparation method thereof, so as to solve the technical problem in the prior art that the wear resistance and lightness of the thermal insulation fabric need to be further improved.

[0007] The purpose of the present invention can be achieved by the following technical scheme: A method for preparing a wear-resistant, lightweight, warm-keeping fabric comprises the following steps:

[0008] S1, adding modified wool fiber, acrylonitrile and N,N-dimethylformamide into a reactor, raising the temperature of the reactor to 60-80°C, adding azobisisobutyronitrile into the reactor, keeping the temperature for 2-4h, and post-treating to obtain composite polyacrylonitrile;

[0009] The reaction equation for preparing composite polyacrylonitrile is:

[0010]

[0011] Where: It indicates modified wool fiber, and “*” indicates the active connection site of organic chain segment.

[0012] The reaction principle for preparing composite polyacrylonitrile is: under the catalysis of azobisisobutyronitrile and heating conditions, the double bonds on the surface of the modified wool fiber and the double bonds of acrylonitrile undergo polymerization reaction, and finally the composite polyacrylonitrile is prepared.

[0013] S2, adding composite polyacrylonitrile, polyvinyl pyrrolidone, antibacterial agent, reinforcing agent, plasticizer, crosslinking agent and N,N-dimethylformamide into a reaction kettle, stirring at room temperature for 10-15 minutes, and obtaining a spinning solution 1;

[0014] S3, using the spinning solution 1 and the spinning solution 2 to electrospin to obtain a hollow acrylic fiber;

[0015] S4. Use modified acrylic fiber to weave lightweight and wear-resistant fabrics.

[0016] Further, in step S1, the stirring rate of the reactor is 80-120rpm, the amount ratio of the modified wool fiber, acrylonitrile, N,N-dimethylformamide and azobisisobutyronitrile is 5-6g:8-10g:60-80mL:1-2g, and the post-treatment is as follows: after the reaction is completed, the reactor is cooled to room temperature, the reaction liquid is added to a rotary evaporator with a water bath temperature of 80-100°C, and the reduced pressure distillation is performed until no liquid is extracted to obtain a composite polypropylene Olefin nitrile; in step S2, the stirring rate of the reactor is 80-120rpm, and the dosage ratio of composite polyacrylonitrile, polyvinyl pyrrolidone, antibacterial agent, reinforcing agent, plasticizer, cross-linking agent and N,N-dimethylformamide is 12-15g:1-2g:0.5-0.8g:0.5-0.8g:0.5-0.8g:0.3-0.5g:70-80mL; in step S3, the spinning solution 2 is 40-60v% isopropanol aqueous solution.

[0017] Furthermore, the antibacterial agent is one or more of benzalkonium chloride, polyhexamethyleneguanidine and tetradecyltrimethylammonium chloride; the reinforcing agent is one or more of nano-silica, carbon fiber and nano-alumina; the plasticizer is one or more of dibutyl phthalate, triethyl citrate and dioctyl adipate; the cross-linking agent is one or more of hexamethylene diisocyanate, glycidyl methacrylate and melamine formaldehyde resin.

[0018] Further, in step S3, the electrospinning operation includes the following steps:

[0019] A1. Add the spinning solution 1 to the discharge kettle of the electrospinning machine, add the spinning solution 2 to the core solution kettle of the electrospinning machine, and after nitrogen protection is introduced into the instrument, set the voltage of the electrospinning machine to 20-30 kV, the flow rate of the discharge kettle to 1-3 mL / min, and the flow rate of the spinning solution 2 to 1-4 mL / min, so that the spinning solution is slowly extruded from the spinneret to form a hollow thin flow. After being exposed to the air for 10-15 minutes, the hollow thin flow vertically enters an external coagulation water bath with a temperature of 20-40° C. to coagulate to obtain a hollow acrylic fiber blank;

[0020] A2. The hollow acrylic fiber blank is transferred to an ultrasonic device, the temperature of the ultrasonic device is set to 40-60°C, the ultrasonic frequency is 40-60kHz, and after heat preservation and ultrasonication for 1-2 hours, the hollow acrylic fiber blank is transferred to a drying oven at a temperature of 60-80°C and vacuum dried to constant weight to obtain a hollow acrylic fiber.

[0021] The reaction principle for preparing hollow acrylic fibers is as follows: the spinning solution and pore-forming agent in electrospinning gradually dissolve during the ultrasonic process, and eventually the fibers form a hollow porous structure.

[0022] Further, in step S4, the weaving operation is: selecting 75-100D hollow acrylic fiber, the number of monofilaments is 36-48F, setting the twist of the yarn to 300-500 twists / m, the twist direction is Z twist, and after the twisting is completed, heat setting is performed at a temperature of 60-80°C, and winding is performed at a speed of 500-600m / min to obtain the yarn, and the yarns are used as warp yarns and weft yarns respectively, and the lightweight wear-resistant fabric is woven; the imperial count of the warp yarn is 30-40s, the imperial count of the weft yarn is 35-45s, and the density of the lightweight wear-resistant fabric is 120-160 warp yarns and 90-120 weft yarns per square inch.

[0023] Furthermore, the preparation method of the modified wool fiber comprises the following steps:

[0024] B1. Add the wool modified material, dicyclohexylcarbodiimide and dichloromethane into a reactor, stir at room temperature for 30-40 minutes, add glutathione into the reactor, continue stirring for 4-6 hours, and post-treat to obtain an activated filler;

[0025] The reaction equation for preparing activated filler is:

[0026]

[0027] Where: , “*” indicates the active connection site of the organic chain segment.

[0028] The reaction principle for preparing the activated filler is: under the promotion of the dehydrating agent dicyclohexylcarbodiimide, the core structure of the wool modified material activates the carboxyl group on the surface of the multilayer graphene and the thiol group of glutathione to undergo a dehydration reaction, and finally the activated filler is prepared.

