Self-cleaning wash-free fabric and preparation method thereof
By modifying cotton fabric and coating it with modified epoxy resin, the problems in the fabric cleaning process were solved, achieving self-cleaning, antibacterial and UV-resistant effects, and improving the fabric's waterproof, oil-proof and antistatic properties.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-04
- Publication Date
- 2026-04-07
AI Technical Summary
Existing fabrics are prone to pilling or deformation during cleaning, affecting aesthetics and comfort. Washing also wastes water and energy, and chemical detergents pollute the environment and lack self-cleaning, UV protection, and antibacterial properties.
By modifying cotton fabric and coating it with modified epoxy resin, a modified fabric with self-cleaning, antibacterial and UV-resistant properties is formed through the reaction of chemicals such as malic acid, maleic anhydride, sodium bisulfite, 2-hydroxylauric acid, and R-aminoethyl-B-aminopropyltrimethoxysilane.
It achieves a self-cleaning effect on the fabric, improves antistatic properties, enhances dust resistance, reduces surface energy, has good waterproof and oil-proof properties, and is also UV resistant and antibacterial.
Smart Images
Figure BDA0004209136020000111 
Figure BDA0004209136020000121
Abstract
Description
Technical Field
[0001] This invention relates to the field of fabric technology, specifically to a self-cleaning, wash-free fabric and its preparation method. Background Technology
[0002] With the improvement of people's material and cultural living standards, the heat-insulating function of fabrics is no longer sufficient to meet people's needs. In order to meet people's increasingly diverse requirements for the performance of textiles, different textile technologies are used to endow fabrics with different functions. Since ultraviolet rays are ubiquitous in daily life, a small amount of ultraviolet rays can have beneficial effects on the human body, but a large amount of ultraviolet rays can disrupt the immune system and reduce the body's immune function. In addition, people inevitably come into contact with various bacteria, fungi and other microorganisms in their lives. Under suitable external conditions, these microorganisms can multiply rapidly and spread diseases through contact and other means, affecting people's health and normal work, study and life.
[0003] Meanwhile, fabrics often need to be washed for cleaning, and frequent washing can easily cause pilling or deformation, affecting both appearance and comfort. Furthermore, garment washing results in a significant waste of water and energy, and chemical detergents also pollute the environment. Therefore, there is an urgent need to develop a fabric with self-cleaning properties, UV resistance, and antibacterial properties. Summary of the Invention
[0004] The purpose of this invention is to provide a self-cleaning, wash-free fabric and its preparation method to solve the problems existing in the prior art.
[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution: a self-cleaning, wash-free fabric, wherein the self-cleaning, wash-free fabric is obtained by coating modified cotton fabric with modified epoxy resin coating.
[0006] Furthermore, the modified cotton fabric is prepared from malic acid, cotton fabric, maleic anhydride, sodium bisulfite, 2-hydroxylauric acid, R-aminoethyl-B-aminopropyltrimethoxysilane, perfluorooctyltrimethoxysilane, and hexamethyldisiloxane.
[0007] Furthermore, the modified epoxy resin is prepared from E-44 epoxy resin, 3-amino-4-nitrobenzaldehyde, 3,4-diaminophenylacetone, hydroxylamine hydrochloride, and 2-bromoethanol.
[0008] Furthermore, a method for preparing a self-cleaning, wash-free fabric includes the following preparation steps:
[0009] (1) Mix the pretreated fabric, maleic anhydride, concentrated sulfuric acid, and toluene in a mass ratio of 1:1.1:0.05:3 to 1:1.8:0.05:6. After reacting at 70°C for 3 to 5 hours, remove the mixture and wash it with chloroform and deionized water 5 times in sequence. Then add sodium bisulfite at 0.3 to 0.4 times the mass of the pretreated fabric and isopropanol aqueous solution at 3 to 5 times the mass of the pretreated fabric. The mass ratio of isopropanol to deionized water in the isopropanol aqueous solution is 3.9:1. After reacting at 80 to 88°C for 6 hours, add sodium bisulfite at 0.2 times the mass of the pretreated fabric and continue reacting for 6 hours. Remove the mixture and wash it with methanol aqueous solution and petroleum ether 4 times in sequence. The mass ratio of methanol to deionized water in the methanol aqueous solution is 3.2:1 to obtain sulfonated fabric.
[0010] (2) The sulfonated fabric, 2-hydroxylauric acid, iodine, p-toluenesulfonic acid, ethanol and deionized water are mixed in a mass ratio of 1:1.5:0.9:0.4:2:1 to 1:2.4:1.3:0.4:5:1. The mixture is reacted at 100 rpm and 60°C for 90 to 120 minutes. After cooling to room temperature, it is taken out and washed with saturated saline solution until the pH of the washing solution is 7 to obtain lauryl ester fabric.
[0011] (3) Mix lauryl ester fabric and N-methylpyrrolidone in a mass ratio of 1:4 to 1:6. Under an ice-water bath, add 0.8 to 0.9 times the mass of lauryl ester fabric with oxaloyl chloride. Stir at 10°C and 80 rpm for 50 to 70 minutes. Then add 0.8 to 0.9 times the mass of lauryl ester fabric with R-aminoethyl-B-aminopropyltrimethoxysilane. React at 35 to 40°C for 4 hours. Remove the product and wash it 6 times with distilled water and ethyl acetate, and then wash it 3 times with saturated saline solution to obtain silane fabric.
[0012] (4) Mix silane fabric, perfluorooctyltrimethoxysilane, potassium hydroxide and ethanol in a mass ratio of 1:0.8:0.1:3 to 1:1.2:0.1:5, heat to 70 to 84°C, add hexamethyldisiloxane in 0.8 to 1.4 times the mass of silane fabric, react for 4 hours, take it out, dry it under vacuum of 100 kPa and 90°C for 1 to 3 hours to obtain modified cotton fabric;
[0013] (5) Anhydrous potassium phosphate, potassium iodide, intermediate C, 2-bromoethanol, and acetonitrile were mixed in a mass ratio of 0.8:0.6:1:0.4:10 to 0.9:0.7:1:0.6:10 and heated to 85°C. After reacting for 5 to 7 hours, the mixture was filtered and the filtrate was distilled at 200 to 300 rpm and 85°C for 3 to 5 hours. Then, 8.6 times the mass of intermediate C in deionized water was added and stirred until homogeneous. The ethyl acetate layers were extracted with ethyl acetate and combined. The mixture was dried with anhydrous sodium sulfate for 1 hour and then distilled at 85°C for 1 to 2 hours to obtain the oxime ether compound.
