Comfortable and breathable textile fabric and preparation method thereof

Abstract

The invention relates to the technical field of multi-layer composite fabrics, and discloses a comfortable and breathable textile fabric and a preparation method thereof.Based on the Mannich reaction mechanism, 1, 3-bis (3-aminopropyl) tetramethyldisiloxane, vanillin and phosphorous acid serve as raw materials, and a vanillin-based nitrogen-phosphorus-silicon flame-retardant monomer is prepared; then preparing two efficient flame retardants by taking the vanillin-based nitrogen-phosphorus-silicon flame-retardant monomer as a raw material, and dispersing the flame retardants in deionized water to obtain a flame-retardant finishing solution; putting a chinlon fabric into the flame-retardant finishing liquid for dipping treatment, taking out and drying to obtain a flame-retardant chinlon fabric, and finally preparing the textile fabric by taking the flame-retardant chinlon fabric as an outer layer and taking a comfortable and breathable cotton fabric as an inner layer through a polyurethane resin adhesive lamination compounding process. The textile fabric prepared by the invention has good comfortable air permeability and flame retardant property.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of multi-layer composite fabrics, in particular to a comfortable and breathable textile fabric and a preparation method thereof. BACKGROUND

[0002] The material of the textile fabric includes cotton fabric, polyester fabric, nylon fabric, etc. In the fields of fire protection, industry, energy, etc., employees often work in various extreme environments such as high temperature, open fire, electric arc, etc. Fabrics with flame-retardant function are of great significance in protecting the safety of workers. At the same time, the comfort and breathability of the fabric are also crucial. It can effectively remove sweat and moisture, avoid stuffiness and stickiness, reduce skin irritation and allergy risk, and improve the wearing experience.

[0003] Among them, nylon fabric is widely used in protective clothing, carpets, safety airbags, military clothing, etc. due to its excellent mechanical properties, wear resistance, easy dyeing, and good elastic recovery. However, the limiting oxygen index of nylon is only about 23%, and it will produce high-temperature molten droplets during combustion, causing secondary fire damage to human skin and possibly causing the spread of fire.

[0004] Research has found that the flame-retardant properties of nylon fabric can be improved through blending modification, copolymerization modification, and coating finishing methods. Among them, the coating finishing method has the characteristics of simple process, strong compatibility, and wide applicability, and has become one of the effective methods to improve the flame-retardant properties of nylon fabric.

[0005] In the prior art, a multi-layer composite structure design is often used to realize the synergistic optimization of fabric flame retardancy, breathability, and comfort through the combination of different functional layers.

[0006] Search found: Jiangnan University published a master's degree thesis by Liang Fuwei in 2023 entitled "Preparation and Performance Research of Flame-retardant Super-hydrophobic Micro-nano Composite Coating Finished Cotton Fabric" through Mannich reaction to prepare a P / N / Si multi-element synergistic flame retardant PPA-POSS. However, in the preparation of vanillin-based nitrogen-phosphorus-silicon flame retardant monomer, the application uses bio-based aromatic compound vanillin as raw material, which has a unique aromatic smell. Its molecular structure contains hydroxyl and aldehyde groups, which makes it have multiple activities in chemical reactions. When applied to fabrics, it will not produce irritating odor, and the hydroxyl groups in its structure can form hydrogen bonds with the amide bonds of nylon fabric, etc., enhancing its flame-retardant and wash-resistant properties, avoiding the washing and peeling of the finishing agent. In addition, graphene can further improve the flame-retardant properties of the fabric. SUMMARY

[0007] The application utilizes the newly developed vanillin-based nitrogen-phosphorus-silicon flame retardant or graphene-based nitrogen-phosphorus-silicon flame retardant to perform flame-retardant modification on the polyamide fabric, and then the flame-retardant polyamide fabric is used as an outer layer, the cotton fabric is used as an inner layer, and a polyurethane resin adhesive is used for laminated composite process to prepare the textile fabric, which has good flame-retardant performance and comfortable and breathable performance.