[0029] B2. Add the pre-treated wool fiber, activated filler and deionized water into an ultrasonic instrument, perform ultrasonic treatment for 1-2 hours, and perform post-treatment to obtain modified wool fiber.

[0030] The reaction principle for preparing modified wool fibers is as follows: under the promotion of ultrasound and heating, the active functional group carboxyl on the surface of the pre-treated wool fibers reacts with the amino group on the surface of the activated filler to eventually form a stable cross-linked structure to obtain modified wool fibers.

[0031] Furthermore, in step B1, the usage ratio of wool modified material, dicyclohexylcarbodiimide, dichloromethane and glutathione is 8-10g:1-2g:30-40mL:4-5g, and the post-treatment is: after the reaction is completed, the reaction liquid is filtered to collect the filter cake, and the filter cake is washed 3-5 times with anhydrous ethanol and deionized water, and then the filter cake is placed in a drying oven at a temperature of 40-60°C and vacuum dried until the filter cake has a constant weight to obtain an activated filler.

[0032] Furthermore, in step B2, the amount ratio of the pre-treated wool fiber, the activated filler and the deionized water is 5-6g:2-3g:30-40mL, the power of the ultrasonic instrument is 80-90W, the temperature is 70-90°C, and the frequency is 40-60kHz. The pre-treatment operation is: the wool fiber is transferred to a sodium carbonate solution with a concentration of 0.06-0.08mol / L for ultrasonication, the bath ratio is 1:80-100, and the ultrasonic frequency is 20-40khz. After the ultrasonication is completed, the wool fiber is washed with deionized water for 3-5 times, and then transferred to a drying oven at a temperature of 60°C and dried to constant weight to obtain the pre-treated wool fiber; the post-treatment is: after the reaction is completed, the reaction liquid is filtered to collect the filter cake, the filter cake is washed with anhydrous ethanol and deionized water for 3-5 times, and then the filter cake is placed in a drying oven at a temperature of 40-60°C and vacuum dried to a constant weight to obtain the modified wool fiber.

[0033] Furthermore, the preparation method of the wool modified material comprises the following steps:

[0034] C1. Add multilayer graphene and ethanol to a reactor and stir. After stirring at room temperature for 15-20 minutes, pour the mixed acid solution into the reactor and raise the temperature of the reactor to 40-60° C. After acidification for 0.5 hours, add potassium permanganate to the reactor and stir at this temperature for 8-12 hours. After post-treatment, obtain activated multilayer graphene.

[0035] C2. Add activated multilayer graphene, butyl titanate, 3-(triethoxysilyl)propyl methacrylate and anhydrous ethanol into a reactor and stir. After stirring at room temperature for 15-20 minutes, continue to drop deionized water and polyvinyl pyrrolidone. After the temperature of the reactor is increased to 40-60°C, use 1-1.5 mol / L ammonia solution to adjust the pH of the system to 8-9, keep warm for 24-36 hours to obtain a composite gel, and then post-treat to obtain a wool modified material.

[0036] The reaction principle for preparing the wool modified material is as follows: after being promoted by an acidified liquid, the oxidizability of potassium permanganate is significantly improved, thereby oxidizing multilayer graphene so that a large number of active functional groups appear on its surface and between its hierarchical structures to obtain activated multilayer graphene; butyl titanate and 3-(triethoxysilyl)propyl methacrylate are hydrolyzed under the catalysis of alkaline conditions to form a cross-linked network on the surface of the activated multilayer graphene, and a composite gel is obtained after aging; after ultrasonic removal of the pore-forming agent and drying and evaporation of the solvent, a complex pore structure of the material appears; and the active functional groups between the hierarchical structures of the activated multilayer graphene are exposed by grinding to obtain the wool modified material.

[0037] Further, in step C1, the stirring rate of the reactor is 80-120rpm, the amount ratio of multilayer graphene, ethanol, acidified solution and oxidant is 5-8g:18-24mL:10-12mL:3-5g, the acidified solution is 98.0wt% concentrated sulfuric acid and 30-40wt% nitric acid mixed in a volume ratio of 3:1, and the post-treatment includes: after the reaction is completed, the reaction liquid is filtered to collect the filter cake, the filter cake is washed 3-5 times with anhydrous ethanol and deionized water, and the filter cake is placed in a drying oven at a temperature of 40-60°C and vacuum dried until the filter cake has a constant weight to obtain activated multilayer graphene; in step C2, the stirring rate of the reactor is 6 0-80rpm, the amount ratio of activated multilayer graphene, butyl titanate, 3-(triethoxysilyl)propyl methacrylate, anhydrous ethanol, deionized water and polyvinyl pyrrolidone is 1-2g:3-6g:0.3-0.5g:30-40mL:10-20mL:0.1-0.2g, and the post-treatment includes: after the reaction is completed, the reaction liquid is filtered to collect the filter cake, the filter cake deionized water is placed in an ultrasonic instrument at a temperature of 40°C for 2h, and the ultrasonic frequency is 40kHz. After the ultrasonication is completed, the porous material is filtered to obtain the porous material, and the porous material is vacuum dried to constant weight, and ground through a 400-600 mesh sieve to obtain a wool modified material.

[0038] The invention also provides a wear-resistant, lightweight, warm-keeping fabric, which is obtained by adopting a preparation method of the wear-resistant, lightweight, warm-keeping fabric.