[0014] (6) E-44 epoxy resin, ethylene glycol monobutyl ether, and ethanol are mixed in a mass ratio of 1:4:1.7 to 1:6:2.6. Under nitrogen protection, the mixture is heated to 80°C and stirred until dissolved. Then, 0.3 to 0.5 times the mass of E-44 epoxy resin oxime ether compound is added. After reacting for 12 to 14 hours, the mixture is filtered and washed five times with ethanol and water. The mixture is then dried at 50°C under a vacuum of -0.08 MPa for 48 hours to obtain the modified epoxy resin.
[0015] (7) Mix modified epoxy resin, polyvinyl alcohol and ethanol in a mass ratio of 30:3:5 to 40:5:10, stir at 100 to 130°C and 300 rpm for 30 min, then cool to 40 to 50°C, add 0.06 to 0.2 times the mass of modified epoxy resin of polyamide 650 and 0.06 to 0.1 times the mass of modified epoxy resin of accelerator, stir at 5000 rpm for 10 min to obtain modified epoxy resin coating; apply 0.08 to 0.2 times the mass of modified cotton fabric of modified epoxy resin coating to modified cotton fabric, dry at 80°C for 8 h to obtain self-cleaning and wash-free fabric.
[0016] Furthermore, the preparation method of the pretreated fabric in step (1) is as follows: a fabric with a weight of 120-160 g / m² is prepared. 2 The cotton fabric is immersed in an acid solution at a ratio of 1:10 to 1:20 for 10 to 20 minutes. After immersion, it is subjected to one dip and two nipping processes, with a nipping rate of 75 to 80% each time. After pre-drying at 70 to 80°C for 20 minutes, it is baked at 130 to 140°C for 30 minutes to obtain the pretreated fabric.
[0017] Furthermore, the acid solution contains malic acid, disodium hydrogen phosphate, and deionized water in a mass ratio of 10:5:85.
[0018] Further, the intermediate C in step (5) is prepared by mixing benzotriazole compound, hydroxylamine hydrochloride and ethanol in a mass ratio of 1:0.2:11 to 1:0.3:11, reacting at 80°C for 3 to 4 hours, cooling to room temperature, filtering and taking the filtrate, distilling at -0.08 MPa and 40°C for 60 to 70 minutes, adding 9 times the mass of deionized water of benzotriazole compound, mixing evenly, extracting with ethyl acetate, combining the ethyl acetate layers, drying with anhydrous sodium sulfate for 1 hour, and distilling at 80°C for 1 to 2 hours to obtain intermediate C.
[0019] Furthermore, the method for preparing the benzotriazole compound is as follows:
[0020] a. Mix 3-amino-4-nitrobenzaldehyde, 36% hydrochloric acid, and deionized water in a mass ratio of 1:2.8:2.7 to 1:3.5:2.7. Stir at 60-80 rpm for 30 minutes, then cool to -8°C. Add 1.2-1.6 times the mass of 3-amino-4-nitrobenzaldehyde in a sodium nitrite aqueous solution, with a sodium nitrite to deionized water mass ratio of 8.2:15. React for 20-34 minutes, then add urea to the starch-iodine mixture. The potassium chloride test paper turned slightly blue, indicating intermediate A. Deionized water, sodium carbonate, and 3,4-diaminophenylacetone were mixed in a mass ratio of 8:3:1 to 12:5:1. The mixture was stirred at 60 rpm and at 10 to 15 °C. Then, intermediate A, which was 1 to 2 times the mass of 3,4-diaminophenylacetone, was added at a rate of 0.2 mL / min. The reaction was allowed to proceed for 2 to 3 hours. The solid was then filtered and washed three times with a methanol-water solution in which the mass ratio of methanol to deionized water was 1:19. The solid was dried at 60 °C for 8 hours to obtain intermediate B.
[0021] b. Mix intermediate B, sodium hydroxide, and deionized water in a mass ratio of 1:0.3:0.5 to 1:0.4:0.5. While stirring at 70 rpm, add zinc powder at a rate of 1.0 to 1.3 times the mass of intermediate B at a rate of 1.0 to 1.4 g / min. Simultaneously add sodium hydroxide at a rate of 0.4 to 0.5 times the mass of intermediate B and deionized water at a rate of 1 to 2 times the mass of intermediate B. Heat to 60°C and hold for 1 to 2 hours. Then heat to 70°C and hold for 1 to 2 hours. Cool to room temperature, filter, and collect the filtrate. Add hydrochloric acid to adjust the pH of the filtrate to 1 to 2. Filter to collect the solid, wash with deionized water four times, and dry at 40°C for 10 hours to obtain the benzotriazole compound.
[0022] Furthermore, the promoter in step (7) is 2-ethylimidazole or 4-methylimidazole.
[0023] Further, in step (7), the modified epoxy resin, polyvinyl alcohol, ethanol, polyamide 650, and accelerator are mixed in a mass ratio of 30:3:5:1.8:1.8 to 40:5:10:8:4.
[0024] Compared with the prior art, the beneficial effects achieved by the present invention are:
[0025] This invention first modifies cotton fabric and then coats it with modified epoxy resin to obtain a self-cleaning, wash-free fabric, thereby achieving self-cleaning, antibacterial, and UV-resistant effects.
[0026] First, this invention utilizes the reaction between the carboxyl group of malic acid and the hydroxyl group of cotton fabric to connect the fibers, making the fabric structure more compact. This prevents water, oil, dust, and other impurities from easily penetrating the fabric, thus improving its self-cleaning effect. The hydroxyl group of malic acid reacts with maleic anhydride to generate a carboxyl group. Sodium bisulfite reacts with the double bond, forming a sulfonic acid group-metal ionic bond in the side chain. This bond can dissolve the complex to generate positive and negative ions for ionic conductivity, improving antistatic properties, preventing dust accumulation on the fabric, and enhancing its self-cleaning effect. Finally, the carboxyl group reacts with the hydroxyl group of 2-hydroxylauric acid to generate a lauryl ester group. After chlorination, the carboxyl group of 2-hydroxylauric acid reacts with the amino group of R-aminoethyl-B-aminopropyltrimethoxysilane to generate… Amide groups introduce certain hydrophilic groups, promoting moisture absorption and release of static charge, improving the fabric's dust-repellent effect, and enhancing its self-cleaning properties. R-aminoethyl-B-aminopropyltrimethoxysilane polymerizes with perfluorooctyltrimethoxysilane and hexamethyldisiloxane to form polyorganosiloxane, which exhibits good smoothness in the fabric, effectively reducing dust embedding or snagging, and decreasing dust adhesion. In addition, it works together with the fluorocarbon structure to reduce surface energy and improve the fabric's waterproof and oil-repellent properties. At the same time, long-chain compounds such as lauryl are wrapped around the fiber surface, and the polyorganosiloxane and fluorocarbon compounds away from the fiber surface isolate the fabric from the external environment, enhancing the fabric's self-cleaning effect.
