Warm-keeping and moisture-permeable cold-proof cotton-padded clothes composite fabric and preparation method thereof

Abstract

The invention discloses a warm-keeping moisture-permeable cold-proof cotton-padded clothes composite fabric and a preparation method thereof, belongs to the technical field of composite fabrics, and aims to solve the technical problem that the thermal insulation property, moisture permeability, toughness and wear resistance of a cotton-padded clothes composite fabric in the prior art need to be further improved. Adding acrylic puree, microencapsulated polyethylene glycol, modified montmorillonite and an auxiliary additive into a reaction kettle to prepare a spinning solution, performing spinning and drafting on the spinning solution, performing reflux treatment by using a dopamine solution to obtain acrylic fibers, finally adding the acrylic fibers into a knitting machine, and knitting by using a warp and weft knitting method to obtain a finished product. The cotton-padded clothes composite fabric is obtained. Through the synergistic effect of the microencapsulated polyethylene glycol, the modified montmorillonite and the dopamine solution, the thermal insulation performance, the moisture permeability, the toughness and the wear resistance of the cotton clothes composite fabric are further improved.

Description

Technical Field

[0001] This invention relates to the field of composite fabric technology, specifically to a warm, breathable, and cold-proof cotton-padded composite fabric and its preparation method. Background Technology

[0002] In the field of composite fabric technology, cold-proof cotton clothing fabrics need to meet the comprehensive requirements of warmth, moisture permeability, abrasion resistance and mechanical properties to adapt to the wearing comfort and durability in cold environments. However, cotton clothing fabrics prepared by traditional processes have performance imbalance problems and it is difficult to take multiple core indicators into account.

[0003] Currently, traditional thermal fabrics mostly rely on heavy fiber filling or coating treatments. While these can improve insulation, they significantly sacrifice breathability, leading to sweat buildup and discomfort from dampness and cold. Furthermore, the fabrics lack flexibility and abrasion resistance, making them prone to breakage and damage over time. Some improvement solutions attempt to optimize performance by adding single functional components, such as using polyethylene glycol for heat storage modification. However, these lack a stable coating structure, leading to component loss and failing to achieve long-lasting insulation. Other solutions involve simply adding nanoparticles to increase strength, but uneven particle dispersion reduces breathability, further exacerbating the moisture-wicking shortcomings. Simultaneously, fiber surface modification technologies are relatively limited; conventional treatments struggle to form a stable functional layer on the fiber surface, failing to effectively strengthen fiber interfacial bonding or create efficient moisture transport channels. Moreover, a multi-component synergistic mechanism is lacking; each functional component functions independently, failing to achieve simultaneous improvements in insulation, breathability, toughness, and abrasion resistance through structural design and component combination. Consequently, the overall performance of these fabrics fails to meet the demands of high-end cold-weather clothing.

[0004] To address this technical deficiency, a solution is proposed. Summary of the Invention

[0005] The purpose of this invention is to provide a warm and breathable cold-proof cotton-padded composite fabric and its preparation method, which solves the technical problem that the thermal insulation performance, moisture permeability, elongation at break and abrasion resistance of cotton-padded composite fabrics in the prior art need to be further improved.

[0006] The objective of this invention can be achieved through the following technical solution: a method for preparing a warm, breathable, and cold-resistant cotton-padded composite fabric, comprising the following steps:

[0007] S1. Add acrylic fiber sizing, microencapsulated polyethylene glycol, modified montmorillonite and auxiliary additives to a reaction vessel, stir at 20-30℃ for 20-30 min, and stir under a vacuum of -0.08MPa for 1-2 h to obtain spinning solution.

[0008] S2. Add the spinning solution to the metering pump, and after extrusion through the spinneret, stretch it 2-3 times. The stretched fiber is sprayed with sodium sulfonate aqueous solution and then transferred to dopamine solution for reflux treatment to obtain acrylic fiber.

[0009] S3. Add acrylic fibers to the weaving machine and weave them using a warp and weft weaving method to obtain a cotton-padded composite fabric.

[0010] Further, in step S1, the ratio of the acrylonitrile sizing, microencapsulated polyethylene glycol, modified montmorillonite, and auxiliary additives is 100g:8-12g:1-3g:3-4g; in step S2, the sodium sulfonate aqueous solution has a mass fraction of 5%, a spraying pressure of 0.2MPa, and a spraying time of 15-20s; in step S3, in the warp and weft knitting method, the warp density is 40-60 count, and the weft density is 40-60 count.

[0011] Furthermore, the preparation method of the acrylic fiber sizing is as follows: acrylonitrile, methyl acrylate, and itaconic acid are added to a reaction vessel containing dimethylformamide, and stirred for 30-40 minutes under a nitrogen atmosphere at 20-30°C. Then, azobisisobutyronitrile is added, and the mixture is heated to 60-70°C and reacted for 3-5 hours. After that, hydroquinone solution is added and stirred for another 15-20 minutes. After the reaction is completed, acrylic fiber sizing is obtained. The ratio of acrylonitrile, methyl acrylate, itaconic acid, dimethylformamide, azobisisobutyronitrile, and hydroquinone is 23-24 mL:7 mL:1-2 g:75-80 mL:0.2-0.3 g:0.8-1.5 mL. The hydroquinone solution is obtained by dissolving 1 g of hydroquinone in 19 mL of dimethylformamide.