[0039] The present invention has the following beneficial effects:

[0040] 1. The present invention prepares a wool modified material and activates it, then modifies the wool fiber to overcome its defects such as poor wear resistance and high temperature resistance, and introduces carbon-carbon double bonds on its surface, so that the modified wool fiber serves as a skeleton hybrid organic segment structure in the process of composite polyacrylonitrile synthesis, thereby improving the mechanical properties of the composite polyacrylonitrile, and utilizing the conductivity of the wool modified material to promote the electrostatic spinning process, introducing a pore-forming agent and a spinning solution in the process of spinning pore formation to form a stable porous hollow structure of the material, and finally preparing a hollow acrylic fiber with a hollow porous structure, and weaving a lightweight wear-resistant fabric.

[0041] 2. The present invention prepares titanium dioxide particles with activated multilayer graphene as the core and double bonds on the surface as wool modification material, and after the surface is activated by glutathione, the active functional group amino on the surface combines with the pre-treated wool fiber to obtain modified wool fiber, and the double bonds on the wool modification material are used as cross-linking groups to continuously polymerize acrylonitrile with the modified wool fiber as the matrix to obtain composite polyacrylonitrile, so that the polyacrylonitrile segment produces a complex spatial segment structure, and the wool fiber is used as a skeleton to significantly enhance the wear resistance and elongation at break of the material; highly conductive titanium dioxide is introduced as the shell structure of the activated multilayer graphene and carbon-carbon double bonds are introduced in the process of forming the shell structure, the former produces a stable electric field effect in the electrostatic spinning process, promotes the spinning solution to be more delicate and uniform, and the carbon-carbon double bonds enable the composite polyacrylonitrile to form a more stable structure with the modified wool fiber during the synthesis process, thereby forming a network structure in the fiber, which is helpful to disperse stress and increase the overall durability of the fiber, and finally significantly enhances the wear resistance and tensile strength of the material.

[0042] 3. The present invention introduces pore-forming agents and spinning liquid during the spinning pore-forming process to form a stable porous hollow structure of the material. The air layer contained in the hollow fiber has a very low thermal conductivity, which effectively isolates the external cold air and the heat loss in the body. The porous structure of the fiber provides an additional insulation layer, thereby further improving the warmth retention performance. The porous structure not only insulates, but also allows air circulation, which helps to discharge moisture from the body. When the human body sweats, moisture will escape through these tiny pores. The hollow fiber can absorb and conduct moisture through capillary action, and migrate from the skin surface to the outside of the fiber. This moisture transmission effect from wet to dry further enhances the moisture permeability of the fabric. DETAILED DESCRIPTION

[0043] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0044] The multilayer graphene used in the present invention is purchased from Chengdu Jiacai Technology Co., Ltd., and the product number is JCMRGO.

[0045] Example 1

[0046] This embodiment provides a method for preparing a wear-resistant, lightweight, warm-keeping fabric, comprising the following steps:

[0047] Step 1: Preparation of wool modified material

[0048] Weigh: 300.0L 98.0wt% concentrated sulfuric acid and 100.0mL 30wt% nitric acid and mix to obtain an acidified solution;

[0049] Weigh: 500.0g of multilayer graphene and 1.8L of ethanol are added to a reactor and stirred at a stirring rate of 80rpm. After stirring at room temperature for 15min, 1.0L of mixed acid solution is poured into the reactor, and the temperature of the reactor is raised to 40°C. After acidification for 0.5h, 300.0g of potassium permanganate is added to the reactor, and the mixture is stirred at this temperature for 8h. After the reaction is completed, the reaction solution is filtered to collect the filter cake. After washing the filter cake 3 times with anhydrous ethanol and deionized water, the filter cake is placed in a drying oven at a temperature of 40°C and vacuum dried until the filter cake has a constant weight, thereby obtaining activated multilayer graphene;

[0050] Weigh: 100.0g activated multilayer graphene, 300.0g butyl titanate, 30.0g 3-(triethoxysilyl)propyl methacrylate and 3.0L anhydrous ethanol, add into the reactor and stir, stir at room temperature for 15min, then continue to drop 1.0L deionized water and 10.0g polyvinyl pyrrolidone, after the temperature of the reactor rises to 40°C, use 1.0mol / L ammonia solution to adjust the pH of the system to 8, keep warm for 24h to obtain a composite gel, after the reaction is completed, filter the reaction liquid to collect the filter cake, place the filter cake deionized water in an ultrasonic instrument at a temperature of 40°C for 2h, and the ultrasonic frequency is 40kHz. After the ultrasonication is completed, filter to obtain a porous material, vacuum dry the porous material to constant weight, and grind it through a 400-mesh sieve to obtain a wool modified material.

[0051] Step 2: Preparation of modified wool fiber

[0052] Weigh: 800.0g wool modified material, 100.0g dicyclohexylcarbodiimide and 3.0L dichloromethane are added to the reactor, stirred at room temperature for 30min, and then 400.0g glutathione is added to the reactor, and stirring is continued for 4h. After the reaction is completed, the reaction liquid is filtered to collect the filter cake, and the filter cake is washed with anhydrous ethanol and deionized water for 3 times, and then placed in a drying oven at a temperature of 40°C and vacuum dried until the filter cake has a constant weight to obtain an activated filler;

[0053] Weigh: 100.0 g of wool fiber was transferred to a 0.06 mol / L sodium carbonate solution for ultrasonic treatment, with a bath ratio of 1:80 and an ultrasonic frequency of 20 khz. After the ultrasonic treatment, the wool fiber was washed with deionized water for 3 times, and then transferred to a drying oven at a temperature of 60° C. and dried to constant weight to obtain pre-treated wool fiber;

[0054] Weigh: 500.0g pre-treated wool fiber, 200.0g activated filler and 3.0L deionized water and add them into an ultrasonic instrument. The power of the ultrasonic instrument is 80W, the temperature is 70℃, the frequency is 40kHz, and the ultrasonic treatment is performed for 1h. After the reaction is completed, the reaction liquid is filtered to collect the filter cake. After washing the filter cake with anhydrous ethanol and deionized water for 3 times, the filter cake is placed in a drying oven at a temperature of 40℃ and vacuum dried until the filter cake has a constant weight to obtain modified wool fiber.

