A thermal insulation and warming aerogel fabric

Abstract

The present application relates to the technical field of fabrics, and specifically discloses a thermal insulation and thermal insulation aerogel fabric, which is composed of polyimide aerogel fiber, coffee carbon fiber, and wool fiber; the polyimide aerogel fiber comprises the following raw materials in parts by weight: 40-60 parts of modified polyamic acid, 10-12 parts of ultrafine hemp stalk core powder, 4-8 parts of chitosan, and 1-2 parts of sophora biosurfactant; the modified polyamic acid comprises the following raw materials in parts by weight: 10-20 parts of surface-modified nano-silica, 20-40 parts of 4,4-diaminodiphenyl ether, 20-40 parts of pyromellitic anhydride, 40-60 parts of melamine, and 60-80 parts of N-methylpyrrolidone. The above scheme has a simple formula and a strict ratio. The obtained thermal insulation and thermal insulation aerogel fabric has good thermal insulation and thermal insulation properties and significant mechanical properties, and has broad application prospects.

Description

Technical Field

[0001] The present application relates to the technical field of fabrics, and more specifically, to a thermal insulation and warming aerogel fabric. Background Art

[0002] With the rapid development of the economy and technology, people's living standards are constantly improving, and clothing requirements are becoming increasingly stringent. Most of the thermal insulation fabrics commonly available on the market achieve this by filling two layers of fabric with insulating fibers, such as down, animal hair, and porous synthetic fibers. However, to ensure sufficient still air in the fabric, the fibers in these insulating textiles are often fluffy and bulky, affecting wearer convenience and aesthetics, and are therefore gradually falling out of favor.

[0003] Aerogel fibers have the characteristics of high specific surface area ratio, high porosity, light weight and low density. The volume ratio of air contained in aerogel fibers to the volume of fibers is incomparable to ordinary fibers. Therefore, aerogel fibers have gradually become the new favorite of thermal insulation and warm fabrics. At present, commonly used aerogel fibers include polyimide aerogel fibers, which have excellent properties of ultra-thinness, thermal insulation, hydrophobicity and breathability. However, due to the porous structure of polyimide aerogel fibers, the mechanical properties of polyimide aerogel fibers are reduced, and the fiber's waterproofness is poor, which greatly limits the application and development of polyimide aerogel fibers. Therefore, it is urgent to propose a thermal insulation and warming aerogel fabric to ensure that the polyimide aerogel fabric has significant thermal insulation and warming properties while also having excellent mechanical properties. Summary of the Invention

[0004] In order to solve the problem of poor mechanical properties of existing polyimide aerogel fibers, the present application provides a thermal insulation and warming aerogel fabric.

[0005] This application provides a thermal insulation and warming aerogel fabric, which adopts the following technical solutions:

[0006] A thermal insulation and warming aerogel fabric, composed of polyimide aerogel fiber, coffee carbon fiber, and wool fiber;

[0007] The polyimide aerogel fiber comprises the following raw materials in parts by weight: 40-60 parts of modified polyamic acid, 10-12 parts of superfine hemp stalk core powder, 4-8 parts of chitosan, and 1-2 parts of sophorolipid.

[0008] By adopting the above technical scheme, the heat-insulating and warming aerogel fabric of the present application is composed of polyimide aerogel fiber, coffee carbon fiber, and wool fiber. The polyimide aerogel fiber has high strength, hydrophobicity, flexibility, and flame retardancy, and exhibits significant heat-insulating performance at ultra-low and high temperatures; coffee carbon fiber is an environmentally friendly fiber with excellent warming, deodorization, moisture absorption and breathability, and can self-heat; wool fiber has the advantages of good elasticity, strong hygroscopicity, and good warmth retention; the aerogel fabric of the present application not only has excellent heat-insulating and warming functions, but also has significant mechanical properties, and has broad application prospects in many fields.