[0012] Reaction mechanism:

[0013] Under a nitrogen atmosphere, acrylonitrile, methyl acrylate, and itaconic acid are stirred and dispersed in dimethylformamide to form a homogeneous monomer solution. Subsequently, azobisisobutyronitrile (AIBN) is added to break the N=N bonds in the molecule, generating highly reactive cyano radicals. These radicals act as initiation centers, sequentially attacking and opening the carbon-carbon double bonds in the three monomer molecules. Through initiation and propagation processes, the three monomers undergo free radical copolymerization. Once the polymer molecular weight in the system reaches a preset range, hydroquinone terminates the chain propagation reaction by capturing the remaining reactive free radicals in the system, ultimately forming a homogeneous viscous solution of the random copolymer of the three monomers in dimethylformamide, i.e., acrylic fiber sizing.

[0014] Furthermore, the preparation method of the microencapsulated polyethylene glycol is as follows: chitosan is added to an acetic acid solution, and stirred at 20-30°C until the chitosan is completely dissolved. Then, polyethylene glycol is added, and the solution is stirred until it is transparent and homogeneous. Polyoxyethylene sorbitan monooleate and benzyl alcohol are added, and the mixture is stirred for 30-60 minutes. Then, sodium hydroxide solution is added dropwise to adjust the pH of the solution to 6.5-7.0. Finally, sodium tripolyphosphate aqueous solution is added dropwise. After the addition is complete, the mixture is ultrasonically dispersed for 10-20 minutes. After post-treatment, microencapsulated polyethylene glycol is obtained.

[0015] Reaction mechanism:

[0016] Acetic acid solution protonates the amino groups on the chitosan molecular chain, transforming chitosan from hydrophobic to water-soluble, resulting in a homogeneous aqueous phase. Polyethylene glycol, due to its hydrophilicity, is compatible with the aqueous phase and is uniformly dispersed in the chitosan solution. Subsequently, polyoxyethylene sorbitan monooleate is added as an emulsifier; its hydrophilic end anchors the aqueous phase, while its hydrophobic end encapsulates benzyl alcohol. Stirring forms a stable oil-water emulsion, dispersing benzyl alcohol into tiny oil droplets. Sodium hydroxide solution is added to neutralize excess acetic acid and simultaneously deprotonates the chitosan amino groups, restoring moderate hydrophobicity. Added sodium tripolyphosphate undergoes ionic cross-linking through electrostatic interaction between phosphate groups and the chitosan amino groups, forming a continuous and stable chitosan cross-linked wall material on the surface of the oil droplets and around the polyethylene glycol dispersed in the aqueous phase. Finally, after centrifugation, freeze-drying, pulverization, and sieving, composite microcapsules with a chitosan cross-linked structure as the wall material and encapsulating polyethylene glycol and benzyl alcohol are obtained.

[0017] Furthermore, the ratio of chitosan, acetic acid solution, polyethylene glycol, polyoxyethylene sorbitan monooleate, benzyl alcohol, and sodium tripolyphosphate aqueous solution is 1g:50mL:0.8g:0.5-0.6g:0.3g:25mL, the mass fraction of the acetic acid solution is 1.5%, the mass fraction of the sodium hydroxide solution is 1%, and the mass fraction of the sodium tripolyphosphate aqueous solution is 2%. The post-processing operation includes: after the reaction is completed, centrifugation is performed, the product is transferred to a vacuum drying oven, freeze-dried at -40℃ for 72h, pulverized, and passed through a 300-mesh sieve to obtain microencapsulated polyethylene glycol.

[0018] Furthermore, the modified montmorillonite is prepared by the following steps:

[0019] A1. Add montmorillonite to deionized water and stir at 50-60℃ for 20-30 minutes. Then add KH560 solution dropwise. After the addition is complete, stir for 3-4 hours and then process to obtain organomontmorillonite.

[0020] A2. Add the organic montmorillonite to deionized water and stir at 20-30℃ for 10-20 minutes. Then add polyacrylic acid and stannous octoate and stir at 50-60℃ for 3-4 hours. After post-treatment, the modified montmorillonite is obtained.

[0021] Reaction mechanism:

[0022] The ethoxy group of KH560 undergoes hydrolysis under weakly acidic conditions to generate silanol groups. Subsequently, the silanol groups undergo a condensation reaction with the hydroxyl groups on the surface of montmorillonite to form stable Si-O-Al covalent bonds, anchoring the KH560 molecules to the surface of montmorillonite and introducing a large number of active epoxy groups. Then, after dispersing the epoxy-modified montmorillonite in deionized water, the carboxyl groups on the polyacrylic acid molecular chain undergo a ring-opening esterification reaction with the epoxy groups on the surface of montmorillonite under the action of stannous octoate catalyst, generating stable -COC- covalent bonds. This allows the hydrophilic carboxyl segments of polyacrylic acid to be firmly grafted onto the surface of montmorillonite. Finally, the introduction of high-density hydrophilic carboxyl groups endows montmorillonite with superhydrophilic properties, thus preparing the target modified montmorillonite.

