Preparation method of high-temperature-resistant fabric

Abstract

The application discloses a preparation method of high-temperature-resistant fabric, and relates to the technical field of the fabric.The antibacterial agent is prepared from 2-(dimethylamino)-5-formylbenzyl cyanide, pyrrole and 6,6'-diazido-6,6'-dideoxyfucose, can kill or inhibit the propagation of bacteria, and thus the fabric has antibacterial effect;the flame retardant is prepared from triethoxysilane, graphene oxide, tributyl borate, dichloromethane and the antibacterial agent, can improve the high-temperature resistance of the fabric, and can promote the carbonization, crosslinking and expansion of the fabric to form a three-dimensional network structure carbon layer with silicon-carbon-boron structure when the fabric is burned, so that the fabric has flame retardation effect;the flame retardant, polyvinyl chloride and other additives are mixed to prepare synthetic leather, and then the synthetic leather is attached to a base cloth to obtain the high-temperature-resistant fabric.The fabric prepared by the application has antibacterial and flame retardation effects.

Description

Technical Field

[0001] This invention relates to the field of fabric technology, specifically to a method for preparing a high-temperature resistant fabric. Background Technology

[0002] my country is the world's largest producer, exporter, and consumer of textiles, accounting for more than a quarter of global exports. Fabrics are essential to all aspects of people's lives, and with the growth of people's material and cultural needs, the demand for special functions in fabrics is increasing, such as flame retardancy. Currently, most fabrics lack flame retardancy and are easily ignited when exposed to open flames or sparks. The flames spread rapidly and are difficult to extinguish, producing dense smoke and toxic gases, causing significant property damage and casualties.

[0003] Furthermore, fabrics are breeding grounds for bacteria, viruses, and other microorganisms. These microorganisms can cause cross-infection through contact with the human body, harming health and causing adverse allergic reactions such as headaches, fever, sore throat, and tonsillitis. Moreover, dust, sweat, sebum, and other substances adhering to the fabric surface react with resident bacteria on the skin and external microorganisms, producing low-grade fatty acids and volatile compounds that easily emit foul odors, severely impacting the environment. Prolonged contact can also affect human health. Therefore, developing a fabric with flame-retardant and antibacterial properties is particularly important. Summary of the Invention

[0004] The purpose of this invention is to provide a high-temperature resistant 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 high-temperature resistant fabric, wherein the high-temperature resistant fabric is made of synthetic leather and a base fabric; the synthetic leather is made of flame retardant, polyvinyl chloride K13S and other additives; the base fabric has a weight of 150 g / m². 2 The weaving of cloth.

[0006] Furthermore, the flame retardant is prepared from chloroboroxysilicon nanosheets and an antibacterial agent; the chloroboroxysilicon nanosheets are prepared from triethoxysilane, graphene oxide, tributyl borate, and dichloromethane.

[0007] Furthermore, the antibacterial agent is prepared from p-2-(dimethylamino)-5-carboxybenzonitrile, pyrrole, and 6,6'-diazido-6,6'-dideoxytrehalose.

[0008] Furthermore, the other main additives include plasticizers, foaming agents, dispersants, and stabilizers.

[0009] Furthermore, the plasticizer is triphenyl phosphate, o-trimethyl phosphate, m-trimethyl phosphate, or p-trimethyl phosphate; the foaming agent is azodicarbonamide; the dispersant is polyethylene wax or paraffin wax; and the stabilizer is calcium stearate or methyl tin mercaptan.