[0055] Step 3: Preparation of Spinning Solution 1

[0056] Weigh: 500.0g modified wool fiber, 800.0g acrylonitrile and 6.0L N, N-dimethylformamide and add them into a reactor, stir at a rate of 80rpm, after the temperature of the reactor is raised to 60°C, add 100.0g azobisisobutyronitrile into the reactor, keep warm for 2h, after the reaction is completed, cool the reactor to room temperature, add the reaction liquid into a rotary evaporator with a water bath temperature of 80°C, and distill under reduced pressure until no liquid is produced to obtain composite polyacrylonitrile;

[0057] Weigh: 1.2 kg of composite polyacrylonitrile, 100.0 g of polyvinyl pyrrolidone, 50.0 g of benzalkonium chloride, 50.0 g of nano-silicon dioxide, 50.0 g of triethyl citrate, 50.0 g of hexamethylene diisocyanate and 7.0 L of N,N-dimethylformamide, add into a reaction kettle, stir at room temperature for 10 min, and obtain spinning solution 1.

[0058] Step 4: Preparation of hollow polyester fibers

[0059] Weigh: 10.0L spinning solution 1 is added to the discharge kettle of the electrospinning machine, 10.0L 40v% isopropanol aqueous solution is added to the core liquid kettle of the electrospinning machine, after nitrogen protection is introduced into the instrument, the voltage of the electrospinning machine is set to 20kV, the flow rate of the discharge kettle is 1.0L / h, and the flow rate of the spinning solution 2 is 1.0L / h, so that the spinning solution is slowly squeezed out from the spinneret to form a hollow thin flow, after being exposed to the air for 10min, the hollow thin flow vertically enters an external coagulation water bath at a temperature of 20°C, and coagulates to obtain a hollow acrylic fiber blank;

[0060] The hollow acrylic fiber blank was transferred to an ultrasonic device, the temperature of the ultrasonic instrument was set to 40°C, the ultrasonic frequency was 40kHz, and the temperature was kept for ultrasonication for 1 hour. The hollow acrylic fiber blank was transferred to a drying oven at a temperature of 60°C and vacuum dried to constant weight to obtain a hollow acrylic fiber.

[0061] Step 5: Prepare lightweight and wear-resistant fabrics

[0062] 75D hollow acrylic fiber is selected, the number of monofilaments is 36F, the twist of the yarn is set to 300 twists / m, the twist direction is Z twist, and after the twisting is completed, it is heat-set at a temperature of 60°C and wound at a speed of 500m / min to obtain the yarn. The yarns are used as warp yarn and weft yarn respectively, and the lightweight wear-resistant fabric is woven; the imperial count of the warp yarn is 30s, and the imperial count of the weft yarn is 35s. The density of the lightweight wear-resistant fabric is 120 warp yarns and 90 weft yarns per square inch.

[0063] Example 2

[0064] This embodiment provides a method for preparing a wear-resistant, lightweight, warm-keeping fabric, comprising the following steps:

[0065] Step 1: Preparation of wool modified material

[0066] Weigh: 300.0 mL 98.0 wt % concentrated sulfuric acid and 100.0 mL 40 wt % nitric acid and mix to obtain an acidified solution;

[0067] Weigh: 800.0g of multilayer graphene and 2.4L of ethanol are added to a reactor and stirred at a stirring rate of 120rpm. After stirring at room temperature for 20min, 1.2L of mixed acid solution is poured into the reactor, and the temperature of the reactor is raised to 60°C. After acidification for 0.5h, 500.0g of potassium permanganate is added to the reactor, and the mixture is stirred at this temperature for 12h. After the reaction is completed, the reaction solution is filtered to collect the filter cake. After the filter cake is washed 5 times with anhydrous ethanol and deionized water, the filter cake is placed in a drying oven at a temperature of 60°C and vacuum dried until the filter cake has a constant weight, thereby obtaining activated multilayer graphene;

[0068] Weigh: 200.0g activated multilayer graphene, 600.0g butyl titanate, 50.0g 3-(triethoxysilyl)propyl methacrylate and 4.0L anhydrous ethanol, add into the reactor and stir, stir at room temperature for 20min, then continue to add 2.0L deionized water and 20.0g polyvinyl pyrrolidone, after the temperature of the reactor rises to 60°C, use 1.5mol / L ammonia solution to adjust the pH of the system to 9, keep warm for 36h to obtain a composite gel; after the reaction is completed, filter the reaction liquid to collect the filter cake, place the filter cake deionized water in an ultrasonic instrument at a temperature of 40°C for 2h, and the ultrasonic frequency is 40kHz. After the ultrasonication is completed, filter to obtain a porous material, vacuum dry the porous material to constant weight, and grind it through a 600-mesh sieve to obtain a wool modified material.

[0069] Step 2: Preparation of modified wool fiber

[0070] Weigh: 1000.0g wool modified material, 200.0g dicyclohexylcarbodiimide and 4.0L dichloromethane are added to the reactor, stirred at room temperature for 40min, and then 500.0g glutathione is added to the reactor, and stirring is continued for 6h. After the reaction is completed, the reaction liquid is filtered to collect the filter cake, and the filter cake is washed with anhydrous ethanol and deionized water for 5 times, and then placed in a drying oven at a temperature of 60°C and vacuum dried until the filter cake has a constant weight to obtain an activated filler;

[0071] Weigh: 100.0 g wool fiber is transferred to a 0.08 mol / L sodium carbonate solution for ultrasonic treatment, the bath ratio is 1:100, the ultrasonic frequency is 40 khz, after the ultrasonic treatment, it is washed with deionized water for 5 times, and then transferred to a drying oven at a temperature of 60°C and dried to constant weight to obtain pre-treated wool fiber;

[0072] Weigh: 600.0g of pretreated wool fiber, 300.0g of activated filler and 4.0L of deionized water and add them into an ultrasonic instrument. The power of the ultrasonic instrument is 90W, the temperature is 90℃, the frequency is 60kHz, and the ultrasonic treatment is carried out for 2h. After the reaction is completed, the reaction liquid is filtered to collect the filter cake. After washing the filter cake with anhydrous ethanol and deionized water for 5 times, the filter cake is placed in a drying oven at a temperature of 60℃ and vacuum dried until the filter cake has constant weight to obtain modified wool fiber.