[0023] Further, in step A1, the ratio of montmorillonite, deionized water, and KH560 solution is 1g:19mL:3mL. The KH560 solution is obtained by dissolving 1.5g of KH560 in 30mL of 90wt% ethanol solution, then adding acetic acid to adjust the pH of the solution to 4-5, and stirring for 20-30min. The post-treatment operation includes: after the reaction, filtration, washing with deionized water 3-5 times, drying in a vacuum drying oven at 60℃ for 12h, grinding, and passing through a 200-mesh sieve to obtain organomontmorillonite. In step A2, the ratio of organomontmorillonite, deionized water, polyacrylic acid solution, and stannous octoate is 1g:15mL:0.4g:0.015g. The post-treatment operation includes: after the reaction, filtration, washing with deionized water 3-5 times, drying in a vacuum drying oven at 60℃ for 12h, grinding, and passing through a 200-mesh sieve to obtain modified montmorillonite.

[0024] Further, in step S2, the dopamine solution is prepared by adding dopamine hydrochloride, sodium carbonate, deionized water and 1,4-dioxane into a reaction vessel and stirring at 20-30°C for 20-30 minutes to obtain a dopamine solution; the ratio of the amount of dopamine hydrochloride, sodium carbonate, deionized water and 1,4-dioxane is 2-2.2g:1.1g:12mL:12mL.

[0025] Reaction mechanism:

[0026] Dopamine hydrochloride dissolves in the system, and sodium carbonate acts as an alkalizer, neutralizing the hydrochloric acid in the dopamine hydrochloride. At the same time, it promotes the activation of the catechol groups in the dopamine molecule and partially causes oxidative self-polymerization, forming polydopamine oligomers containing active groups such as catechol and amino groups. These oligomers are dispersed in a mixed solvent of water and 1,4-dioxane to form a dopamine solution.

[0027] Further, in step S2, the reflux treatment includes: immersing the drawn fiber in a dopamine solution, refluxing it under a nitrogen atmosphere at 100-110°C for 20-22 hours, removing it after the reaction, washing it with distilled water at 70-80°C, then refluxing it in ethanol at 80°C for 5-6 hours, removing it, and drying it under vacuum at 60°C for 12 hours to obtain acrylic fiber; the ratio of the drawn fiber to the dopamine solution is 1g:25mL.

[0028] Reaction mechanism:

[0029] After immersing the drawn fibers in a dopamine solution, they are first refluxed under a nitrogen atmosphere to accelerate the oxidative self-polymerization reaction of dopamine and polydopamine, forming more polydopamine. The polydopamine molecules interact with the cyano groups on the surface of the drawn fibers through hydrogen bonds formed by their surface active amino and hydroxyl groups, forming a uniform polydopamine coating layer on the fiber surface. After the reaction, the ungrafted free polydopamine is removed by washing with distilled water, and further purified by reflux with ethanol. Finally, the fibers are vacuum dried to obtain acrylic fibers with polydopamine grafted on the surface.

[0030] The present invention also proposes a warm and breathable cotton-padded composite fabric, which is prepared by the above-mentioned warm and breathable cotton-padded composite fabric preparation process.

[0031] The present invention has the following beneficial effects:

[0032] 1. In this invention, the hydrophilic carboxyl groups on the surface of modified montmorillonite interact with the polar groups of acrylonitrile slurry, providing a stable dispersion carrier for microencapsulated polyethylene glycol and preventing its aggregation. The polydopamine coating layer formed on the fiber surface after treatment with dopamine solution can further anchor the functional components, so that the microencapsulated polyethylene glycol is evenly distributed inside and on the surface of the fiber. The polyethylene glycol inside the microcapsules can achieve heat storage and insulation through phase change, while the chitosan cross-linked wall material reduces heat loss. Combined with the fluffy fiber structure of the acrylonitrile slurry itself, the three work together to construct a highly efficient heat insulation system, which greatly improves the thermal insulation performance of the composite fabric.

[0033] 2. In this invention, the polyacrylic acid segments grafted with modified montmorillonite bring a large number of hydrophilic groups, and the chitosan wall material of the microcapsules also has good hydrophilicity. The two, together with the amino and hydroxyl groups formed on the surface of the acrylic slurry after dopamine treatment, construct a continuous hydrophilic channel. The porous structure of the microcapsules can adsorb water vapor, and the hydrophilic groups of the modified montmorillonite accelerate the penetration and transport of water vapor. The dopamine coating layer can enhance the interaction between the fiber and water vapor, so that the fabric can quickly absorb sweat from the body surface and diffuse it to the outside, achieving a combination of efficient moisture absorption and breathability.

[0034] 3. In this invention, the polydopamine coating layer formed by the dopamine solution enhances the interfacial bonding force between fibers. Modified montmorillonite, as a nano-reinforcing phase, is uniformly dispersed in the acrylic slurry, which can disperse stress under load. The microencapsulated polyethylene glycol elastic chitosan wall material can buffer external force impact through deformation, reducing the risk of local fiber breakage. At the same time, the uniform dispersion of each component avoids stress concentration inside the fabric. The surface roughness of the fibers after dopamine treatment optimizes the structural tightness after weaving and improves the frictional stability between fibers. This not only enhances the fabric's resistance to breakage during stretching but also improves its resistance to frictional loss. Detailed Implementation

[0035] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0036] In this application, the polyoxyethylene dehydrated sorbitan monooleate is selected from Wuhan Maikairui Chemical Co., Ltd., with CAS number 9005-65-6 and model number 500-019-9;

[0037] In this application, the polyethylene glycol is selected from Yunsheng Chemical (Shandong) Co., Ltd., CAS No. 25322-68-3, model 0123;

[0038] In this application, montmorillonite, Lingshou County Tairun Mineral Products Co., Ltd., item number 9846465;

[0039] In this application, polyacrylic acid, Jinan Juyang Chemical Technology Co., Ltd., CAS No. 9003-01-4, has an active ingredient content of 99%.