[0010] Furthermore, a method for preparing a high-temperature resistant fabric includes the following preparation steps: (1) Tetracyanoporphyrin, 6,6'-diazido-6,6'-dideoxytrehalose, cuprous bromide, hexamethyltriethylenetriamine, and N,N-dimethylformamide were mixed in a mass ratio of 9:5:1:11:3~11:7:3:15:3 and reacted at 50~60℃ for 2~4h under a nitrogen atmosphere. After freezing in liquid nitrogen for 30~60s, n-hexane was added until precipitation was complete. The mixture was filtered, washed 3~5 times with deionized water, and vacuum dried at -0.08MPa and 50~60℃ for 12h to obtain an antibacterial agent. (2) Mix chloroboroxysilicon nanosheets, antibacterial agent, deionized water and N,N-dimethylformamide in a mass ratio of 20:1:10:10~30:3:20:10, react at 200~300rpm and 110~150℃ for 2~4h, and wash with anhydrous ethanol and deionized water 3~5 times in sequence to obtain flame retardant; (3) Mix polyvinyl chloride K13S, flame retardant, foaming agent, plasticizer, stabilizer and dispersant in a mass ratio of 60:5:1:40:0.5:3~80:15:3:60:0.5:5, and knead at 20~40 rpm and 120~140℃ for 0.5~1.5 h. Then, coarsely knead at a steam pressure of 0.5~0.7 MPa and a roller gap of 3 mm for 3~5 min, and finely knead at a steam pressure of 0.4~0.6 MPa and a roller gap of 2 mm for 3~5 min. Finally, calender at 120~160℃ to obtain synthetic leather with a thickness of 0.1~0.3 mm. Lay the synthetic leather onto the base fabric and foam and emboss it at a pressure of 0.2~0.4 MPa and 180~200°C to obtain a high-temperature resistant fabric.

[0011] Further, the preparation method of tetracyanoporphyrin in step (1) is as follows: p-2-(dimethylamino)-5-carboxybenzonitrile and propionic acid are mixed in a mass ratio of 0.6:20~0.8:20, stirred at 200~300 rpm and 80~140℃ for 3~5 min, then pyrrole with a mass of 0.8~1.0 times that of p-2-(dimethylamino)-5-carboxybenzonitrile and acetic anhydride with a mass of 2~3 times that of p-2-(dimethylamino)-5-carboxybenzonitrile are added, the reaction is continued for 20~60 min, cooled to room temperature, methanol with a mass of 10~20 times that of p-2-(dimethylamino)-5-carboxybenzonitrile is added, the mixture is allowed to stand for 12 h, filtered, and vacuum dried at -0.08 MPa and 50~60℃ for 12 h to obtain tetracyanoporphyrin.

[0012] Further, the method for preparing chloroboronoxysilicon nanosheets in step (2) is as follows: In a nitrogen / oxygen mixed atmosphere at 700~800℃, the volume ratio of nitrogen to oxygen in the nitrogen / oxygen mixed atmosphere is 1:3. After preheating the intermediate product 2 for 20~40 min, the temperature is raised to 900~1000℃. Then, 0.1~0.3 times the mass of intermediate product 2 of tributyl borate and 0.05~0.07 times the mass of intermediate product 2 of dichloromethane are sprayed onto the intermediate product 2 in sequence. The reaction is continued for 20~40 min to obtain chloroboronoxysilicon nanosheets.

[0013] Furthermore, the intermediate product 2 is prepared by mixing intermediate product 1 and ammonia water at a mass ratio of 1:20 to 1:30, reacting at 200 to 300 rpm for 24 to 32 hours, centrifuging and washing with deionized water at 15,000 rpm 3 to 5 times, and freeze-drying at a vacuum of 50 Pa and -10 to -30 °C for 15 to 25 hours to obtain intermediate product 2.

[0014] Further, the intermediate product 1 is prepared as follows: graphene oxide and N,N-dimethylformamide are mixed at a mass ratio of 0.1:40 to 0.3:40, and sonicated at 500 to 800 W for 1 hour. Then, 1.1 to 1.3 times the mass of N,N-dimethylformamide in triethoxysilane and 0.006 to 0.008 times the mass of N,N-dimethylformamide in azobisisobutyronitrile are added. The mixture is reacted at 100 to 200 rpm and 60 to 80 °C for 24 to 32 hours. After centrifugation at 15,000 rpm for 5 to 10 minutes, the precipitate is collected and washed 3 to 5 times with N,N-dimethylformamide at 15,000 rpm. The precipitate is then collected to obtain intermediate product 1.

[0015] Compared with the prior art, the beneficial effects achieved by the present invention are: This invention involves mixing flame retardants, polyvinyl chloride, and other additives to obtain synthetic leather, which is then laminated with a base fabric to obtain a high-temperature resistant fabric. The flame retardant is made from triethoxysilane, graphene oxide, tributyl borate, dichloromethane, and an antibacterial agent, and has antibacterial and flame-retardant effects.