[0027] Secondly, after the amino group of 3-amino-4-nitrobenzaldehyde is diazotized, a chloroazo group is generated. The chloride ion reacts with the aryl group of 3,4-diaminophenylacetone, and the azo group and nitro group form a ring, forming a benzotriazole group. This allows the modified epoxy resin to effectively absorb ultraviolet light, thereby improving the fabric's UV resistance. After the ketone group of 3,4-diaminophenylacetone reacts with hydroxylamine hydrochloride, it reacts with the bromide ion of 2-bromoethanol to generate an oxime ether group. This allows the modified epoxy resin to effectively inhibit bacterial growth, thereby improving the fabric's antibacterial properties. The amino group of 3,4-diaminophenylacetone reacts with the epoxy resin to obtain a modified epoxy resin. When coated on the surface of the modified fabric, the aldehyde group of the modified epoxy resin reacts with the amino group of the modified fabric, allowing the resin to adhere tightly to the fiber surface. While enhancing the effect, a Schiff base structure is generated, which works together with the oxime ether group to improve the fabric's antibacterial properties. Detailed Implementation
[0028] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0029] To more clearly illustrate the method provided by the present invention, the following embodiments are provided in detail. The test methods for various indicators of the self-cleaning, wash-free fabric produced in the following embodiments are as follows:
[0030] Self-cleaning: Take the same size of the example and comparative examples, fold them into 2 layers, rub them 20 times with a paper tube wrapped with plastic, and quickly cover the top of a cardboard box containing fresh cigarette ash. Observe the phenomenon of the fabric absorbing cigarette ash. Measure the water repellency level according to GB / T 4745, test the oil repellency level according to GB / T 19977, and test the stain resistance level according to GB / T 30159.
[0031] UV resistance: The transmittance of the same size sample in the example and comparative examples was tested on a HITACHI-3310 UV-Vis spectrophotometer between 290 and 400 nm. Data was recorded every 5 nm. The UVA and UVB of the UV-resistant and breathable composite fabric were determined according to the transmittance T calculation formula in GB / T18830, and then the UPF value was obtained.
[0032] Antibacterial: The antibacterial rates of Escherichia coli and Staphylococcus aureus were tested using examples and comparative samples of the same size according to GB / T 20944.3.
[0033] Example 1
[0034] (1) The weight is 120g / m 2 The cotton fabric was immersed in an acid solution at a ratio of 1:10. The mass ratio of malic acid, disodium hydrogen phosphate and deionized water in the acid solution was 10:5:85. After immersion for 10 minutes, the fabric was subjected to one immersion and two nipping processes with a nipping rate of 75% each time. After pre-drying at 70℃ for 20 minutes, the fabric was baked at 130℃ for 30 minutes to obtain the pretreated fabric.
[0035] (2) The pretreated fabric, maleic anhydride, concentrated sulfuric acid and toluene were mixed in a mass ratio of 1:1.1:0.05:3. After reacting at 70°C for 3 hours, the mixture was removed and washed with chloroform and deionized water 5 times in sequence. Then, sodium bisulfite (0.3 times the mass of the pretreated fabric) and isopropanol aqueous solution (3 times the mass of the pretreated fabric) were added. The mass ratio of isopropanol to deionized water in the isopropanol aqueous solution was 3.9:1. After reacting at 80°C for 6 hours, sodium bisulfite (0.2 times the mass of the pretreated fabric) was added. After reacting for another 6 hours, the mixture was removed and washed with methanol aqueous solution and petroleum ether 4 times in sequence. The mass ratio of methanol to deionized water in the methanol aqueous solution was 3.2:1. The sulfonated fabric was obtained.
[0036] (3) The sulfonated fabric, 2-hydroxylauric acid, iodine, p-toluenesulfonic acid, ethanol and deionized water were mixed in a mass ratio of 1:1.5:0.9:0.4:2:1. After reacting at 100 rpm and 60°C for 90 min, the mixture was cooled to room temperature, removed and washed with saturated saline solution until the pH of the washing solution was 7 to obtain lauryl ester fabric.
[0037] (4) Mix lauryl ester fabric and N-methylpyrrolidone at a mass ratio of 1:4. Under ice-water bath, add 0.8 times the mass of lauryl ester fabric with oxaloyl chloride. Stir at 10℃ and 80 rpm for 50 min. Then add 0.8 times the mass of lauryl ester fabric with R-aminoethyl-B-aminopropyltrimethoxysilane. React at 35℃ for 4 h. Remove the product and wash it 6 times with distilled water and ethyl acetate, and then wash it 3 times with saturated saline solution to obtain silane fabric.
[0038] (5) Mix silane fabric, perfluorooctyltrimethoxysilane, potassium hydroxide and ethanol in a mass ratio of 1:0.8:0.1:3, heat to 70°C, add hexamethyldisiloxane in 0.8 times the mass of silane fabric, react for 4 hours, take it out, dry it under vacuum of 100 kPa and 90°C for 1 hour to obtain modified cotton fabric.
[0039] (6) Mix 3-amino-4-nitrobenzaldehyde, 36% hydrochloric acid, and deionized water in a mass ratio of 1:2.8:2.7. Stir at 60 rpm for 30 min, cool to -8℃, and add 1.2 times the mass of sodium nitrite aqueous solution of 3-amino-4-nitrobenzaldehyde. The mass ratio of sodium nitrite to deionized water in the sodium nitrite aqueous solution is 8.2:15. After reacting for 20 min, add urea until starch-potassium iodide test paper turns slightly blue to obtain intermediate A. Mix deionized water, sodium carbonate, and 3,4-diaminophenylacetone in a mass ratio of 8:3:1. Stir at 60 rpm and at 10℃, add 1 times the mass of intermediate A of 3,4-diaminophenylacetone at 0.2 mL / min. React for 2 h, filter to obtain solid, wash 3 times with methanol aqueous solution. The mass ratio of methanol to deionized water in the methanol aqueous solution is 1:19. Dry at 60℃ for 8 h to obtain intermediate B.