[0040] Example 1

[0041] This embodiment provides a method for preparing a warm, breathable, and cold-proof cotton-padded composite fabric, including the following steps:

[0042] S1. Preparation of acrylic fiber slurry

[0043] Weigh out 1 kg of hydroquinone and dissolve it in 19 L of dimethylformamide to obtain a hydroquinone solution;

[0044] Weigh out 23L of acrylonitrile, 7L of methyl acrylate and 1kg of itaconic acid and add them to a reactor containing 75L of dimethylformamide. Stir for 30 minutes under a nitrogen atmosphere at 20°C. Then add 0.2kg of azobisisobutyronitrile and heat to 60°C to react for 3 hours. Then add 0.8L of hydroquinone solution and stir for another 15 minutes. After the reaction is complete, acrylic fiber slurry is obtained.

[0045] S2, Preparation of microencapsulated polyethylene glycol

[0046] Weigh 1 kg of chitosan and add it to 50 L of 1.5 wt% acetic acid solution. Stir at 20 °C until the chitosan is completely dissolved. Then add 0.8 kg of polyethylene glycol and stir until the solution is clear and homogeneous. Add 0.5 kg of polyoxyethylene sorbitan monooleate and 0.3 kg of benzyl alcohol and continue stirring for 30 min. Then add 1 wt% sodium hydroxide solution to adjust the pH of the solution to 6.5. Finally, add 25 L of 2 wt% sodium tripolyphosphate aqueous solution. After the addition is complete, sonicate and disperse for 10 min. After the reaction is complete, centrifuge and transfer the product to a vacuum drying oven. Freeze-dry at -40 °C for 72 h, then pulverize and pass through a 300 mesh sieve to obtain microencapsulated polyethylene glycol.

[0047] S3. Preparation of modified montmorillonite

[0048] Weigh out 15g of KH560 and dissolve it in 300mL of 90wt% ethanol solution. Then add acetic acid to adjust the pH of the solution to 4 and stir for 20min to obtain KH560 solution.

[0049] Weigh 1 kg of montmorillonite and add it to 19 L of deionized water. Stir at 50 °C for 20 min. Then add 3 L of KH560 solution dropwise. After the addition is complete, stir for 3 h. After the reaction is complete, filter, wash 3 times with deionized water, place in a vacuum drying oven at 60 °C and dry for 12 h. Grind and pass through a 200 mesh sieve to obtain organomontmorillonite.

[0050] Weigh 1 kg of organomontmorillonite and add it to 15 L of deionized water. Stir at 20 °C for 10 min. Then add 400 g of polyacrylic acid and 15 g of stannous octoate. Stir at 50 °C for 3 h. After the reaction is complete, filter the mixture, wash it three times with deionized water, and dry it in a vacuum drying oven at 60 °C for 12 h. Grind the mixture and pass it through a 200 mesh sieve to obtain modified montmorillonite.

[0051] S4. Preparation of spinning solution

[0052] Weigh out 100 kg of acrylic fiber slurry, 8 kg of microencapsulated polyethylene glycol, 1 kg of modified montmorillonite, and 3 kg of auxiliary additives and add them to the reaction vessel. Stir at 20°C for 20 min and then stir at a vacuum of -0.08 MPa for 1 h to obtain the spinning solution.

[0053] S5. Preparation of dopamine solution

[0054] Weigh out 2 kg of dopamine hydrochloride, 1.1 kg of sodium carbonate, 12 L of deionized water and 12 L of 1,4-dioxane and add them to the reaction vessel. Stir at 20 °C for 20 min to obtain a dopamine solution.

[0055] S6. Preparation of acrylic fibers

[0056] The spinning solution was added to a metering pump, and after being extruded through a spinneret, it was drawn twice. The drawn fiber was sprayed with a 5wt% sodium sulfonate aqueous solution at a spray pressure of 0.2MPa for 15s. Then, 1kg of the drawn fiber was immersed in 25L of dopamine solution and refluxed at 100℃ under a nitrogen atmosphere for 20h. After the reaction was completed, it was taken out, washed with distilled water at 70℃, and then refluxed in ethanol at 80℃ for 5h. After that, it was taken out and dried under vacuum at 60℃ for 12h to obtain acrylic fiber.

[0057] S7. Preparation of cotton-padded composite fabric

[0058] Acrylic fibers are added to a weaving machine and woven using a warp and weft weaving method with a warp density of 40 count and a weft density of 40 count to obtain a cotton-padded composite fabric.

[0059] Example 2

[0060] This embodiment provides a method for preparing a warm, breathable, and cold-proof cotton-padded composite fabric, including the following steps:

[0061] S1. Preparation of acrylic fiber slurry

[0062] Weigh out 1 kg of hydroquinone and dissolve it in 19 L of dimethylformamide to obtain a hydroquinone solution;

[0063] Weigh out 23.5L of acrylonitrile, 7L of methyl acrylate and 1.5kg of itaconic acid and add them to a reactor containing 78L of dimethylformamide. Stir for 35 minutes under a nitrogen atmosphere at 25°C. Then add 0.2kg of azobisisobutyronitrile and heat to 60°C to react for 4 hours. Then add 1.2L of hydroquinone solution and stir for another 18 minutes. After the reaction is complete, acrylic fiber slurry is obtained.