[0016] First, the antibacterial agent is prepared from p-2-(dimethylamino)-5-carboxybenzonitrile, pyrrole, and 6,6'-diazido-6,6'-dideoxytrehalose. Tetracyanoporphyrin is prepared by condensing the aldehyde group in p-2-(dimethylamino)-5-carboxybenzonitrile with pyrrole. This tetracyanoporphyrin generates reactive oxygen species under light irradiation, which act on microorganisms, leading to their death and thus giving the fabric an antibacterial effect. Tetracyanoporphyrin reacts with the cyano group and the azide group in 6,6'-diazido-6,6'-dideoxytrehalose to generate a triazole structure, which is then bridged and polymerized to form a network structure. The triazole structure inhibits bacterial proliferation while synergistically enhancing the conjugated system of the porphyrin with the network structure, thereby increasing the photocatalytic activity of the porphyrin structure and enhancing the antibacterial effect.

[0017] Secondly, after triethoxysilane polymerizes on the surface of the siloxy groups in graphene oxide to form a silica layer, the graphene oxide decomposes under high temperature and oxygen conditions. Simultaneously, tributyl borate and dichloromethane are sprayed, causing boron and chlorine to be doped into the silica, forming chloroboronoxysilicon nanosheets. These nanosheets improve the high-temperature resistance of the material through the high heat resistance of the boronoxysilicon structure, the barrier effect of the layered structure, and the restriction effect of molecular chain movement. During combustion, they can produce boric acid to promote the dehydration and carbonization of oxygen-containing groups, and form a three-dimensional network carbon layer with a silicon-carbon-boron structure through cross-linking and aggregation with silicon and boron. This blocks flammable gases and heat transfer, thus giving the fabric a flame-retardant effect. The chlorine groups in the chloroboronoxysilicon nanosheets react with the tertiary amine in the antibacterial agent to form a quaternary ammonium structure, which enhances the antibacterial effect. During combustion, they can be thermally decomposed to form ammonia, causing the carbon layer to expand and further enhancing the barrier effect of the carbon layer, thus enhancing the flame-retardant effect. In addition, the flame retardant can react with the chlorine groups in polyvinyl chloride through hydroxyl groups to inhibit the dehydrochlorination reaction of polyvinyl chloride, thereby improving the high-temperature resistance of the fabric. Detailed Implementation

[0018] 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.

[0019] To more clearly illustrate the method provided by the present invention, the following embodiments are provided in detail. The testing methods for various indicators of the high-temperature resistant fabric produced in the following embodiments are as follows: Antibacterial effect: The antibacterial rate of the examples and comparative examples of equal size was measured in a dark environment under irradiation by an 808 laser with an intensity of 0.3 watts per square centimeter, according to QB / T4715. High temperature resistance: After drying the same size of the example and comparative examples at 60 degrees Celsius for 12 hours, the fabric’s 5% thermal decomposition temperature was tested using a thermogravimetric analyzer under a nitrogen atmosphere, a flow rate of 50 ml per minute and a heating rate of 10 degrees Celsius per minute. Flame retardant effect: Take equal-sized examples and comparative examples, test the burning time and burning phenomena of the fabrics according to UL94, and evaluate the flame retardant level.