[0073] Step 3: Preparation of Spinning Solution 1

[0074] Weigh: 600.0g modified wool fiber, 1000.0g acrylonitrile and 8.0L N, N-dimethylformamide are added to a reactor with a stirring rate of 120rpm. After the temperature of the reactor is raised to 80°C, 200.0g azobisisobutyronitrile is added to the reactor and the reaction is carried out for 4h. After the reaction is completed, the reactor is cooled to room temperature and the reaction liquid is added to a rotary evaporator with a water bath temperature of 100°C, and the mixture is distilled under reduced pressure until no liquid is produced to obtain composite polyacrylonitrile;

[0075] Weigh: 1.5 kg of composite polyacrylonitrile, 200.0 g of polyvinyl pyrrolidone, 80.0 g of benzalkonium chloride, 80.0 g of nano-silicon dioxide, 80.0 g of triethyl citrate, 80.0 g of hexamethylene diisocyanate and 8.0 L of N,N-dimethylformamide, add into a reaction kettle, stir at room temperature for 15 min, and obtain spinning solution 1.

[0076] Step 4: Preparation of hollow polyester fibers

[0077] Weigh: 10.0L spinning solution 1 is added to the discharge kettle of the electrospinning machine, 20.0L 60v% isopropanol aqueous solution is added to the core liquid kettle of the electrospinning machine, after nitrogen protection is introduced into the instrument, the voltage of the electrospinning machine is set to 30kV, the flow rate of the discharge kettle is 2.0L / h, and the flow rate of the spinning solution 2 is 4.0L / h, so that the spinning solution is slowly squeezed out from the spinneret to form a hollow thin flow, after being exposed to the air for 15min, the hollow thin flow vertically enters an external coagulation water bath at a temperature of 40°C, and coagulates to obtain a hollow acrylic fiber blank;

[0078] The hollow acrylic fiber blank was transferred to an ultrasonic device, the temperature of the ultrasonic instrument was set to 60°C, the ultrasonic frequency was 60kHz, and the temperature was kept for 2 hours. The hollow acrylic fiber blank was transferred to a drying oven at a temperature of 80°C and vacuum dried to constant weight to obtain a hollow acrylic fiber.

[0079] Step 5: Prepare lightweight and wear-resistant fabrics

[0080] 100D hollow acrylic fiber is selected, the number of monofilaments is 48F, the twist of the yarn is set to 500 twists / m, the twist direction is Z twist, and after the twisting is completed, it is heat-set at a temperature of 80°C and wound at a speed of 6600m / min to obtain the yarn. The yarns are used as warp yarn and weft yarn respectively, and the lightweight wear-resistant fabric is woven; the imperial count of the warp yarn is 40s, and the imperial count of the weft yarn is 45s. The density of the lightweight wear-resistant fabric is 160 warp yarns and 120 weft yarns per square inch.

[0081] Example 3

[0082] This embodiment provides a method for preparing a wear-resistant, lightweight, warm-keeping fabric, comprising the following steps:

[0083] Step 1: Preparation of wool modified material

[0084] Weigh: 300.0 mL 98.0 wt % concentrated sulfuric acid and 100.0 mL 40.0 wt % nitric acid and mix to obtain an acidified solution;

[0085] Weigh: 650.0g of multilayer graphene and 2.1L of ethanol are added to a reactor and stirred at a stirring rate of 100rpm. After stirring at room temperature for 18min, 1.0L of mixed acid solution is poured into the reactor, and the temperature of the reactor is raised to 60°C. After acidification for 0.5h, 400.0g of potassium permanganate is added to the reactor, and the reaction mixture is stirred for 10h. After the reaction is completed, the reaction liquid is filtered to collect the filter cake. After washing the filter cake 4 times with anhydrous ethanol and deionized water, the filter cake is placed in a drying oven at a temperature of 50°C and vacuum dried until the filter cake has a constant weight to obtain activated multilayer graphene;

[0086] Weigh: 200.0g activated multilayer graphene, 600.0g butyl titanate, 50.0g 3-(triethoxysilyl)propyl methacrylate and 3.5L anhydrous ethanol, add into the reactor and stir, stir at room temperature for 18min, then continue to drop 1.5L deionized water and 15.0g polyvinyl pyrrolidone, after the temperature of the reactor rises to 50°C, use 1.2mol / L ammonia solution to adjust the pH of the system to 9, keep warm for 30h, obtain composite gel, after the reaction is completed, filter the reaction liquid to collect the filter cake, place the filter cake deionized water in an ultrasonic instrument at a temperature of 40°C for 2h, and the ultrasonic frequency is 40kHz. After the ultrasonication is completed, filter to obtain the porous material, vacuum dry the porous material to constant weight, and grind it through a 500-mesh sieve to obtain the wool modified material.