[0064] S2, Preparation of microencapsulated polyethylene glycol

[0065] Weigh 1 kg of chitosan and add it to 50 L of 1.5 wt% acetic acid solution. Stir at 25 °C until the chitosan is completely dissolved. Then add 0.8 kg of polyethylene glycol and stir until the solution is clear and homogeneous. Add 0.5 kg of polyoxyethylene sorbitan monooleate and 0.3 kg of benzyl alcohol and continue stirring for 45 min. Then add 1 wt% sodium hydroxide solution to adjust the pH of the solution to 6.8. Finally, add 25 L of 2 wt% sodium tripolyphosphate aqueous solution. After the addition is complete, sonicate and disperse for 15 min. After the reaction is complete, centrifuge and transfer the product to a vacuum drying oven. Freeze-dry at -40 °C for 72 h, then pulverize and pass through a 300 mesh sieve to obtain microencapsulated polyethylene glycol.

[0066] S3. Preparation of modified montmorillonite

[0067] Weigh out 15g of KH560 and dissolve it in 300mL of 90wt% ethanol solution. Then add acetic acid dropwise to adjust the pH of the solution to 4.5 and stir for 25min to obtain KH560 solution.

[0068] Weigh 1 kg of montmorillonite and add it to 19 L of deionized water. Stir at 55 °C for 25 min, then add 3 L of KH560 solution dropwise. After the addition is complete, stir for 3.5 h. After the reaction is complete, filter, wash 4 times with deionized water, dry in a vacuum drying oven at 60 °C for 12 h, grind, and pass through a 200 mesh sieve to obtain organomontmorillonite.

[0069] Weigh 1 kg of organomontmorillonite and add it to 15 L of deionized water. Stir at 25 °C for 15 min. Then add 400 g of polyacrylic acid and 15 g of stannous octoate. Stir at 55 °C for 3.5 h. After the reaction is complete, filter the mixture, wash it 4 times with deionized water, dry it in a vacuum drying oven at 60 °C for 12 h, grind it, and pass it through a 200 mesh sieve to obtain modified montmorillonite.

[0070] S4. Preparation of spinning solution

[0071] Weigh out 100 kg of acrylic fiber slurry, 10 kg of microencapsulated polyethylene glycol, 2 kg of modified montmorillonite, and 3.5 kg of auxiliary additives and add them to the reaction vessel. Stir at 25°C for 25 min and then stir under a vacuum of -0.08 MPa for 1.5 h to obtain the spinning solution.

[0072] S5. Preparation of dopamine solution

[0073] Weigh out 2.1 kg of dopamine hydrochloride, 1.1 kg of sodium carbonate, 12 L of deionized water and 12 L of 1,4-dioxane and add them to the reaction vessel. Stir at 25 °C for 25 min to obtain a dopamine solution.

[0074] S6. Preparation of acrylic fibers

[0075] The spinning solution was added to a metering pump, and after being extruded through a spinneret, it was stretched twice. The stretched fiber was sprayed with a 5wt% sodium sulfonate aqueous solution at a spray pressure of 0.2MPa for 18s. Then, 1kg of stretched fiber was immersed in 25L of dopamine solution and refluxed at 100℃ under a nitrogen atmosphere for 21h. After the reaction was completed, the fiber was taken out, washed with distilled water at 75℃, and then refluxed in ethanol at 80℃ for 5.5h. After that, the fiber was taken out and dried under vacuum at 60℃ for 12h to obtain acrylic fiber.

[0076] S7. Preparation of cotton-padded composite fabric

[0077] Acrylic fibers are added to a weaving machine and woven using a warp and weft weaving method with a warp density of 50 count and a weft density of 50 count to obtain a cotton-padded composite fabric.

[0078] Example 3

[0079] This embodiment provides a method for preparing a warm, breathable, and cold-proof cotton-padded composite fabric, including the following steps:

[0080] S1. Preparation of acrylic fiber slurry

[0081] Weigh out 1 kg of hydroquinone and dissolve it in 19 L of dimethylformamide to obtain a hydroquinone solution;

[0082] Weigh out 24L of acrylonitrile, 7L of methyl acrylate and 2kg of itaconic acid and add them to a reactor containing 80L of dimethylformamide. Stir for 40min under a nitrogen atmosphere at 30℃. Then add 0.3kg of azobisisobutyronitrile and heat to 70℃ for 5h. Then add 1.5L of hydroquinone solution and stir for another 20min. After the reaction is complete, acrylic fiber slurry is obtained.

[0083] S2, Preparation of microencapsulated polyethylene glycol

[0084] Weigh 1 kg of chitosan and add it to 50 L of 1.5 wt% acetic acid solution. Stir at 30 °C until the chitosan is completely dissolved. Then add 0.8 kg of polyethylene glycol and stir until the solution is clear and homogeneous. Add 0.6 kg of polyoxyethylene sorbitan monooleate and 0.3 kg of benzyl alcohol and continue stirring for 60 min. Then add 1 wt% sodium hydroxide solution to adjust the pH of the solution to 7.0. Finally, add 25 L of 2 wt% sodium tripolyphosphate aqueous solution. After the addition is complete, sonicate and disperse for 20 min. After the reaction is complete, centrifuge and transfer the product to a vacuum drying oven. Freeze-dry at -40 °C for 72 h, then pulverize and pass through a 300 mesh sieve to obtain microencapsulated polyethylene glycol.