[0020] Example 1 (1) Mix p-2-(dimethylamino)-5-carboxybenzonitrile and propionic acid at a mass ratio of 0.6:20. Stir at 200 rpm and 80 °C for 3 min. Then add pyrrole at 0.8 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile and acetic anhydride at 2 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile. Continue the reaction for 20 min. Cool to room temperature. Add methanol at 10 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile. Let stand for 12 h. Filter. Dry under vacuum at -0.08 MPa and 50 °C for 12 h to obtain tetracyanoporphyrin. (2) Tetracyanoporphyrin, 6,6'-diazido-6,6'-dideoxytrehalose, cuprous bromide, hexamethyltriethylenetriamine, and N,N-dimethylformamide were mixed in a mass ratio of 9:5:1:11:3 and reacted at 50°C under a nitrogen atmosphere for 2 hours. After freezing in liquid nitrogen for 30 seconds, n-hexane was added until precipitation was complete. The mixture was filtered, washed three times with deionized water, and dried under vacuum at -0.08 MPa and 50°C for 12 hours to obtain an antibacterial agent. (3) Graphene oxide and N,N-dimethylformamide were mixed at a mass ratio of 0.1:40 and sonicated at 500W for 1 h. Triethoxysilane (1.1 times the mass of N,N-dimethylformamide) and azobisisobutyronitrile (0.006 times the mass of N,N-dimethylformamide) were added. The mixture was reacted at 100 rpm and 60℃ for 24 h. After centrifugation at 15000 rpm for 5 min, the precipitate was collected and washed three times with N,N-dimethylformamide at 15000 rpm. The precipitate was collected to obtain intermediate product 1. Intermediate product 1 and ammonia were mixed at a mass ratio of 1:20. After mixing and reacting at 200 rpm for 24 h, the mixture was washed three times by centrifugation with deionized water at 15000 rpm and then freeze-dried at -30℃ under vacuum of 50 Pa for 15 h to obtain intermediate product 2. In a nitrogen / oxygen mixed atmosphere at 700℃, with a nitrogen to oxygen volume ratio of 1:3, intermediate product 2 was preheated for 20 min and then heated to 900℃. 0.1 times the mass of intermediate product 2 of tributyl borate and 0.05 times the mass of intermediate product 2 of dichloromethane were sprayed onto intermediate product 2 sequentially, and the reaction was continued for 20 min to obtain chloroboroxysilicon nanosheets. (4) Mix chloroboroxysilicon nanosheets, antibacterial agent, deionized water and N,N-dimethylformamide in a mass ratio of 20:1:10:10, react at 200 rpm and 110 °C for 2 h, and then wash with anhydrous ethanol and deionized water three times in sequence to obtain flame retardant. (5) Mix polyvinyl chloride K13S, flame retardant, azodicarbonamide, triphenyl phosphate, calcium stearate and polyethylene wax in a mass ratio of 60:5:1:40:0.5:3. After mixing at 20 rpm and 120°C for 0.5 h, rough refining at a steam pressure of 0.5 MPa and a roller gap of 3 mm for 3 min, refining at a steam pressure of 0.4 MPa and a roller gap of 2 mm for 3 min, and then calendering at 120~160°C to obtain a synthetic leather with a thickness of 0.1 mm. Lay the synthetic leather onto the base fabric and foam and emboss it at a pressure of 0.2 MPa and 180°C to obtain a high-temperature resistant fabric.

[0021] Example 2 (1) Mix p-2-(dimethylamino)-5-carboxybenzonitrile and propionic acid at a mass ratio of 0.7:20. Stir at 250 rpm and 110 °C for 4 min. Then add pyrrole at 0.9 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile and acetic anhydride at 2.5 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile. Continue the reaction for 40 min. Cool to room temperature. Add methanol at 15 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile. Let stand for 12 h. Filter and dry under vacuum at -0.08 MPa and 55 °C for 12 h to obtain tetracyanoporphyrin. (2) Tetracyanoporphyrin, 6,6'-diazido-6,6'-dideoxytrehalose, cuprous bromide, hexamethyltriethylenetriamine, and N,N-dimethylformamide were mixed in a mass ratio of 10:6:2:13:3 and reacted at 55°C under a nitrogen atmosphere for 3 hours. After freezing in liquid nitrogen for 45 seconds, n-hexane was added until precipitation was complete. The mixture was filtered, washed four times with deionized water, and dried under vacuum at -0.08 MPa and 55°C for 12 hours to obtain an antibacterial agent. (3) Graphene oxide and N,N-dimethylformamide were mixed at a mass ratio of 0.2:40 and sonicated at 650W for 1 h. Triethoxysilane (1.2 times the mass of N,N-dimethylformamide) and azobisisobutyronitrile (0.007 times the mass of N,N-dimethylformamide) were added. The mixture was reacted at 150 rpm and 70 °C for 29 h. After centrifugation at 15000 rpm for 7.5 min, the precipitate was collected and washed 4 times with N,N-dimethylformamide at 15000 rpm. The precipitate was collected to obtain intermediate product 1. Intermediate product 1 and ammonia were mixed at a mass ratio of 1:2. 5. After mixing and reacting at 250 rpm for 29 h, the mixture was washed four times by centrifugation with deionized water at 15000 rpm and then freeze-dried at -20℃ under vacuum of 50 Pa for 20 h to obtain intermediate product 2. In a nitrogen / oxygen mixed atmosphere at 750℃, with a nitrogen to oxygen volume ratio of 1:3, intermediate product 2 was preheated for 30 min and then heated to 950℃. 0.2 times the mass of intermediate product 2 of tributyl borate and 0.06 times the mass of intermediate product 2 of dichloromethane were sprayed onto intermediate product 2 sequentially, and the reaction was continued for 30 min to obtain chloroboroxysilicon nanosheets. (4) Chloroboroxysilicon nanosheets, antibacterial agent, deionized water and N,N-dimethylformamide were mixed in a mass ratio of 25:2:15:10 and reacted at 250 rpm and 130 °C for 3 h. The mixture was then washed 4 times with anhydrous ethanol and deionized water to obtain a flame retardant. (5) Polyvinyl chloride K13S, flame retardant, azodicarbonamide, p-trimethylbenzene phosphate, calcium stearate and polyethylene wax are mixed in a mass ratio of 70:10:2:50:0.5:4. After mixing at 30 rpm and 130°C for 1 hour, the mixture is coarsely mixed at a steam pressure of 0.6 MPa and a roller gap of 3 mm for 4 minutes, and then refined at a steam pressure of 0.5 MPa and a roller gap of 2 mm for 4 minutes. Finally, the mixture is calendered at 120~160°C to obtain a synthetic leather with a thickness of 0.2 mm. The synthetic leather is then bonded to the base fabric and foamed and embossed at a pressure of 0.3 MPa and 190°C to obtain a high-temperature resistant fabric.