[0008] To achieve the above-mentioned purpose, the application adopts the following technical scheme: a preparation method of comfortable and breathable textile fabric, comprising the following steps: Step one: based on the Mannich reaction mechanism, vanillin-based nitrogen-phosphorus-silicon flame-retardant monomers are prepared from 1,3-bis(3-aminopropyl)tetramethyldisiloxane, vanillin and phosphorous acid as raw materials; Step two: two kinds of efficient flame retardants are prepared from the vanillin-based nitrogen-phosphorus-silicon flame-retardant monomers as raw materials, the flame retardants are dispersed in deionized water to obtain a flame-retardant finishing liquid; The two kinds of efficient flame retardants are vanillin-based nitrogen-phosphorus-silicon flame retardants and graphene-based nitrogen-phosphorus-silicon flame retardants; Step three: the polyamide fabric is immersed in the flame-retardant finishing liquid for treatment, taken out and dried to obtain a flame-retardant polyamide fabric, the flame-retardant polyamide fabric is used as an outer layer, the comfortable and breathable cotton fabric is used as an inner layer, and a polyurethane resin adhesive is used for laminated composite process to prepare the textile fabric.

[0009] Further, the preparation method of the vanillin-based nitrogen-phosphorus-silicon flame retardant is as follows: based on the Mannich reaction mechanism, the vanillin-based nitrogen-phosphorus-silicon flame retardant is prepared from the vanillin-based nitrogen-phosphorus-silicon flame-retardant monomers, vanillin and phosphorous acid as raw materials.

[0010] Further, the preparation method of the graphene-based nitrogen-phosphorus-silicon flame retardant is as follows: Step S1: based on the amine-alkene reaction mechanism, the imino group in the vanillin-based nitrogen-phosphorus-silicon flame-retardant monomers reacts with the alpha, beta-unsaturated alkene functional group in 3-(methacryloyloxy)propyl trimethoxysilane to prepare a nitrogen-phosphorus-silicon flame-retardant silane coupling agent; Step S2: the graphene is modified by the nitrogen-phosphorus-silicon flame-retardant silane coupling agent to prepare the graphene-based nitrogen-phosphorus-silicon flame retardant.

[0011] Further, in the laminated composite process, the sizing amount of the polyurethane resin adhesive is 15-25 g / m 2 , the pressing temperature is 110-120℃, the composite pressure is 3-5kgf / cm 2 , and the laminating time is 3-8s.

[0012] Further, the structure of the textile fabric is an outer layer of flame-retardant polyamide fabric / adhesive layer / inner layer of cotton fabric.

[0013] The application has the following beneficial effects: The application is based on a Mannich reaction mechanism, and a novel vanillin-based nitrogen-phosphorus-silicon flame-retardant monomer is synthesized; then two efficient flame retardants (specifically, vanillin-based nitrogen-phosphorus-silicon flame retardants and graphene-based nitrogen-phosphorus-silicon flame retardants) are prepared through the Mannich reaction of the vanillin-based nitrogen-phosphorus-silicon flame-retardant monomer and / or modification of graphene; then the polyamide fabric is immersed in a flame-retardant finishing liquid prepared from the flame retardants; finally, a flame-retardant comfortable and breathable textile fabric is prepared through a polyurethane resin adhesive lamination composite process, with the flame-retardant polyamide fabric as an outer layer and cotton fabric as an inner layer. The experimental results show that the textile fabric prepared by the application is not only comfortable and breathable, but also has good flame-retardant performance. DETAILED DESCRIPTION

[0014] In order to improve the flame-retardant performance of the textile fabric, the application independently develops a vanillin-based nitrogen-phosphorus-silicon flame-retardant monomer, and two efficient flame retardants are synthesized using the vanillin-based nitrogen-phosphorus-silicon flame-retardant monomer as a raw material, and the polyamide fabric is modified by the two efficient flame retardants, which significantly improves the flame-retardant performance of the textile fabric. Example 1