[0040] (7) Mix intermediate B, sodium hydroxide, and deionized water in a mass ratio of 1:0.3:0.5. Stir at 70 rpm, add zinc powder at a mass of 1 g / min equal to that of intermediate B, and add sodium hydroxide at a mass of 0.4 times that of intermediate B and deionized water at a mass of 1 times that of intermediate B. Heat to 60°C and keep warm for 1 h, then heat to 70°C and keep warm for 1 h. Cool to room temperature, filter and collect the filtrate, add hydrochloric acid until the pH of the filtrate is 1, filter and collect the solid, wash with deionized water 4 times, and dry at 40°C for 10 h to obtain benzotriazole compound;
[0041] (8) Mix benzotriazole compound, hydroxylamine hydrochloride and ethanol at a mass ratio of 1:0.2:11, react at 80℃ for 3h, cool to room temperature, filter and collect the filtrate, distill at -0.08MPa and 40℃ for 60min, add 9 times the mass of deionized water of benzotriazole compound, mix well, extract with ethyl acetate, combine the ethyl acetate layers, dry with anhydrous sodium sulfate for 1h, and distill at 80℃ for 1h to obtain intermediate C;
[0042] (9) Anhydrous potassium phosphate, potassium iodide, intermediate C, 2-bromoethanol and acetonitrile were heated to 85°C in a mass ratio of 0.8:0.6:1:0.4:10 and reacted for 5 hours. The filtrate was filtered and distilled at 200 rpm and 85°C for 3 hours. Deionized water with a mass of 8.6 times that of intermediate C was added and stirred evenly. The ethyl acetate layers were extracted with ethyl acetate and combined. The mixture was dried with anhydrous sodium sulfate for 1 hour and distilled at 85°C for 1 hour to obtain the oxime ether compound.
[0043] (10) E-44 epoxy resin, ethylene glycol monobutyl ether and ethanol were mixed in a mass ratio of 1:4:1.7. Under nitrogen protection, the mixture was heated to 80°C and stirred until dissolved. Then, 0.3 times the mass of E-44 epoxy resin oxime ether compound was added. After reacting for 12 hours, the mixture was filtered and washed with ethanol and water five times in sequence. The mixture was then dried at 50°C under a vacuum of -0.08 MPa for 48 hours to obtain the modified epoxy resin.
[0044] (11) Mix modified epoxy resin, polyvinyl alcohol and ethanol in a mass ratio of 30:3:5, stir at 100℃ and 300rpm for 30min, cool down to 40℃, add polyamide 650 at 0.06 times the mass of modified epoxy resin and 2-ethylimidazole at 0.06 times the mass of modified epoxy resin, stir at 5000rpm for 10min to obtain modified epoxy resin coating; apply modified epoxy resin coating at 0.08 times the mass of modified cotton fabric to modified cotton fabric, dry at 80℃ for 8h to obtain self-cleaning no-wash fabric.
[0045] Example 2
[0046] (1) The weight is 140g / m 2 The cotton fabric was immersed in an acid solution at a ratio of 1:15. The mass ratio of malic acid, disodium hydrogen phosphate and deionized water in the acid solution was 10:5:85. After immersion for 15 minutes, the fabric was subjected to one immersion and two nipping processes with a nipping rate of 78% each time. After pre-drying at 75°C for 20 minutes, the fabric was baked at 135°C for 30 minutes to obtain the pre-treated fabric.
[0047] (2) The pretreated fabric, maleic anhydride, concentrated sulfuric acid and toluene were mixed in a mass ratio of 1:1.14:0.05:4.5 and reacted at 70°C for 4 hours. The mixture was then removed and washed with chloroform and deionized water 5 times in sequence. Then, sodium bisulfite (0.35 times the mass of the pretreated fabric) and isopropanol aqueous solution (4 times the mass of the pretreated fabric) were added. The mass ratio of isopropanol to deionized water in the isopropanol aqueous solution was 3.9:1. The mixture was reacted at 84°C for 6 hours. Then, sodium bisulfite (0.2 times the mass of the pretreated fabric) was added and the mixture was reacted for another 6 hours. The mixture was then removed and washed with methanol aqueous solution and petroleum ether 4 times in sequence. The mass ratio of methanol to deionized water in the methanol aqueous solution was 3.2:1. The sulfonated fabric was obtained.
[0048] (3) The sulfonated fabric, 2-hydroxylauric acid, iodine, p-toluenesulfonic acid, ethanol and deionized water were mixed in a mass ratio of 1:1.9:1.1:0.4:3.5:1. The mixture was reacted at 100 rpm and 60°C for 105 min. After cooling to room temperature, the mixture was taken out and washed with saturated saline solution until the pH of the washing solution was 7 to obtain lauryl ester fabric.
[0049] (4) Mix lauryl ester fabric and N-methylpyrrolidone at a mass ratio of 1:5. Add 0.85 times the mass of lauryl ester fabric with oxaloyl chloride under an ice-water bath. Stir at 10°C and 80 rpm for 60 min. Then add 0.85 times the mass of lauryl ester fabric with R-aminoethyl-B-aminopropyltrimethoxysilane. React at 38°C for 4 h. Remove the product and wash it 6 times with distilled water and ethyl acetate, and then wash it 3 times with saturated saline solution to obtain silane fabric.
[0050] (5) Mix silane fabric, perfluorooctyltrimethoxysilane, potassium hydroxide and ethanol in a mass ratio of 1:1:0.1:4, heat to 77°C, add hexamethyldisiloxane in 1.1 times the mass of silane fabric, react for 4 hours, take out, dry at 90°C under vacuum of 100 kPa for 2 hours to obtain modified cotton fabric.
[0051] (6) Mix 3-amino-4-nitrobenzaldehyde, 36% hydrochloric acid, and deionized water in a mass ratio of 1:3.1:2.7. Stir at 70 rpm for 30 min, cool to -8℃, and add sodium nitrite aqueous solution with a mass ratio of 1.4 times that of 3-amino-4-nitrobenzaldehyde. The mass ratio of sodium nitrite to deionized water in the sodium nitrite aqueous solution is 8.2:15. After reacting for 27 min, add urea until starch-potassium iodide test paper turns slightly blue to obtain intermediate A. Mix deionized water, sodium carbonate, and 3,4-diaminophenylacetone in a mass ratio of 10:4:1. Stir at 60 rpm and at 12℃, add intermediate A with a mass ratio of 0.2 mL / min at 1.5 times that of 3,4-diaminophenylacetone. React for 2.5 h, filter to obtain solid, wash 3 times with methanol aqueous solution with a mass ratio of methanol to deionized water of 1:19, and dry at 60℃ for 8 h to obtain intermediate B.