[0022] Example 3 (1) Mix p-2-(dimethylamino)-5-carboxybenzonitrile and propionic acid at a mass ratio of 0.8:20. Stir at 300 rpm and 140 °C for 5 min. Then add pyrrole at 1.0 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile and acetic anhydride at 3 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile. Continue the reaction for 60 min. Cool to room temperature. Add methanol at 20 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile. Let stand for 12 h. Filter. Dry under vacuum at -0.08 MPa and 60 °C for 12 h to obtain tetracyanoporphyrin. (2) Tetracyanoporphyrin, 6,6'-diazido-6,6'-dideoxytrehalose, cuprous bromide, hexamethyltriethylenetriamine, and N,N-dimethylformamide were mixed in a mass ratio of 11:7:3:15:3 and reacted at 60°C under a nitrogen atmosphere for 4 hours. After freezing in liquid nitrogen for 60 seconds, n-hexane was added until precipitation was complete. The mixture was filtered, washed five times with deionized water, and dried under vacuum at -0.08 MPa and 60°C for 12 hours to obtain an antibacterial agent. (3) Graphene oxide and N,N-dimethylformamide were mixed at a mass ratio of 0.3:40 and sonicated at 800W for 1 h. Triethoxysilane (1.3 times the mass of N,N-dimethylformamide) and azobisisobutyronitrile (0.008 times the mass of N,N-dimethylformamide) were added. The mixture was reacted at 200 rpm and 80℃ for 32 h. After centrifugation at 15000 rpm for 10 min, the precipitate was collected and washed 5 times with N,N-dimethylformamide at 15000 rpm. The precipitate was collected to obtain intermediate product 1. Intermediate product 1 and ammonia were mixed at a mass ratio of 1:30. After mixing and reacting at 300 rpm for 32 h, the mixture was washed five times by centrifugation with deionized water at 15000 rpm and then freeze-dried at -30℃ under vacuum of 50 Pa for 25 h to obtain intermediate product 2. In a nitrogen / oxygen mixed atmosphere at 800℃, with a nitrogen to oxygen volume ratio of 1:3, intermediate product 2 was preheated for 40 min and then heated to 1000℃. Tributyl borate (0.3 times the mass of intermediate product 2) and dichloromethane (0.07 times the mass of intermediate product 2) were sprayed onto intermediate product 2 sequentially, and the reaction was continued for 40 min to obtain chloroboroxysilicon nanosheets. (4) Chloroboroxysilicon nanosheets, antibacterial agent, deionized water and N,N-dimethylformamide were mixed in a mass ratio of 30:3:20:10 and reacted at 300 rpm and 150 °C for 4 h. The mixture was then washed 5 times with anhydrous ethanol and deionized water to obtain a flame retardant. (5) Polyvinyl chloride K13S, flame retardant, azodicarbonamide, o-trimethylbenzene phosphate, methyltin mercaptan and paraffin are mixed in a mass ratio of 80:15:3:60:0.5:5 and then mixed at 40 rpm and 140°C for 1.5 h. After that, the mixture is roughened for 5 min at a steam pressure of 0.7 MPa and a roller gap of 3 mm, and then refined for 5 min at a steam pressure of 0.6 MPa and a roller gap of 2 mm. Finally, the mixture is calendered at 120~160°C to obtain a synthetic leather with a thickness of 0.3 mm. The synthetic leather is then bonded to the base fabric and foamed and embossed at a pressure of 0.4 MPa and 200°C to obtain a high-temperature resistant fabric.