[0085] S3. Preparation of modified montmorillonite

[0086] Weigh out 15g of KH560 and dissolve it in 300mL of 90wt% ethanol solution. Then add acetic acid to adjust the pH of the solution to 5 and stir for 30min to obtain KH560 solution.

[0087] Weigh 1 kg of montmorillonite and add it to 19 L of deionized water. Stir at 60 °C for 30 min. Then add 3 L of KH560 solution dropwise. After the addition is complete, stir for 4 h. After the reaction is complete, filter, wash 5 times with deionized water, place in a vacuum drying oven at 60 °C and dry for 12 h. Grind and pass through a 200 mesh sieve to obtain organomontmorillonite.

[0088] Weigh 1 kg of organomontmorillonite and add it to 15 L of deionized water. Stir at 30 °C for 20 min. Then add 400 g of polyacrylic acid and 15 g of stannous octoate. Stir at 60 °C for 4 h. After the reaction is complete, filter the mixture, wash it 5 times with deionized water, and dry it in a vacuum drying oven at 60 °C for 12 h. Grind the mixture and pass it through a 200 mesh sieve to obtain modified montmorillonite.

[0089] S4. Preparation of spinning solution

[0090] Weigh out 100 kg of acrylic fiber slurry, 12 kg of microencapsulated polyethylene glycol, 3 kg of modified montmorillonite, and 4 kg of auxiliary additives and add them to the reaction vessel. Stir at 30°C for 30 min and then stir under a vacuum of -0.08 MPa for 2 h to obtain the spinning solution.

[0091] S5. Preparation of dopamine solution

[0092] Weigh out 2.2 kg of dopamine hydrochloride, 1.1 kg of sodium carbonate, 12 L of deionized water and 12 L of 1,4-dioxane and add them to the reaction vessel. Stir at 30 °C for 30 min to obtain a dopamine solution.

[0093] S6. Preparation of acrylic fibers

[0094] The spinning solution was added to a metering pump, and after being extruded through a spinneret, it was stretched three times. The stretched fiber was sprayed with a 5wt% sodium sulfonate aqueous solution at a spray pressure of 0.2MPa for 20s. Then, 1kg of stretched fiber was immersed in 25L of dopamine solution and refluxed at 110℃ under a nitrogen atmosphere for 22h. After the reaction was completed, the fiber was taken out, washed with distilled water at 80℃, and then refluxed in ethanol at 80℃ for 6h. After that, the fiber was taken out and dried under vacuum at 60℃ for 12h to obtain acrylic fiber.

[0095] S7. Preparation of cotton-padded composite fabric

[0096] Acrylic fibers are added to a weaving machine and woven using a warp and weft weaving method with a warp density of 60 count and a weft density of 60 count to obtain a cotton-padded composite fabric.

[0097] Comparative Example 1

[0098] The difference between this comparative example and Example 3 is that step S2 is omitted, and the polyethylene glycol in step S2 is used instead of the microencapsulated polyethylene glycol in step S4.

[0099] Comparative Example 2

[0100] The difference between this comparative example and Example 3 is that step S3 is omitted, and the modified montmorillonite in step S4 is replaced with the montmorillonite in step S3.

[0101] Comparative Example 3

[0102] The difference between this comparative example and Example 3 is that step S5 is omitted, and the fibers in step S6 are not treated with dopamine solution.

[0103] Performance testing:

[0104] The heat retention rate of the cotton composite fabrics prepared in Examples 1-3 and Comparative Examples 1-3 was determined according to the standard GB / T 35762-2017 "Test Methods for Heat Transfer Properties of Textiles - Plate Method".

[0105] The moisture permeability of the cotton-padded composite fabrics prepared in Examples 1-3 and Comparative Examples 1-3 was determined in accordance with the standard GB / T 12704.1-2009 "Textiles - Test methods for moisture permeability of fabrics - Part 1: Moisture absorption method".

[0106] The elongation at break of the cotton-padded composite fabrics prepared in Examples 1-3 and Comparative Examples 1-3 was determined in accordance with the standard GB / T 3923.1-2013 "Textiles - Tensile Properties of Fabrics - Part 1: Determination of Breaking Strength and Elongation at Break (Strip Method)".