[0052] (7) Mix intermediate B, sodium hydroxide, and deionized water at a mass ratio of 1:0.35:0.5. Stir at 70 rpm, add zinc powder at a mass of 1.15 times that of intermediate B at a rate of 1.2 g / min, and simultaneously add sodium hydroxide at a mass of 0.45 times that of intermediate B and deionized water at a mass of 1.5 times that of intermediate B. Heat to 60°C and keep warm for 1.5 h, then heat to 70°C and keep warm for 1.5 h. Cool to room temperature, filter and collect the filtrate, add hydrochloric acid until the pH of the filtrate is 1.5, filter and collect the solid, wash with deionized water 4 times, and dry at 40°C for 10 h to obtain benzotriazole compound;
[0053] (8) Mix benzotriazole compound, hydroxylamine hydrochloride and ethanol at a mass ratio of 1:0.25:11, react at 80℃ for 3.5h, cool to room temperature, filter and collect the filtrate, distill at -0.08MPa vacuum and 40℃ for 65min, add 9 times the mass of deionized water of benzotriazole compound, mix well, extract with ethyl acetate, combine the ethyl acetate layers, dry with anhydrous sodium sulfate for 1h, and distill at 80℃ for 1.5h to obtain intermediate C;
[0054] (9) Anhydrous potassium phosphate, potassium iodide, intermediate C, 2-bromoethanol and acetonitrile were heated to 85°C in a mass ratio of 0.85:0.65:1:0.5:10 and reacted for 6 hours. The filtrate was filtered and distilled at 250 rpm and 85°C for 4 hours. Deionized water with a mass of 8.6 times that of intermediate C was added and stirred evenly. The ethyl acetate layers were extracted with ethyl acetate and combined. The mixture was dried with anhydrous sodium sulfate for 1 hour and distilled at 85°C for 1.5 hours to obtain the oxime ether compound.
[0055] (10) E-44 epoxy resin, ethylene glycol monobutyl ether and ethanol were mixed in a mass ratio of 1:5:2.2. Under nitrogen protection, the mixture was heated to 80°C and stirred to dissolve. Then, 0.4 times the mass of the oxime ether compound of E-44 epoxy resin was added. After reacting for 13 hours, the mixture was filtered and washed with ethanol and water five times in sequence. The mixture was then dried at 50°C under a vacuum of -0.08 MPa for 48 hours to obtain the modified epoxy resin.
[0056] (11) Mix modified epoxy resin, polyvinyl alcohol and ethanol in a mass ratio of 35:4:7.5, stir at 115℃ and 300rpm for 30min, cool down to 45℃, add polyamide 650 at 0.13 times the mass of modified epoxy resin and 4-methylimidazole at 0.08 times the mass of modified epoxy resin, stir at 5000rpm for 10min to obtain modified epoxy resin coating; apply modified epoxy resin coating at 0.14 times the mass of modified cotton fabric to modified cotton fabric, dry at 80℃ for 8h to obtain self-cleaning no-wash fabric.
[0057] Example 3
[0058] (1) The weight is 160g / m2 The cotton fabric was immersed in an acid solution at a ratio of 1:20. The mass ratio of malic acid, disodium hydrogen phosphate, and deionized water in the acid solution was 10:5:85. After immersion for 20 minutes, the fabric was subjected to one immersion and two nipping processes, with a nipping rate of 80% each time. After pre-drying at 80℃ for 20 minutes, the fabric was baked at 140℃ for 30 minutes to obtain the pretreated fabric.
[0059] (2) The pretreated fabric, maleic anhydride, concentrated sulfuric acid and toluene were mixed in a mass ratio of 1:1.8:0.05:6 and reacted at 70°C for 5 hours. The mixture was then removed and washed with chloroform and deionized water 5 times in sequence. Sodium bisulfite (0.4 times the mass of the pretreated fabric) and isopropanol aqueous solution (5 times the mass of the pretreated fabric) were then added. The mass ratio of isopropanol to deionized water in the isopropanol aqueous solution was 3.9:1. The mixture was reacted at 88°C for 6 hours. Sodium bisulfite (0.2 times the mass of the pretreated fabric) was then added and the mixture was reacted for another 6 hours. The mixture was then removed and washed with methanol aqueous solution and petroleum ether 4 times in sequence. The mass ratio of methanol to deionized water in the methanol aqueous solution was 3.2:1. The sulfonated fabric was obtained.
[0060] (3) The sulfonated fabric, 2-hydroxylauric acid, iodine, p-toluenesulfonic acid, ethanol and deionized water were mixed in a mass ratio of 1:2.4:1.3:0.4:5:1. After reacting at 100 rpm and 60°C for 120 min, the mixture was cooled to room temperature, removed and washed with saturated saline solution until the pH of the washing solution was 7 to obtain lauryl ester fabric.
[0061] (4) Mix lauryl ester fabric and N-methylpyrrolidone at a mass ratio of 1:6. Add 0.9 times the mass of lauryl ester fabric with oxaloyl chloride under an ice-water bath. Stir at 10°C and 80 rpm for 70 min. Then add 0.9 times the mass of lauryl ester fabric with R-aminoethyl-B-aminopropyltrimethoxysilane. React at 40°C for 4 h. Remove the product and wash it 6 times with distilled water and ethyl acetate, and then wash it 3 times with saturated saline solution to obtain silane fabric.
[0062] (5) Mix silane fabric, perfluorooctyltrimethoxysilane, potassium hydroxide and ethanol in a mass ratio of 1:1.2:0.1:5, heat to 84°C, add hexamethyldisiloxane in 1.4 times the mass of silane fabric, react for 4 hours, take it out, dry it under vacuum of 100 kPa and 90°C for 3 hours to obtain modified cotton fabric.