[0023] Comparative Example 1 The only difference between Comparative Example 1 and Example 2 is the absence of step (1). Step (2) is replaced by: mixing 2-(dimethylamino)-5-formylbenzonitrile, 6,6'-diazido-6,6'-dideoxytrehalose, cuprous bromide, hexamethyltriethylenetriamine, and N,N-dimethylformamide in a mass ratio of 10:6:2:13:3, reacting under a nitrogen atmosphere at 55°C for 3 hours, freezing in liquid nitrogen for 45 seconds, adding n-hexane until precipitation is complete, filtering, washing four times with deionized water, and vacuum drying at -0.08 MPa at 55°C for 12 hours to obtain the antibacterial agent. The remaining steps are the same as in Example 2.

[0024] Comparative Example 2 The only difference between Comparative Example 2 and Example 2 is the absence of step (2). Step (1) is changed as follows: 2-(dimethylamino)-5-carboxybenzonitrile and propionic acid are mixed at a mass ratio of 0.7:20. After stirring at 250 rpm and 110°C for 4 min, 0.9 times the mass of pyrrole and 2.5 times the mass of acetic anhydride are added to 2-(dimethylamino)-5-carboxybenzonitrile. The reaction is continued for 40 min, cooled to room temperature, and 15 times the mass of methanol is added. The mixture is allowed to stand for 12 h, filtered, and vacuum dried at -0.08 MPa and 55°C for 12 h to obtain the antibacterial agent. The remaining steps are the same as in Example 2.

[0025] Comparative Example 3 (1) Mix p-2-(dimethylamino)-5-carboxybenzonitrile and propionic acid at a mass ratio of 0.7:20. Stir at 250 rpm and 110 °C for 4 min. Then add pyrrole at 0.9 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile and acetic anhydride at 2.5 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile. Continue the reaction for 40 min. Cool to room temperature. Add methanol at 15 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile. Let stand for 12 h. Filter and dry under vacuum at -0.08 MPa and 55 °C for 12 h to obtain tetracyanoporphyrin. (2) Tetracyanoporphyrin, 6,6'-diazido-6,6'-dideoxytrehalose, cuprous bromide, hexamethyltriethylenetriamine, and N,N-dimethylformamide were mixed in a mass ratio of 10:6:2:13:3 and reacted at 55°C under a nitrogen atmosphere for 3 hours. After freezing in liquid nitrogen for 45 seconds, n-hexane was added until precipitation was complete. The mixture was filtered, washed four times with deionized water, and dried under vacuum at -0.08 MPa and 55°C for 12 hours to obtain an antibacterial agent. (3) Graphene oxide and N,N-dimethylformamide were mixed at a mass ratio of 0.2:40 and sonicated at 650W for 1 h. Then, 1.2 times the mass of N,N-dimethylformamide in triethoxysilane and 0.007 times the mass of N,N-dimethylformamide in azobisisobutyronitrile were added. The mixture was reacted at 150 rpm and 70 °C for 29 h. After centrifugation at 15000 rpm for 7.5 min, the precipitate was collected and washed 4 times with N,N-dimethylformamide at 15000 rpm. Intermediate product 1 was obtained; intermediate product 1 and ammonia water were mixed at a mass ratio of 1:25, reacted at 250 rpm for 29 h, washed 4 times by centrifugation with deionized water at 15000 rpm, and freeze-dried at a vacuum of 50 Pa and -20 °C for 20 h to obtain intermediate product 2; in a nitrogen / oxygen mixed atmosphere at 750 °C, with a nitrogen to oxygen volume ratio of 1:3, intermediate product 2 was preheated for 30 min, then heated to 950 °C and reacted for another 30 min to obtain silica nanosheets; (4) Mix silica nanosheets, antibacterial agent, deionized water and N,N-dimethylformamide in a mass ratio of 25:2:15:10, react at 250 rpm and 130 °C for 3 h, and then wash with anhydrous ethanol and deionized water 4 times in sequence to obtain flame retardant. (5) Polyvinyl chloride K13S, flame retardant, azodicarbonamide, p-trimethylbenzene phosphate, calcium stearate and polyethylene wax are mixed in a mass ratio of 70:10:2:50:0.5:4. After mixing at 30 rpm and 130°C for 1 hour, the mixture is coarsely mixed at a steam pressure of 0.6 MPa and a roller gap of 3 mm for 4 minutes, and then refined at a steam pressure of 0.5 MPa and a roller gap of 2 mm for 4 minutes. Finally, the mixture is calendered at 120~160°C to obtain a synthetic leather with a thickness of 0.2 mm. The synthetic leather is then bonded to the base fabric and foamed and embossed at a pressure of 0.3 MPa and 190°C to obtain a high-temperature resistant fabric.