[0015] The vanillin-based nitrogen-phosphorus-silicon flame-retardant monomer is prepared, and the preparation mechanism is as follows: 1,3-bis(3-aminopropyl)tetramethyldisiloxane, vanillin and phosphorous acid are used as raw materials, and the vanillin-based nitrogen-phosphorus-silicon flame-retardant monomer is prepared through a Mannich reaction, and the specific experimental steps are as follows: 2.4g of 1,3-bis(3-aminopropyl)tetramethyldisiloxane and 50mL of N,N-dimethylacetamide are added to a three-necked flask equipped with a mechanical stirrer, a condensation reflux device, and mixed, and heated to 40℃ in an oil bath, then 3.1g of vanillin is added, and reacted for 20min, 1.64g of phosphorous acid is dissolved in 30mL of deionized water to obtain an aqueous phosphorous acid solution, and then the aqueous phosphorous acid solution is added to the three-necked flask, and the temperature of the system is increased to 70℃, and reacted for 12h, after the reaction is completed, the product is treated by dialysis and rotary evaporation to obtain the vanillin-based nitrogen-phosphorus-silicon flame-retardant monomer. The chemical structural formula of the vanillin-based nitrogen-phosphorus-silicon flame-retardant monomer is as follows: ; The hydrogen nuclear magnetic resonance spectrum of the vanillin-based nitrogen-phosphorus-silicon flame-retardant monomer is as follows: 1 H NMR(DMSO-d6, 400MHz) δ: 0.09(s, 12H), 0.72-0.78(m, 4H), 1.43-1.49(m, 4H), 2.76-2.85(m, 4H), 3.81(s, 6H), 4.61-4.65(m, 2H), 5.13-5.17(m, 2H), 6.81-6.82(d, 2H), 7.04-7.10(m, 4H), 8.52-8.56(d, 6H). Example 2:

[0016] The preparation mechanism of the vanillin-based nitrogen-phosphorus-silicon flame retardant is as follows: vanillin-based nitrogen-phosphorus-silicon flame retardant monomer, vanillin and phosphorous acid are used as raw materials, and the vanillin-based nitrogen-phosphorus-silicon flame retardant is prepared by Mannich reaction. The specific experimental steps are as follows: 3g of vanillin-based nitrogen-phosphorus-silicon flame retardant is added to 50mL of N,N-dimethylacetamide, the temperature is raised to 40℃, 1.4g of vanillin is added, and the reaction is stirred for 20min. 0.8g of phosphorous acid is dissolved in 20mL of deionized water to obtain an aqueous phosphorous acid solution, which is then added to the above system, the temperature is raised to 70℃, and the reaction is carried out for 12h. After the solvent is removed by rotary evaporation, filtration, washing and drying at 80℃ for 8h, the vanillin-based nitrogen-phosphorus-silicon flame retardant is prepared. The chemical structural formula of the vanillin-based nitrogen-phosphorus-silicon flame retardant is: ; The proton nuclear magnetic resonance spectrum of the vanillin-based nitrogen-phosphorus-silicon flame retardant monomer is as follows: 1 H NMR(DMSO-d6, 400MHz)δ:0.09(s, 12H), 0.73-0.77(t, 4H), 1.44-1.50(m, 4H), 2.67-2.70(t, 4H), 3.81-3.84(d, 12H), 4.53-4.55(d, 2H), 4.69-4.71(d, 2H), 6.46(d, 2H), 6.56-6.58(m, 2H), 6.79-6.82(d, 2H), 7.02(m, 2H), 7.08-7.11(m, 2H), 7.30-7.32(d, 2H), 8.02(s, 4H), 8.52(s, 2H), 8.59(s, 4H), 9.90(s, 2H). Example Three:

[0017] The preparation of graphene-based nitrogen-phosphorus-silicon flame retardant includes the following steps: Step S1: Preparation of nitrogen-phosphorus-silicon flame-retardant silane coupling agent, the preparation mechanism is as follows: based on the amine-alkene reaction mechanism, the imino group in the vanillin-based nitrogen-phosphorus-silicon flame retardant monomer reacts with the α,β-unsaturated alkene functional group in 3-(methacryloyloxy) propyl trimethoxysilane to prepare a nitrogen-phosphorus-silicon flame-retardant silane coupling agent. The specific experimental steps are as follows: 3g of vanillin-based nitrogen-phosphorus-silicon flame retardant monomer is placed in 50mL of acetone, mixed uniformly, 2.2g of 3-(methacryloyloxy) propyl trimethoxysilane is added, and the reaction is stirred at room temperature for 24h. The acetone is removed by rotary evaporation, filtered, washed, and dried in a vacuum drying oven at 80℃ for 6h to prepare the nitrogen-phosphorus-silicon flame-retardant silane coupling agent. The chemical structural formula of the nitrogen-phosphorus-silicon flame-retardant silane coupling agent is: ; The hydrogen nuclear magnetic resonance spectrum of the nitrogen-phosphorus-silicon flame-retardant silane coupling agent is as follows: 1 H NMR (DMSO-d6, 400 MHz) δ: 0.09 (s, 12H), 0.70-0.75 (m, 8H), 1.10-1.11 (d, 6H), 1.42-1.49 (m, 4H), 1.76-1.83 (m, 4H), 2.54-2.57 (m, 4H), 2.65-2.73 (m, 2H), 2.75-2.96 (dd, 4H), 3.56 (s, 18H), 3.81 (s, 6H), 4.07-4.12 (m, 6H), 6.79-6.80 (d, 2H), 6.96-6.97 (d, 2H), 7.07-7.09 (d, 2H), 8.50 (s, 4H), 8.52 (s, 2H); Step S2: preparation of graphene-based nitrogen-phosphorus-silicon flame retardant, its preparation mechanism is: using nitrogen-phosphorus-silicon flame-retardant silane coupling agent to modify graphene, graphene-based nitrogen-phosphorus-silicon flame retardant is prepared, the specific experimental steps are as follows: 2g graphene is added to 50mL mixed acid (the volume ratio of concentrated nitric acid and concentrated sulfuric acid is 3:1), stirred for 6h, cooled and diluted with deionized water, filtered, washed, and the product is dried in a freeze dryer for 24h to obtain acidified graphene; 2.5g of nitrogen-phosphorus-silicon flame-retardant silane coupling agent is added to 100mL deionized water, the pH value of the system is adjusted to 4 using glacial acetic acid, mixed, 3g of acidified graphene is added, stirred for 8h, then filtered, washed, and dried at 80℃ for 10h to prepare graphene-based nitrogen-phosphorus-silicon flame retardant. Example Four:

[0018] (1) Preparation of textile fabric A, including the following steps: Step 1: 15g of vanillin-based nitrogen-phosphorus-silicon flame retardant is dissolved in 100mL deionized water to obtain a flame-retardant finishing liquid, then the nylon fabric (purchased from Suzhou Changjiang Textile Technology Co., Ltd.) is immersed in the flame-retardant finishing liquid at a bath ratio of nylon fabric: flame-retardant finishing liquid = 1:50 for 30min, after the immersion is completed, the fabric is dried in an oven at 60℃ for 1h to obtain a flame-retardant nylon fabric; Step 2: using the flame-retardant nylon fabric as the outer layer and the comfortable and breathable cotton fabric (purchased from Jinzhou Xinteng Textile Sales Place) as the inner layer, a lamination composite process is carried out by using polyurethane resin adhesive, wherein the glue amount is 20g / m 2 , the pressing temperature is 115℃, the composite pressure is 4kgf / cm 2 , the lamination time is 5s, and the textile fabric A is prepared.

[0019] (2) Preparation of textile fabric B: only use graphene-based nitrogen-phosphorus-silicon flame retardant instead of vanillin-based nitrogen-phosphorus-silicon flame retardant in textile fabric A, the rest is the same as textile fabric A, to prepare textile fabric B.

[0020] (3) Preparation of textile fabric C: the difference between it and textile fabric A is only that no flame-retardant finishing liquid is used. Performance test:

[0021] ①According to GB / T 5454-1997 "Textiles - Determination of the limiting oxygen index", the limiting oxygen index of textile fabric A, textile fabric B and textile fabric C is measured by ZR-1 oxygen index tester, the flame retardant performance of the fabric is evaluated, textile fabric A, textile fabric B and textile fabric C are washed according to GB / T 8629-2017 "Textiles - Domestic washing and drying procedures", after drying, the limiting oxygen index of the fabric is measured again to evaluate its flame retardant washing resistance, the size of the fabric is 150mm x 58mm, the specific test results are shown in Table 1; ②According to GB / T 5453-1997 "Textiles - Determination of the air permeability of fabrics", the air permeability of textile fabric A, textile fabric B and textile fabric C is tested by YG461E air permeability tester, the air permeability of the fabric is evaluated, the test area of the fabric is 20cm 2 , the constant test pressure difference is 200Pa, the specific test results are shown in Table 1; Table 1 Performance test results From the data in Table 1, compared with textile fabric C, the limiting oxygen index of textile fabric A and textile fabric B prepared by the present application is greater than 32%, after washing for 20 times, the limiting oxygen index of the fabric decreases slightly, but the increase is small, so it is known that impregnating the flame-retardant finishing liquid on the surface of the nylon fabric can significantly improve the flame-retardant performance of the fabric, and by designing the cotton fabric air permeable layer, the fabric is given good air permeability; ④According to GB / T 18318.1-2009 "Textiles - Determination of the bending properties - Part 1: inclined method", the bending stiffness of textile fabric A, textile fabric B and textile fabric C is tested by electronic stiffness tester BY-01C, the comfort performance of the fabric is evaluated, the specific test results are shown in Table 2; Table 2 Comfort performance test results From the data in Table 2, it can be concluded that the textile fabric prepared by the present application has small bending stiffness and good softness, so it is known that using cotton fabric as the inner layer makes the prepared textile fabric have good comfort performance.