[0063] (6) Mix 3-amino-4-nitrobenzaldehyde, 36% hydrochloric acid, and deionized water in a mass ratio of 1:3.5:2.7. Stir at 80 rpm for 30 min, cool to -8℃, and add 1.6 times the mass of sodium nitrite aqueous solution of 3-amino-4-nitrobenzaldehyde. The mass ratio of sodium nitrite to deionized water in the sodium nitrite aqueous solution is 8.2:15. After reacting for 34 min, add urea until starch-potassium iodide test paper turns slightly blue to obtain intermediate A. Mix deionized water, sodium carbonate, and 3,4-diaminophenylacetone in a mass ratio of 12:5:1. Stir at 60 rpm and at 15℃, add 0.2 mL / min of intermediate A of 3,4-diaminophenylacetone. React for 3 h, filter to obtain solid, wash 3 times with methanol aqueous solution. The mass ratio of methanol to deionized water in the methanol aqueous solution is 1:19. Dry at 60℃ for 8 h to obtain intermediate B.
[0064] (7) Mix intermediate B, sodium hydroxide, and deionized water in a mass ratio of 1:0.4:0.5. Stir at 70 rpm, add zinc powder at a mass of 1.3 times that of intermediate B at a rate of 1.4 g / min, and add sodium hydroxide at a mass of 0.5 times that of intermediate B and deionized water at a mass of 2 times that of intermediate B. Heat to 60°C and keep warm for 2 hours. Then heat to 70°C and keep warm for 2 hours. Cool to room temperature, filter and collect the filtrate. Add hydrochloric acid until the pH of the filtrate is 2. Filter and collect the solid. Wash with deionized water 4 times and dry at 40°C for 10 hours to obtain benzotriazole compound.
[0065] (8) Mix benzotriazole compound, hydroxylamine hydrochloride and ethanol at a mass ratio of 1:0.3:11, react at 80℃ for 4h, cool to room temperature, filter and collect the filtrate, distill at -0.08MPa and 40℃ for 70min, add 9 times the mass of deionized water of benzotriazole compound, mix well, extract with ethyl acetate, combine the ethyl acetate layers, dry with anhydrous sodium sulfate for 1h, and distill at 80℃ for 2h to obtain intermediate C;
[0066] (9) Anhydrous potassium phosphate, potassium iodide, intermediate C, 2-bromoethanol and acetonitrile were heated to 85°C in a mass ratio of 0.9:0.7:1:0.6:10 and reacted for 7 hours. The filtrate was filtered and distilled at 300 rpm and 85°C for 5 hours. Then, 8.6 times the mass of intermediate C was added to deionized water and stirred evenly. The ethyl acetate layers were extracted with ethyl acetate and combined. The mixture was dried with anhydrous sodium sulfate for 1 hour and distilled at 85°C for 2 hours to obtain the oxime ether compound.
[0067] (10) E-44 epoxy resin, ethylene glycol monobutyl ether and ethanol were mixed in a mass ratio of 1:6:2.6. Under nitrogen protection, the mixture was heated to 80°C and stirred until dissolved. Then, 0.5 times the mass of the oxime ether compound of E-44 epoxy resin was added. After reacting for 14 hours, the mixture was filtered and washed with ethanol and water five times in sequence. The mixture was then dried at 50°C under a vacuum of -0.08 MPa for 48 hours to obtain the modified epoxy resin.
[0068] (11) Mix modified epoxy resin, polyvinyl alcohol and ethanol in a mass ratio of 40:5:10, stir at 130℃ and 300rpm for 30min, cool down to 50℃, add 0.2 times the mass of modified epoxy resin of polyamide 650 and 0.1 times the mass of modified epoxy resin of 2-ethylimidazole, stir at 5000rpm for 10min to obtain modified epoxy resin coating; apply 0.2 times the mass of modified epoxy resin coating to modified cotton fabric, dry at 80℃ for 8h to obtain self-cleaning no-wash fabric.
[0069] Comparative Example 1
[0070] The difference between Comparative Example 1 and Example 2 is that step (1) is omitted, and step (2) is changed to: a weight of 140 g / m 2 Cotton fabric, maleic anhydride, concentrated sulfuric acid, and toluene were mixed in a mass ratio of 1:1.14:0.05:4.5 and reacted at 70°C for 4 hours. The mixture was then removed and washed five times successively with chloroform and deionized water. Next, sodium bisulfite (0.35 times the mass of the cotton fabric) and isopropanol aqueous solution (4 times the mass of the cotton fabric) were added, with a mass ratio of isopropanol to deionized water of 3.9:1. The mixture was reacted at 84°C for 6 hours. Then, sodium bisulfite (0.2 times the mass of the cotton fabric) was added, and the reaction continued for another 6 hours. The mixture was then removed and washed four times successively with methanol aqueous solution and petroleum ether, with a mass ratio of methanol to deionized water of 3.2:1, yielding sulfonated fabric. The remaining steps were the same as in Example 2.
[0071] Comparative Example 2
[0072] The difference between Comparative Example 2 and Example 2 is that step (2) is omitted, and step (3) is changed to: mixing pretreated fabric, 2-hydroxylauric acid, iodine, p-toluenesulfonic acid, ethanol, and deionized water in a mass ratio of 1:1.9:1.1:0.4:3.5:1, reacting at 100 rpm and 60°C for 105 min, cooling to room temperature, removing, and washing with saturated saline solution until the pH of the washing solution is 7, to obtain lauryl ester fabric. The remaining steps are the same as in Example 2.
[0073] Comparative Example 3
[0074] The difference between Comparative Example 3 and Example 2 is that step (3) is omitted, and step (4) is changed to: sulfonated fabric and N-methylpyrrolidone are mixed at a mass ratio of 1:5, and under ice-water bath, 0.85 times the mass of sulfonated fabric oxaloyl chloride is added. After stirring at 10°C and 80 rpm for 60 min, 0.85 times the mass of sulfonated fabric R-aminoethyl-B-aminopropyltrimethoxysilane is added. After reacting at 38°C for 4 h, the mixture is taken out and washed 6 times with distilled water and ethyl acetate, and then washed 3 times with saturated brine to obtain silane fabric. The remaining steps are the same as in Example 2.
[0075] Comparative Example 4
[0076] The difference between Comparative Example 4 and Example 2 is that steps (4) and (5) are omitted, and step (11) is changed to: mixing modified epoxy resin, polyvinyl alcohol, and ethanol in a mass ratio of 35:4:7.5, stirring at 115°C and 300 rpm for 30 min, then cooling to 45°C, adding 0.13 times the mass of the modified epoxy resin of polyamide 650 and 0.08 times the mass of the modified epoxy resin of 4-methylimidazole, stirring at 5000 rpm for 10 min to obtain a modified epoxy resin coating; applying 0.14 times the mass of the lauryl ester fabric to the modified epoxy resin coating, drying at 80°C for 8 h to obtain a self-cleaning, wash-free fabric. The remaining steps are the same as in Example 2.