[0107] The mass abrasion rate of the cotton composite fabrics prepared in Examples 1-3 and Comparative Examples 1-3 was determined according to standard FZ / T 01151-2019 "Textiles - Test Method for Abrasion Resistance of Fabrics - Accelerated Friction Method". The specific test results are shown in Table 1 below:

[0108] Table 1 - Performance Test Data of Samples

[0109]

[0110] Data Analysis

[0111] Comparative analysis of the data in Table 1 above shows that the cotton-padded composite fabric prepared by this invention has a heat retention rate of 49.2% and a moisture permeability of 9.93 × 10⁻⁶. 3 g / (m 2 (24h), elongation at break 31.7%, mass wear rate 0.82%;

[0112] Comparative Example 1 showed that replacing microencapsulated polyethylene glycol with ordinary polyethylene glycol resulted in a decrease in heat retention rate to 39.3%. The core issue is that ordinary polyethylene glycol lacks the protective coating of chitosan cross-linked wall material, making it prone to component loss and unable to stably perform its phase change heat storage function. Furthermore, it cannot form a synergistic heat-locking system with modified montmorillonite and acrylonitrile slurry, leading to an accelerated heat loss rate and a decrease in moisture permeability to 8.83 × 10⁻⁶. 3 g / (m 2 •24h), because of the lack of water vapor transport channels provided by the porous structure of microcapsules, and because ordinary polyethylene glycol cannot form a continuous hydrophilic network with the hydrophilic groups of modified montmorillonite and the active groups of polydopamine, the sweat absorption and diffusion efficiency is greatly reduced, the elongation at break is only 25.9%, and the mass wear rate rises to 1.17%. Since ordinary polyethylene glycol does not have the deformation buffering effect of microcapsule elastic wall material, it cannot disperse local stress when the fiber is under force, and is prone to concentrated breakage. At the same time, its bonding force with the fiber interface is weak, and it cannot play a reinforcing and protective role during friction, which aggravates the wear of the fabric.

[0113] Comparative Example 2 used unmodified montmorillonite, with a thermal insulation rate of 40.8%, lower than the example. The core reason for this is that the unmodified montmorillonite lacks hydrophilic carboxyl groups on its surface, making it unable to form a stable interaction with the polar groups of the acrylic fiber slurry. This prevents it from providing a uniformly dispersed carrier for the microencapsulated polyethylene glycol, leading to the aggregation of the insulation components, reduced heat transfer efficiency, and a moisture permeability of only 7.84 × 10⁻⁶. 3 g / (m 2 The 24h value was the lowest among all tested samples. This is because the unmodified montmorillonite was not grafted with polyacrylic acid segments and lacked a continuous water vapor transport channel constructed by high-density hydrophilic groups. Water vapor penetration and diffusion were severely hindered. The performance of 26.6% elongation at break and 1.46% mass wear rate reflects the poor dispersibility of unmodified montmorillonite. It cannot be uniformly dispersed in the acrylonitrile slurry as a nano-reinforcing phase. It is difficult to disperse stress under stress, and the fiber is prone to local breakage. At the same time, its bonding force with the fiber interface is weak, and it is easy to fall off during friction, which aggravates the wear of the fabric.

[0114] Comparative Example 3 fibers, which were not treated with dopamine solution, had the highest mass wear rate of 1.68% among all tested samples. Their elongation at break (27.8%) was significantly lower than that of the Example 3, and their insulation efficiency dropped to 42.8%, which, while higher than the previous two comparative examples, was still far lower than the Example 3. This was mainly due to the lack of a polydopamine coating layer to anchor the functional components, uneven dispersion of microencapsulated polyethylene glycol and modified montmorillonite in the fibers, and partial agglomeration leading to decreased insulation efficiency. The moisture permeability was 8.34 × 10⁻⁶. 3 g / (m 2The 24h delay is due to the absence of a polydopamine layer containing amino and hydroxyl groups on the fiber surface. This weakens the interaction between the fiber and water vapor, hindering the rapid adsorption and transport of water vapor. The most prominent issues are the deterioration of breaking elongation and abrasion resistance. The core reason is that the lack of a polydopamine coating layer leads to a significant decrease in the interfacial bonding force between fibers. At the same time, the smooth fiber surface results in insufficient structural tightness after weaving and poor frictional stability. This makes the fabric prone to fiber slippage and breakage during stretching and fiber shedding during friction, ultimately manifesting as a dual deterioration in both toughness and abrasion resistance.

[0115] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to specific implementations. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims

1. A method for preparing a cold-proof and moisture-permeable cotton coat composite fabric, characterized in that, The method comprises the following steps: S1, acrylonitrile, methyl acrylate and itaconic acid are added to a reaction kettle containing dimethylformamide, stirred at 20-30℃ under nitrogen atmosphere for 30-40min, then azobisisobutyronitrile is added, heated to 60-70℃ and reacted for 3-5h, then hydroquinone solution is added and stirred for 15-20min, and the acrylonitrile, methyl acrylate, itaconic acid, dimethylformamide, azobisisobutyronitrile and hydroquinone are used in a ratio of 23-24mL:7mL:1-2g:75-80mL:0.2-0.3g:0.8-1.5mL, and the hydroquinone solution is obtained by dissolving 1g of hydroquinone in 19mL of dimethylformamide; S2, the spinning solution is added to a metering pump, extruded through a spinneret and then stretched by 2-3 times, the stretched fiber is sprayed with a sodium sulfonate aqueous solution, then transferred to a dopamine solution for reflux treatment, and an acrylic fiber is obtained; S3, the acrylic fiber is added to a knitting machine and knitted by warp-weft knitting method to obtain a cotton-padded jacket composite fabric.

2. The method of claim 1, wherein the method is characterized by the steps of: In step S1, the amount ratio of the acrylic fiber stock, microencapsulated polyethylene glycol, modified montmorillonite and auxiliary additive is 100g:8-12g:1-3g:3-4g; in step S2, the mass fraction of the sodium sulfonate aqueous solution is 5%, the spraying pressure is 0.2MPa, and the spraying time is 15-20s; in step S3, in the warp-weft knitting method, the warp density is 40-60 ends, and the weft density is 40-60 ends.