Claims

1. A method for preparing a comfortable and breathable textile fabric, characterized in that, Includes the following steps: Step 1: Based on the Mannich reaction mechanism, vanillin-based nitrogen-phosphorus-silicon flame retardant monomers were prepared using 1,3-bis(3-aminopropyl)tetramethyldisiloxane, vanillin, and phosphorous acid as raw materials. Step 2: Two high-efficiency flame retardants were prepared using vanillin-based nitrogen-phosphorus-silicon flame retardant monomers as raw materials. The flame retardants were dispersed in deionized water to obtain a flame retardant finishing liquid. Two of the high-efficiency flame retardants are vanillin-based nitrogen-phosphorus-silicon flame retardant and graphene-based nitrogen-phosphorus-silicon flame retardant; Step 3: Immerse the nylon fabric in a flame-retardant finishing solution, remove and dry to obtain a flame-retardant nylon fabric. Use the flame-retardant nylon fabric as the outer layer and the comfortable and breathable cotton fabric as the inner layer, and then use a polyurethane resin adhesive lamination process to obtain a textile fabric.

2. The method for preparing a comfortable and breathable textile fabric according to claim 1, characterized in that, The chemical structural formula of the vanillin-based nitrogen-phosphorus-silicon flame retardant monomer is: 。 3. The method for preparing a comfortable and breathable textile fabric according to claim 1, characterized in that, The chemical structural formula of the vanillin-based nitrogen-phosphorus-silicon flame retardant is: 。 4. The method for preparing a comfortable and breathable textile fabric according to claim 1, characterized in that, The chemical structural formula of the graphene-based nitrogen-phosphorus-silicon flame retardant is as follows: 。 5. The method for preparing a comfortable and breathable textile fabric according to claim 1, characterized in that, The preparation method of the vanillin-based nitrogen-phosphorus-silicon flame retardant is as follows: based on the Mannich reaction mechanism, the vanillin-based nitrogen-phosphorus-silicon flame retardant monomer, vanillin and phosphorous acid are used as raw materials to prepare the vanillin-based nitrogen-phosphorus-silicon flame retardant.

6. The method for preparing a comfortable and breathable textile fabric according to claim 1, characterized in that, The preparation method of the graphene-based nitrogen-phosphorus-silicon flame retardant is as follows: Step S1: Based on the amine-olefin reaction mechanism, the imino group in the vanillin-based nitrogen-phosphorus-silicon flame retardant monomer reacts with the α,β-unsaturated alkenyl functional group in 3-(methacryloyloxy)propyltrimethoxysilane to prepare a nitrogen-phosphorus-silicon flame retardant silane coupling agent. Step S2: Graphene is modified using a nitrogen-phosphorus-silicon flame-retardant silane coupling agent to prepare a graphene-based nitrogen-phosphorus-silicon flame retardant.

7. The method for preparing a comfortable and breathable textile fabric according to claim 1, characterized in that, In the lamination process, the amount of polyurethane resin adhesive applied is 15-25 g / m³. 2 The pressing temperature is 110-120℃, and the composite pressure is 3-5 kgf / cm. 2 The lamination time is 3-8 seconds.

8. A comfortable and breathable textile fabric prepared by the method according to any one of claims 1-7, characterized in that, The structure of the textile fabric is an outer flame-retardant nylon fabric / adhesive layer / inner cotton fabric.

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