[0077] Comparative Example 5
[0078] The difference between Comparative Example 5 and Example 2 is that steps (6) and (7) are omitted, and step (8) is changed to: 3-amino-4-nitrobenzaldehyde, hydroxylamine hydrochloride, and ethanol are mixed at a mass ratio of 1:0.25:11, reacted at 80°C for 3.5 h, cooled to room temperature, filtered, and the filtrate is distilled at -0.08 MPa and 40°C for 65 min. Then, 9 times the mass of deionized water of 3-amino-4-nitrobenzaldehyde is added, mixed evenly, extracted with ethyl acetate, the ethyl acetate layers are combined, dried with anhydrous sodium sulfate for 1 h, and distilled at 80°C for 1.5 h to obtain intermediate C. The remaining steps are the same as in Example 2.
[0079] Comparative Example 6
[0080] The difference between Comparative Example 6 and Example 2 is that steps (8) and (9) are omitted, and step (10) is changed to: E-44 epoxy resin, ethylene glycol monobutyl ether, and ethanol are mixed in a mass ratio of 1:5:2.2, heated to 80°C under nitrogen protection, stirred and dissolved, and then 0.4 times the mass of E-44 epoxy resin benzotriazole compound is added. After reacting for 13 hours, the mixture is filtered, washed five times with ethanol and water, and dried at -0.08 MPa and 50°C for 48 hours to obtain the modified epoxy resin. The remaining steps are the same as in Example 2.
[0081] Example of effect
[0082] Table 1 below presents the performance analysis results of the self-cleaning, wash-free fabrics of Examples 1 to 3 and Comparative Examples 1 to 6 of the present invention.
[0083] Table 1
[0084]
[0085]
[0086] A comparison of the dust and oil stain levels in the examples and comparative examples reveals that this invention first utilizes malic acid to connect the fibers, making the fabric structure more compact and preventing impurities such as water, oil, and dust from penetrating the fabric. Then, it reacts with maleic anhydride and sodium bisulfite to form sulfonic acid-metal ion bonds in the side chains, improving antistatic properties and preventing dust accumulation. Next, it reacts and polymerizes with 2-hydroxylauric acid, R-aminoethyl-B-aminopropyltrimethoxysilane, perfluorooctyltrimethoxysilane, and hexamethyldisiloxane, resulting in excellent smoothness in the fabric and reducing dust accumulation. Dust adhesion and reduced surface energy result in excellent waterproof and oil-proof properties. A comparison of UPF and antibacterial experimental data from the examples and comparative examples reveals that this invention first utilizes 3-amino-4-nitrobenzaldehyde and 3,4-diaminophenylacetone to form a benzotriazole group, effectively improving the fabric's UV resistance. Then, it reacts with hydroxylamine hydrochloride and 2-bromoethanol to form an oxime ether group, which inhibits bacterial growth. Next, the epoxy resin is modified; when coated onto the modified fabric surface, the modified epoxy resin chemically bonds with the modified fabric, forming a Schiff base structure, thus enhancing the fabric's antibacterial properties.
[0087] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No markings in the claims should be construed as limiting the scope of the claims.
Claims
1. A self-cleaning, wash-free fabric, characterized in that, The self-cleaning, wash-free fabric is made by coating modified cotton fabric with modified epoxy resin coating.
2. The self-cleaning, wash-free fabric according to claim 1, characterized in that, The modified cotton fabric is prepared from malic acid, cotton fabric, maleic anhydride, sodium bisulfite, 2-hydroxylauric acid, R-aminoethyl-B-aminopropyltrimethoxysilane, perfluorooctyltrimethoxysilane, and hexamethyldisiloxane.
3. The self-cleaning, wash-free fabric according to claim 1, characterized in that, The modified epoxy resin is prepared from E-44 epoxy resin, 3-amino-4-nitrobenzaldehyde, 3,4-diaminophenylacetone, hydroxylamine hydrochloride, and 2-bromoethanol.
4. A method for preparing a self-cleaning, wash-free fabric, characterized in that, The preparation steps include the following: (1) Mix the pretreated fabric, maleic anhydride, concentrated sulfuric acid, and toluene in a mass ratio of 1:1.1:0.05:3 to 1:1.8:0.05:
6. After reacting at 70°C for 3 to 5 hours, remove the mixture and wash it with chloroform and deionized water 5 times in sequence. Then add sodium bisulfite at 0.3 to 0.4 times the mass of the pretreated fabric and isopropanol aqueous solution at 3 to 5 times the mass of the pretreated fabric. The mass ratio of isopropanol to deionized water in the isopropanol aqueous solution is 3.9:
1. After reacting at 80 to 88°C for 6 hours, add sodium bisulfite at 0.2 times the mass of the pretreated fabric and continue reacting for 6 hours. Remove the mixture and wash it with methanol aqueous solution and petroleum ether 4 times in sequence. The mass ratio of methanol to deionized water in the methanol aqueous solution is 3.2:1 to obtain sulfonated fabric. (2) The sulfonated fabric, 2-hydroxylauric acid, iodine, p-toluenesulfonic acid, ethanol and deionized water are mixed in a mass ratio of 1:1.5:0.9:0.4:2:1 to 1:2.4:1.3:0.4:5:
1. The mixture is reacted at 100 rpm and 60°C for 90 to 120 minutes. After cooling to room temperature, it is taken out and washed with saturated saline solution until the pH of the washing solution is 7 to obtain lauryl ester fabric. (3) Mix lauryl ester fabric and N-methylpyrrolidone in a mass ratio of 1:4 to 1:
6. Under an ice-water bath, add 0.8 to 0.9 times the mass of lauryl ester fabric with oxaloyl chloride. Stir at 10°C and 80 rpm for 50 to 70 minutes. Then add 0.8 to 0.9 times the mass of lauryl ester fabric with R-aminoethyl-B-aminopropyltrimethoxysilane. React at 35 to 40°C for 4 hours. Remove the product and wash it 6 times with distilled water and ethyl acetate, and then wash it 3 times with saturated saline solution to obtain silane fabric. (4) Mix silane fabric, perfluorooctyltrimethoxysilane, potassium hydroxide and ethanol in a mass ratio of 1:0.8:0.1:3 to 1:1.2:0.1:5, heat to 70 to 84°C, add hexamethyldisiloxane in 0.8 to 1.4 times the mass of silane fabric, react for 4 hours, take it out, dry it under vacuum of 100 kPa and 90°C for 1 to 3 hours to obtain modified cotton fabric; (5) Mix anhydrous potassium phosphate, potassium iodide, intermediate C, 2-bromoethanol, and acetonitrile in the following mass ratios. The reaction mixture was prepared in the range of 0.8:0.6:1:0.4:10 to 0.9:0.7:1:0.6:
10. The mixture was heated to 85°C and reacted for 5 to 7 hours. The mixture was then filtered and the filtrate was distilled at 200 to 300 rpm and 85°C for 3 to 5 hours. Deionized water at 8.6 times the mass of intermediate C was added and the mixture was stirred until homogeneous. The ethyl acetate layers were extracted with ethyl acetate and combined. The mixture was dried over anhydrous sodium sulfate for 1 hour and then distilled at 85°C for 1 to 2 hours to obtain the oxime ether compound. (6) E-44 epoxy resin, ethylene glycol monobutyl ether, and ethanol are mixed in a mass ratio of 1:4:1.7 to 1:6:2.