[0087] Step 2: Preparation of modified wool fiber

[0088] Weigh: 900.0g wool modified material, 150.0g dicyclohexylcarbodiimide and 3.5L dichloromethane are added to the reactor, stirred at room temperature for 36 minutes, and then 450.0g glutathione is added to the reactor, and stirring is continued for 5 hours. After the reaction is completed, the reaction liquid is filtered to collect the filter cake, and the filter cake is washed with anhydrous ethanol and deionized water for 4 times, and then placed in a drying oven at a temperature of 50°C and vacuum dried until the filter cake has a constant weight to obtain an activated filler;

[0089] Weigh: transfer the wool fiber to a 0.07 mol / L sodium carbonate solution for ultrasonic treatment, with a bath ratio of 1:90 and an ultrasonic frequency of 30 khz. After the ultrasonic treatment, wash the wool fiber with deionized water for 4 times, transfer the fiber to a drying oven at 60°C and dry the dried fiber to a constant weight to obtain the pre-treated wool fiber.

[0090] Weigh: 550.0g pre-treated wool fiber, 240.0g activated filler and 3.5L deionized water and add them into the ultrasonic instrument. The power of the ultrasonic instrument is 84W, the temperature is 80℃, the frequency is 50kHz, and the ultrasonic treatment is carried out for 2h. After the reaction is completed, the reaction liquid is filtered to collect the filter cake. After washing the filter cake with anhydrous ethanol and deionized water for 4 times, the filter cake is placed in a drying oven at a temperature of 50℃ and vacuum dried until the filter cake has constant weight to obtain modified wool fiber.

[0091] Step 3: Preparation of Spinning Solution 1

[0092] Weigh: 550.0g modified wool fiber, 900.0g acrylonitrile and 7.0L N, N-dimethylformamide and add them into a reactor, stir at a rate of 100rpm, after the temperature of the reactor is raised to 70°C, add 150.0g azobisisobutyronitrile into the reactor, keep warm for 3h, after the reaction is completed, cool the reactor to room temperature, add the reaction liquid into a rotary evaporator with a water bath temperature of 90°C, and distill under reduced pressure until no liquid is produced to obtain composite polyacrylonitrile;

[0093] Weigh: 1.5 kg of composite polyacrylonitrile, 150.0 g of polyvinyl pyrrolidone, 60.0 g of benzalkonium chloride, 60.0 g of nano-silicon dioxide, 60.0 g of triethyl citrate, 60.0 g of hexamethylene diisocyanate and 7.2 L of N,N-dimethylformamide, add into a reaction kettle, stir at room temperature for 12 min, and obtain spinning solution 1.

[0094] Step 4: Preparation of hollow polyester fibers

[0095] Weigh: 20.0L spinning solution 1 is added to the discharge kettle of the electrospinning machine, 30.0L 50v% isopropanol aqueous solution is added to the core liquid kettle of the electrospinning machine, after nitrogen protection is introduced into the instrument, the voltage of the electrospinning machine is set to 24kV, the flow rate of the discharge kettle is 2L / h, and the flow rate of the spinning solution 2 is 3L / h, so that the spinning solution is slowly squeezed out from the spinneret to form a hollow thin flow, after being exposed to the air for 12 minutes, the hollow thin flow vertically enters an external coagulation water bath at a temperature of 30°C, and coagulates to obtain a hollow acrylic fiber blank;

[0096] The hollow acrylic fiber blank was transferred to an ultrasonic device, the temperature of the ultrasonic instrument was set to 50°C, the ultrasonic frequency was 50kHz, and the temperature was kept for ultrasonication for 2 hours. The hollow acrylic fiber blank was transferred to a drying oven at a temperature of 70°C and vacuum dried to constant weight to obtain a hollow acrylic fiber.

[0097] Step 5: Prepare lightweight and wear-resistant fabrics

[0098] 84D hollow acrylic fiber is selected, the number of monofilaments is 42F, the twist of the yarn is set to 400 twists / m, the twist direction is Z twist, and after the twisting is completed, it is heat-set at a temperature of 72°C and wound at a speed of 550m / min to obtain the yarn. The yarns are used as warp yarn and weft yarn respectively, and the lightweight wear-resistant fabric is woven; the imperial count of the warp yarn is 35s, and the imperial count of the weft yarn is 40s. The density of the lightweight wear-resistant fabric is 140 warp yarns and 110 weft yarns per square inch.

[0099] Comparative Example 1

[0100] The difference between this comparative example and Example 3 is that step 1 is eliminated, the pretreatment step of wool fiber is retained in step 2, and in step 3, an equal amount of pretreated wool fiber is used to replace the modified wool fiber.

[0101] Comparative Example 2

[0102] The difference between this comparative example and Example 3 is that the step of preparing the wool modified material in step one is eliminated, and in step two, an equal amount of activated multilayer graphene is used to replace the wool modified material.

[0103] Comparative Example 3

[0104] The difference between this comparative example and Example 3 is that the use of polyvinyl pyrrolidone in the step of preparing the spinning solution 1 in step 3 is omitted, and the use of the spinning solution 2 in step 4 is omitted.

[0105] Performance Test:

[0106] The thermal resistance and moisture resistance of the lightweight wear-resistant fabrics prepared in Examples 1-3 and Comparative Examples 1-3 were tested with reference to the standard GB / T 11048-2018 "Determination of thermal resistance and moisture resistance of textiles under steady-state conditions for physiological comfort (evaporative hot plate method)";

[0107] The wear times of the lightweight wear-resistant fabrics prepared in Examples 1-3 and Comparative Examples 1-3 were tested with reference to the standard GB / T 21196.2-2007 "Determination of the abrasion resistance of textile fabrics by the Martindale method - Part 2: Determination of specimen damage";

[0108] The mass per unit area of ​​the lightweight wear-resistant fabrics prepared in Examples 1-3 and Comparative Examples 1-3 was tested with reference to the standard GB / T 4669-2008 "Determination of mass per unit length and mass per unit area of ​​woven textile fabrics";

[0109] With reference to standard GB / T 3923.1-2013 "Tensile properties of textile fabrics Part 1: Determination of breaking strength and elongation at break (strip method)", the elongation at break of the lightweight wear-resistant fabrics prepared in Examples 1-3 and Comparative Examples 1-3 was tested, and the specific data are shown in Table 1.