3. The method for preparing a warm, breathable, and cold-resistant cotton-padded composite fabric according to claim 1, characterized in that, The preparation method of the acrylic fiber stock is as follows: acrylonitrile, methyl acrylate and itaconic acid are added to a reaction kettle containing dimethylformamide, stirred at 20-30℃ under nitrogen atmosphere for 30-40min, then azobisisobutyronitrile is added, heated to 60-70℃ and reacted for 3-5h, then hydroquinone solution is added and stirred for 15-20min, and the acrylonitrile, methyl acrylate, itaconic acid, dimethylformamide, azobisisobutyronitrile and hydroquinone are used in a ratio of 23-24mL:7mL:1-2g:75-80mL:0.2-0.3g:0.8-1.5mL, and the hydroquinone solution is obtained by dissolving 1g of hydroquinone in 19mL of dimethylformamide; 4. The method of claim 1, wherein the method is characterized by the steps of: The preparation method of the microencapsulated polyethylene glycol is as follows: chitosan is added to an acetic acid solution, stirred at 20-30℃ until the chitosan is completely dissolved, then polyethylene glycol is added, followed by stirring until the solution is transparent and uniform, then polyoxyethylene sorbitan monooleate and benzyl alcohol are added, and the stirring is continued for 30-60min, then sodium hydroxide solution is added dropwise to adjust the pH of the solution to 6.5-7.0, and finally sodium tripolyphosphate aqueous solution is added dropwise, and after the addition is completed, ultrasonic dispersion is performed for 10-20min, and post-treatment is performed to obtain the microencapsulated polyethylene glycol.

5. The method of claim 4, wherein the method further comprises the steps of: a) applying a water repellent agent to the outer surface of the first layer; and b) applying a water repellent agent to the outer surface of the second layer. The amount ratio of the chitosan, acetic acid solution, polyethylene glycol, polyoxyethylene sorbitan monooleate, benzyl alcohol and sodium tripolyphosphate aqueous solution is 1g:50mL:0.8g:0.5-0.6g:0.3g:25mL, the mass fraction of the acetic acid solution is 1.5%, the mass fraction of the sodium hydroxide solution is 1%, and the mass fraction of the sodium tripolyphosphate aqueous solution is 2%; the post-treatment operation includes: after the reaction is completed, centrifugal separation is performed, the product is transferred to a vacuum drying box, freeze-dried at-40℃ for 72h, crushed, and passed through a 300 mesh sieve to obtain the microencapsulated polyethylene glycol.

6. The method for preparing a warm, breathable, and cold-resistant cotton-padded composite fabric according to claim 1, characterized in that, The modified montmorillonite is prepared by the following steps: A1, the montmorillonite is added into deionized water, stirred at 50-60℃ for 20-30min, then KH560 solution is added dropwise, after the dropwise addition is completed, stirring for 3-4h, post-processing, to obtain organic montmorillonite; A2, the organic montmorillonite is added into deionized water, stirred at 20-30℃ for 10-20min, then polyacrylic acid and stannous octoate are added, stirred at 50-60℃ for 3-4h, post-processing, to obtain modified montmorillonite.

7. The method of claim 6, wherein the method further comprises the step of applying a water repellent agent to the outer surface of the fabric.

8. The method of claim 6, wherein the method further comprises the step of applying a water repellent agent to the outer surface of the fabric. In step A1, the use amount ratio of the montmorillonite, deionized water and KH560 solution is 1g:19mL:3mL, the KH560 solution is prepared by dissolving 1.5g KH560 in 30mL 90wt% ethanol solution, then adding acetic acid to adjust the pH to 4-5, stirring for 20-30min; in step A2, the use amount ratio of the organic montmorillonite, deionized water, polyacrylic acid solution and stannous octoate is 1g:15mL:0.4g:0.015g.

8. The method for preparing a warm, breathable, and cold-resistant cotton-padded composite fabric according to claim 1, characterized in that, In step S2, the preparation method of the dopamine solution is as follows: dopamine hydrochloride, sodium carbonate, deionized water and 1,4-dioxane are added into a reaction kettle, stirred at 20-30℃ for 20-30min, to obtain a dopamine solution; the use amount ratio of the dopamine hydrochloride, sodium carbonate, deionized water and 1,4-dioxane is 2-2.2g:1.1g:12mL:12mL.

9. The method for preparing a warm, breathable, and cold-resistant cotton-padded composite fabric according to claim 1, characterized in that, In step S2, the reflux treatment includes: the drawn fiber is immersed into the dopamine solution, refluxed at 100-110℃ under nitrogen atmosphere for 20-22h, after the reaction is completed, the fiber is taken out, washed with distilled water at 70-80℃, then refluxed in 80℃ ethanol for 5-6h, taken out, dried at 60℃ under vacuum for 12h, to obtain acrylic fiber; the use amount ratio of the drawn fiber and the dopamine solution is 1g:25mL.

10. A cold protective, moisture permeable, cotton clothing composite fabric, characterized by, The warm and moisture-permeable cotton coat composite fabric is prepared by the cotton coat composite fabric preparation process according to any one of claims 1-9.

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