6. Under nitrogen protection, the mixture is heated to 80°C and stirred until dissolved. Then, 0.3 to 0.5 times the mass of E-44 epoxy resin oxime ether compound is added. After reacting for 12 to 14 hours, the mixture is filtered and washed five times with ethanol and water. The mixture is then dried at 50°C under a vacuum of -0.08 MPa for 48 hours to obtain the modified epoxy resin. (7) Mix modified epoxy resin, polyvinyl alcohol and ethanol in a mass ratio of 30:3:5 to 40:5:10, stir at 100 to 130°C and 300 rpm for 30 min, then cool to 40 to 50°C, add 0.06 to 0.2 times the mass of modified epoxy resin of polyamide 650 and 0.06 to 0.1 times the mass of modified epoxy resin of accelerator, stir at 5000 rpm for 10 min to obtain modified epoxy resin coating; apply 0.08 to 0.2 times the mass of modified cotton fabric of modified epoxy resin coating to modified cotton fabric, dry at 80°C for 8 h to obtain self-cleaning and wash-free fabric.
5. The method for preparing a self-cleaning, wash-free fabric according to claim 4, characterized in that, The preparation method of the pretreated fabric in step (1) is as follows: The fabric has a weight of 120-160 g / m². 2 The cotton fabric is immersed in an acid solution at a ratio of 1:10 to 1:20 for 10 to 20 minutes. After immersion, it is subjected to one dip and two nipping processes, with a nipping rate of 75 to 80% each time. After pre-drying at 70 to 80°C for 20 minutes, it is baked at 130 to 140°C for 30 minutes to obtain the pretreated fabric.
6. The method for preparing a self-cleaning, wash-free fabric according to claim 5, characterized in that, The acid solution contains malic acid, disodium hydrogen phosphate, and deionized water in a mass ratio of 10:5:
85.
7. The method for preparing a self-cleaning, wash-free fabric according to claim 4, characterized in that, The intermediate C in step (5) is prepared by mixing benzotriazole compound, hydroxylamine hydrochloride and ethanol in a mass ratio of 1:0.2:11 to 1:0.3:11, reacting at 80°C for 3 to 4 hours, cooling to room temperature, filtering and collecting the filtrate, distilling at -0.08 MPa and 40°C for 60 to 70 minutes, adding 9 times the mass of deionized water of benzotriazole compound, mixing evenly, extracting with ethyl acetate, combining the ethyl acetate layers, drying with anhydrous sodium sulfate for 1 hour, and distilling at 80°C for 1 to 2 hours to obtain intermediate C.
8. The method for preparing a self-cleaning, wash-free fabric according to claim 7, characterized in that, The method for preparing the benzotriazole compound is as follows: a. Mix 3-amino-4-nitrobenzaldehyde, 36% hydrochloric acid, and deionized water in a mass ratio of 1:2.8:2.7 to 1:3.5:2.
7. Stir at 60-80 rpm for 30 minutes, then cool to -8°C. Add 1.2-1.6 times the mass of 3-amino-4-nitrobenzaldehyde in a sodium nitrite aqueous solution, with a sodium nitrite to deionized water mass ratio of 8.2:
15. React for 20-34 minutes, then add urea to the starch-iodine mixture. The potassium chloride test paper turned slightly blue, indicating intermediate A. Deionized water, sodium carbonate, and 3,4-diaminophenylacetone were mixed in a mass ratio of 8:3:1 to 12:5:
1. The mixture was stirred at 60 rpm and at 10 to 15 °C. Then, intermediate A, which was 1 to 2 times the mass of 3,4-diaminophenylacetone, was added at a rate of 0.2 mL / min. The reaction was allowed to proceed for 2 to 3 hours. The solid was then filtered and washed three times with a methanol-water solution in which the mass ratio of methanol to deionized water was 1:
19. The solid was dried at 60 °C for 8 hours to obtain intermediate B. b. Mix intermediate B, sodium hydroxide, and deionized water in a mass ratio of 1:0.3:0.5 to 1:0.4:0.
5. While stirring at 70 rpm, add zinc powder at a rate of 1.0 to 1.3 times the mass of intermediate B at a rate of 1.0 to 1.4 g / min. Simultaneously add sodium hydroxide at a rate of 0.4 to 0.5 times the mass of intermediate B and deionized water at a rate of 1 to 2 times the mass of intermediate B. Heat to 60°C and hold for 1 to 2 hours. Then heat to 70°C and hold for 1 to 2 hours. Cool to room temperature, filter, and collect the filtrate. Add hydrochloric acid to adjust the pH of the filtrate to 1 to 2. Filter to collect the solid, wash with deionized water four times, and dry at 40°C for 10 hours to obtain the benzotriazole compound.
9. The method for preparing a self-cleaning, wash-free fabric according to claim 4, characterized in that, The promoter in step (7) is 2-ethylimidazole or 4-methylimidazole.
10. The method for preparing a self-cleaning, wash-free fabric according to claim 4, characterized in that, In step (7), the modified epoxy resin, polyvinyl alcohol, ethanol, polyamide 650, and accelerator are mixed in a mass ratio of 30:3:5:1.8:1.8 to 40:5:10:8:4.