[0026] Comparative Example 4 (1) Graphene oxide and N,N-dimethylformamide were mixed at a mass ratio of 0.2:40 and sonicated at 650W for 1 h. Triethoxysilane (1.2 times the mass of N,N-dimethylformamide) and azobisisobutyronitrile (0.007 times the mass of N,N-dimethylformamide) were added. The mixture was reacted at 150 rpm and 70 °C for 29 h. After centrifugation at 15000 rpm for 7.5 min, the precipitate was collected and washed 4 times with N,N-dimethylformamide at 15000 rpm. The precipitate was collected to obtain intermediate product 1. Intermediate product 1 and ammonia were mixed at a mass ratio of 1:2. 5. After mixing and reacting at 250 rpm for 29 h, the mixture was washed four times by centrifugation with deionized water at 15000 rpm and then freeze-dried at -20℃ under vacuum of 50 Pa for 20 h to obtain intermediate product 2. In a nitrogen / oxygen mixed atmosphere at 750℃, with a nitrogen to oxygen volume ratio of 1:3, intermediate product 2 was preheated for 30 min and then heated to 950℃. 0.2 times the mass of intermediate product 2 of tributyl borate and 0.06 times the mass of intermediate product 2 of dichloromethane were sprayed onto intermediate product 2 sequentially, and the reaction was continued for 30 min to obtain chloroboroxysilicon nanosheets. (2) Polyvinyl chloride K13S, flame retardant, azodicarbonamide, p-trimethylbenzene phosphate, calcium stearate and polyethylene wax are mixed in a mass ratio of 70:10:2:50:0.5:4. After mixing at 30 rpm and 130°C for 1 hour, the mixture is coarsely mixed at a steam pressure of 0.6 MPa and a roller gap of 3 mm for 4 minutes, and then refined at a steam pressure of 0.5 MPa and a roller gap of 2 mm for 4 minutes. Finally, the mixture is calendered at 120~160°C to obtain a synthetic leather with a thickness of 0.2 mm. The synthetic leather is then bonded to the base fabric and foamed and embossed at a pressure of 0.3 MPa and 190°C to obtain a high-temperature resistant fabric.

[0027] Example of effect Table 1 below shows the performance analysis results of the high-temperature resistant fabrics using Examples 1 to 3 and Comparative Examples 1 to 4 of the present invention.

[0028] Table 1 A comparison of the antibacterial rate data of the examples and comparative examples in Table 1 reveals that the fabric exhibits good antibacterial properties. Tetracyanoporphyrin, prepared by condensing the aldehyde group of 2-(dimethylamino)-5-carboxybenzonitrile with pyrrole, generates reactive oxygen species under light irradiation, which act on microorganisms, leading to their death and thus giving the fabric an antibacterial effect. Further reaction of tetracyanoporphyrin with 6,6'-diazido-6,6'-dideoxytrehalose bridges the cyanoporphyrin through a triazole structure, enhancing the conjugated porphyrin structure. This synergistic effect with the inhibitory effect of the triazole structure improves the fabric's antibacterial efficacy. The antibacterial agent reacts with chloroboronoxysilicon nanosheets to form a quaternary ammonium structure, further enhancing the antibacterial effect. A comparison of the flame retardant rating and 5% thermal decomposition temperature data of the examples and comparative examples in Table 1 also reveals… The fabric exhibits excellent flame retardant properties. By spraying tributyl borate and dichloromethane onto silica-coated graphene nanosheets under high temperature and oxygen conditions, chloroboronoxysilicon nanosheets are obtained. The high heat resistance and barrier properties of the nanosheets, along with their restriction of molecular chain movement, enhance the material's high-temperature resistance. Simultaneously, during combustion, they promote carbonization and cross-linking, forming a three-dimensional network carbon layer with a silicon-carbon-boron structure. This layer blocks flammable gases and heat transfer, thus giving the fabric a flame-retardant effect. Further reaction between the chloroboronoxysilicon nanosheets and antibacterial agents introduces a quaternary ammonium structure. During combustion, this structure decomposes upon heating to form ammonia, causing the carbon layer to expand and further enhancing its barrier effect, thus increasing the flame-retardant properties. Furthermore, the flame retardant can react with polyvinyl chloride (PVC) to inhibit the dehydrochlorination reaction of PVC, improving the fabric's high-temperature resistance.