[0110] Table 1-Performance test data of each sample

[0111] Project Category Example 1 Example 2 Example 7 Comparative Example 1 Comparative Example 2 Comparative Example 3 <![CDATA[Thermal resistance / m 2 ·K·W -1 > 0.4 0.5 0.5 0.3 0.3 0.1 <![CDATA[Moisture resistance / m 2 ·Pa·W -1 > 321 308 295 342 336 452 Wear times / times 3500 3600 3800 2100 2400 3200 <![CDATA[Grammage per unit area / g·m -2 > 83.2 81.3 78.5 88.9 96.5 152.2 Elongation at break / % 48.0 50.1 52.3 23.5 42.1 44.3

[0112] Data Analysis:

[0113] Comparing and analyzing the data in Table 1 above, the thermal resistance of the lightweight wear-resistant fabric prepared by the present invention is 0.5m 2 ·K·W -1 、Wet resistance 295m 2 ·Pa·W -1 , abrasion resistance 3800 times, unit area mass 78.5g·m -2 And the elongation at break is 52.3;

[0114] By comparing the data of Example 3 and Comparative Example 1, it can be found that the wear resistance and elongation at break of the material are significantly reduced, indicating that the present invention prepares titanium dioxide particles with activated multilayer graphene as the core and double bonds on the surface as the wool modified material, and after the surface is activated by glutathione, the active functional group amino group on the surface combines with the pre-treated wool fiber to obtain the modified wool fiber, and the double bonds on the wool modified material are used as cross-linking groups to continuously polymerize acrylonitrile with the modified wool fiber as the matrix to obtain composite polyacrylonitrile, so that the polyacrylonitrile segment produces a complex spatial segment structure, and the wool fiber is used as the skeleton, which significantly enhances the wear resistance and elongation at break of the material;

[0115] By comparing the data of Example 3 and Comparative Example 2, it can be found that the wear resistance and elongation at break of the material are significantly reduced, indicating that the present invention introduces highly conductive titanium dioxide as the shell structure of activated multilayer graphene and introduces carbon-carbon double bonds in the process of forming the shell structure. The former produces a stable electric field effect during the electrospinning process, promoting the spinning solution to be more delicate and uniform. The carbon-carbon double bonds enable the composite polyacrylonitrile to form a more stable structure with the modified wool fiber during the synthesis process, thereby forming a network structure in the fiber, which helps to disperse stress and increase the overall durability of the fiber, and finally significantly enhances the wear resistance and tensile strength of the material.

[0116] By comparing the data of Example 3 and Comparative Example 3, it can be found that the unit area mass and moisture resistance of the material are significantly improved, and the thermal resistance is significantly reduced, indicating that the present invention introduces a pore-forming agent and a spinning solution in the process of spinning and pore-forming to form a stable porous hollow structure of the material. The air layer contained in the hollow fiber has a very low thermal conductivity, which effectively isolates the external cold air and the heat loss in the body. The porous structure of the fiber provides an additional insulation layer, which increases the complexity of heat transfer inside the material, thereby further improving the warmth retention performance. The porous structure not only insulates heat, but also allows air circulation, which is conducive to the discharge of moisture in the body. When the human body sweats, moisture will escape through these tiny pores. The hollow fiber can absorb and conduct moisture through capillary action, and move from the skin surface to the outside of the fiber. This moisture transmission effect from wet to dry further enhances the moisture permeability of the fabric.

[0117] The present invention prepares a wool modified material and activates it, then modifies the wool fiber to overcome its defects such as poor wear resistance and high temperature resistance, and introduces carbon-carbon double bonds on its surface, so that the modified wool fiber serves as a skeleton hybrid organic chain segment structure in the process of composite polyacrylonitrile synthesis, thereby improving the mechanical properties of the composite polyacrylonitrile, and utilizing the conductivity of the wool modified material to promote the electrospinning process, ultimately preparing hollow acrylic fibers with a hollow porous structure, and weaving them to obtain lightweight and wear-resistant fabrics.

[0118] The above contents are merely examples and explanations of the structure of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the structure of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.

Claims

1. A method for preparing a wear-resistant, lightweight, warm-keeping fabric, characterized in that: The following steps are involved: S1, adding modified wool fiber, acrylonitrile and N,N-dimethylformamide into a reactor, raising the temperature of the reactor to 60-80°C, adding azobisisobutyronitrile into the reactor, keeping the temperature for 2-4h, and post-treating to obtain composite polyacrylonitrile; S2, adding composite polyacrylonitrile, polyvinyl pyrrolidone, antibacterial agent, reinforcing agent, plasticizer, crosslinking agent and N,N-dimethylformamide into a reaction kettle, stirring at room temperature for 10-15 minutes, and obtaining a spinning solution 1; S3, using the spinning solution 1 and the spinning solution 2 to electrospin to obtain a hollow acrylic fiber; S4. Use modified acrylic fiber to weave lightweight and wear-resistant fabrics.

2. The method for preparing a wear-resistant, lightweight, warm-keeping fabric according to claim 1, characterized in that: In step S1, the stirring rate of the reactor is 80-120rpm, and the amount ratio of the modified wool fiber, acrylonitrile, N,N-dimethylformamide and azobisisobutyronitrile is 5-6g:8-10g:60-80mL:1-2g; in step S2, the amount ratio of composite polyacrylonitrile, polyvinyl pyrrolidone, antibacterial agent, reinforcing agent, plasticizer, cross-linking agent and N,N-dimethylformamide is 12-15g:1-2g:0.5-0.8g:0.5-0.8g:0.5-0.8g:0.3-0.5g:70-80mL, and the stirring rate of the reactor is 80-120rpm; in step S3, the spinning solution 2 is a 40-60v% isopropanol aqueous solution.