[0029] 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 method for preparing a high-temperature resistant fabric, characterized in that, The preparation steps include the following: (1) Mix p-2-(dimethylamino)-5-carboxybenzonitrile and propionic acid at a mass ratio of 0.7:

20. Stir at 250 rpm and 110 °C for 4 min. Then add pyrrole at 0.9 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile and acetic anhydride at 2.5 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile. Continue the reaction for 40 min. Cool to room temperature. Add methanol at 15 times the mass of p-2-(dimethylamino)-5-carboxybenzonitrile. Let stand for 12 h. Filter and dry under vacuum at -0.08 MPa and 55 °C for 12 h to obtain tetracyanoporphyrin. (2) Tetracyanoporphyrin, 6,6'-diazido-6,6'-dideoxytrehalose, cuprous bromide, hexamethyltriethylenetriamine, and N,N-dimethylformamide were mixed in a mass ratio of 10:6:2:13:3 and reacted at 55°C under a nitrogen atmosphere for 3 hours. After freezing in liquid nitrogen for 45 seconds, n-hexane was added until precipitation was complete. The mixture was filtered, washed four times with deionized water, and dried under vacuum at -0.08 MPa and 55°C for 12 hours to obtain an antibacterial agent. (3) Graphene oxide and N,N-dimethylformamide were mixed at a mass ratio of 0.2:40 and sonicated at 650W for 1 h. Triethoxysilane (1.2 times the mass of N,N-dimethylformamide) and azobisisobutyronitrile (0.007 times the mass of N,N-dimethylformamide) were added. The mixture was reacted at 150 rpm and 70 °C for 29 h. After centrifugation at 15000 rpm for 7.5 min, the precipitate was collected and washed 4 times with N,N-dimethylformamide at 15000 rpm. The precipitate was collected to obtain intermediate product 1. Intermediate product 1 and ammonia were mixed at a mass ratio of 1:

2.

5. After mixing and reacting at 250 rpm for 29 h, the mixture was washed four times by centrifugation with deionized water at 15000 rpm and then freeze-dried at -20℃ under vacuum of 50 Pa for 20 h to obtain intermediate product 2. In a nitrogen / oxygen mixed atmosphere at 750℃, with a nitrogen to oxygen volume ratio of 1:3, intermediate product 2 was preheated for 30 min and then heated to 950℃. 0.2 times the mass of intermediate product 2 of tributyl borate and 0.06 times the mass of intermediate product 2 of dichloromethane were sprayed onto intermediate product 2 sequentially, and the reaction was continued for 30 min to obtain chloroboroxysilicon nanosheets. (4) Chloroboroxysilicon nanosheets, antibacterial agent, deionized water and N,N-dimethylformamide were mixed in a mass ratio of 25:2:15:10 and reacted at 250 rpm and 130 °C for 3 h. The mixture was then washed 4 times with anhydrous ethanol and deionized water to obtain a flame retardant. (5) Polyvinyl chloride K13S, flame retardant, azodicarbonamide, p-trimethylbenzene phosphate, calcium stearate and polyethylene wax are mixed in a mass ratio of 70:10:2:50:0.5:

4. After mixing at 30 rpm and 130°C for 1 hour, the mixture is coarsely mixed at a steam pressure of 0.6 MPa and a roller gap of 3 mm for 4 minutes, and then refined at a steam pressure of 0.5 MPa and a roller gap of 2 mm for 4 minutes. Finally, the mixture is calendered at 120~160°C to obtain a synthetic leather with a thickness of 0.2 mm. The synthetic leather is then bonded to the base fabric and foamed and embossed at a pressure of 0.3 MPa and 190°C to obtain a high-temperature resistant fabric.

Images