3. The method for preparing a wear-resistant, lightweight, warm-keeping fabric according to claim 1, characterized in that: In step S3, the electrospinning operation includes the following steps: A1. Add the spinning solution 1 to the discharge kettle of the electrospinning machine, add the spinning solution 2 to the core solution kettle of the electrospinning machine, and after nitrogen protection is introduced into the instrument, set the voltage of the electrospinning machine to 20-30 kV, the flow rate of the discharge kettle to 1-3 mL / min, and the flow rate of the spinning solution 2 to 1-4 mL / min, so that the spinning solution is slowly extruded from the spinneret to form a hollow thin flow. After being exposed to the air for 10-15 minutes, the hollow thin flow vertically enters an external coagulation water bath with a temperature of 20-40° C. to coagulate to obtain a hollow acrylic fiber blank; A2. The hollow acrylic fiber blank is transferred to an ultrasonic device, the temperature of the ultrasonic device is set to 40-60°C, the ultrasonic frequency is 40-60kHz, and the ultrasonic is kept warm for 1-2 hours. The hollow acrylic fiber blank is transferred to a drying oven at a temperature of 60-80°C and vacuum dried to constant weight to obtain a hollow acrylic fiber.

4. The method for preparing a wear-resistant, lightweight, warm-keeping fabric according to claim 1, characterized in that: In step S4, the weaving operation is: selecting 75-100D hollow acrylic fiber, the number of monofilaments is 36-48F, setting the twist of the yarn to 300-500 twists / m, the twist direction is Z twist, and after twisting, heat setting is performed at a temperature of 60-80°C, and winding is performed at a speed of 500-600m / min to obtain yarn, the yarns are used as warp yarns and weft yarns, respectively, and weaving to obtain lightweight wear-resistant fabrics; the imperial count of the warp yarns is 30-40s, the imperial count of the weft yarns is 35-45s, and the density of the lightweight wear-resistant fabrics is 120-160 warp yarns and 90-120 weft yarns per square inch.

5. The method for preparing a wear-resistant, lightweight, warm-keeping fabric according to claim 1, characterized in that: The preparation method of modified wool fiber comprises the following steps: B1. Add the wool modified material, dicyclohexylcarbodiimide and dichloromethane into a reactor, stir at room temperature for 30-40 minutes, add glutathione into the reactor, continue stirring for 4-6 hours, and post-treat to obtain an activated filler; B2. Add the pre-treated wool fiber, activated filler and deionized water into an ultrasonic instrument, perform ultrasonic treatment for 1-2 hours, and perform post-treatment to obtain modified wool fiber.

6. The method for preparing a wear-resistant, lightweight, warm-keeping fabric according to claim 5, characterized in that: In step B1, the amount ratio of wool modified material, dicyclohexylcarbodiimide, dichloromethane and glutathione is 8-10g:1-2g:30-40mL:4-5g; in step B2, the amount ratio of pre-treated wool fiber, activated filler and deionized water is 5-6g:2-3g:30-40mL, the power of the ultrasonic instrument is 80-90W, the temperature is 70-90℃, the frequency is 40-60kHz, and the pre-treatment operation is: transfer the wool fiber to a sodium carbonate solution with a concentration of 0.06-0.08mol / L for ultrasonication, the bath ratio is 1:80-100, the ultrasonic frequency is 20-40khz, after the ultrasonication is completed, wash with deionized water for 3-5 times, transfer to a drying oven at a temperature of 60℃ and dry to constant weight to obtain pre-treated wool fiber.

7. The method for preparing a wear-resistant, lightweight, warm-keeping fabric according to claim 1, characterized in that: The preparation method of the wool modified material comprises the following steps: C1. Add multilayer graphene and ethanol to a reactor and stir. After stirring at room temperature for 15-20 minutes, pour the mixed acid solution into the reactor and raise the temperature of the reactor to 40-60° C. After acidification for 0.5 hours, add potassium permanganate to the reactor and stir at this temperature for 8-12 hours. After post-treatment, obtain activated multilayer graphene. C2. Add activated multilayer graphene, butyl titanate, 3-(triethoxysilyl)propyl methacrylate and anhydrous ethanol into a reactor and stir. After stirring at room temperature for 15-20 minutes, continue to drop deionized water and polyvinyl pyrrolidone. After the temperature of the reactor is increased to 40-60°C, use 1-1.5 mol / L ammonia solution to adjust the pH of the system to 8-9, keep warm for 24-36 hours to obtain a composite gel, and then post-treat to obtain a wool modified material.

8. The method for preparing a wear-resistant, lightweight, warm-keeping fabric according to claim 6, characterized in that: In step C1, the stirring rate of the reactor is 80-120rpm, the amount ratio of multilayer graphene, ethanol, acidified solution and oxidant is 5-8g:18-24mL:10-12mL:3-5g, and the acidified solution is obtained by mixing 98.0wt% concentrated sulfuric acid and 30-40wt% nitric acid in a volume ratio of 3:1; in step C2, the stirring rate of the reactor is 60-80rpm, and the amount ratio of activated multilayer graphene, butyl titanate, 3-(triethoxysilyl)propyl methacrylate, anhydrous ethanol, deionized water and polyvinyl pyrrolidone is 1-2g:3-6g:0.3-0.5g:30-40mL:10-20mL:0.1-0.2g.

9. A wear-resistant, lightweight, warm-keeping fabric, characterized in that: The wear-resistant, lightweight, warm-keeping fabric is prepared by the method for preparing the wear-resistant, lightweight, warm-keeping fabric according to any one of claims 1 to 8.

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