[0009] In addition, the polyimide aerogel fiber of the present application uses modified polyamic acid as the main raw material, and adds hemp stalk core ultrafine powder, chitosan, and sophora biosurfactant; the hemp stalk core ultrafine powder has good moisture absorption and moisture conductivity, antibacterial, adsorption, and UV resistance, which can effectively prevent fiber aging. At the same time, the hemp stalk core ultrafine powder can effectively reduce the VOCs content; and the hemp stalk core ultrafine powder and the modified polyamic acid macromolecules are chemically bonded and microporously physically cross-linked, which can form a three-dimensional network structure, making the microstructure of the polyimide aerogel fiber The structure is richer, which not only significantly improves the thermal insulation performance of polyimide aerogel fiber, but also enhances the mechanical properties of polyimide aerogel fiber; chitosan has good antibacterial properties, and there are a large number of active groups on the surface of chitosan. The addition of chitosan can make the comprehensive performance of polyimide aerogel fiber more excellent; sophora biosurfactant is conducive to the uniform dispersion of hemp stalk core ultrafine powder and chitosan in modified polyamic acid, and the components interact with each other and synergistically enhance the effect to form a structurally stable polyimide aerogel fiber with better mechanical properties.

[0010] Preferably, the modified polyamic acid comprises the following raw materials in parts by weight: 10-20 parts of surface-modified nano-silica, 20-40 parts of 4,4-diaminodiphenyl ether, 20-40 parts of pyromellitic anhydride, 40-60 parts of melamine, and 60-80 parts of N-methylpyrrolidone.

[0011] Preferably, the modified polyamic acid is prepared by the following method:

[0012] Add 4,4-diaminodiphenyl ether and surface-modified nano-silica to N-methylpyrrolidone, stir at a speed of 500-1000 r / min for 10-20 minutes, then add pyromellitic anhydride and melamine, maintain the same stirring speed, and continue stirring for 30-60 minutes to obtain modified polyamic acid.

[0013] By adopting the above technical solution, the modified polyamic acid of the present application is obtained by the reaction of diamine and dianhydride, with melamine as a cross-linking agent and surface-modified nano-silica added. At the same time, various process parameters are controlled to effectively ensure that the polyimide has good melt viscosity and appropriate cross-linking density during imidization, thereby greatly improving the thermal insulation performance of the finally obtained polyimide aerogel fiber and enhancing its mechanical properties.

[0014] Preferably, the surface-modified nano-silica is prepared by the following method:

[0015] Nano-silica, bis(4-aminophenoxy)dimethylsilane, and toluene are mixed in a mass ratio of 10-20:1-3:30-60, stirred at a speed of 1100-1500 r / min for 5-10 minutes, and then heated under reflux at 60-80° C. for 6-8 hours while maintaining the same stirring speed and continuously introducing nitrogen. After the reaction is completed, the mixture is filtered, washed, and dried to obtain surface-modified nano-silica.

[0016] By adopting the above technical solution, the present application uses bis(4-aminophenoxy)dimethylsilane to modify nano-silica, so that the surface of the nano-silica contains a large number of amino groups, which can improve the dispersibility and stability of the surface-modified nano-silica; on the one hand, the surface-modified nano-silica can serve as a reinforcing phase to improve the high temperature resistance and mechanical properties of the polyimide aerogel fiber; on the other hand, the amino groups on the surface of the nano-silica can react with pyromellitic anhydride to enrich the three-dimensional cross-linked structure of the modified polyamic acid, thereby forming a porous structure in the prepared polyimide aerogel fiber, and the porous structure is not easy to collapse, thereby ensuring that the polyimide aerogel fiber has excellent thermal insulation properties while also having good mechanical properties.

[0017] Preferably, the polyimide aerogel fiber is prepared by the following method:

[0018] S1. Add hemp stalk core ultrafine powder, chitosan, and sophorolipid to the modified polyamic acid, mix well, and then perform vacuum degassing for 20-40 minutes to obtain a spinning solution;

[0019] S2. Using a wet spinning process, squeeze the spinning solution obtained in step S1 into a 10-20° C. mixing coagulation bath and perform solvent replacement for 8-12 hours to obtain modified polyamic acid hydrogel fibers;

[0020] S3. The modified polyamic acid hydrogel fiber obtained in step S2 is dried with supercritical carbon dioxide and then thermally stretched to obtain polyimide aerogel fiber.

[0021] By adopting the above-mentioned technical scheme, in the process of preparing polyimide aerogel fibers, the present application first adds ultrafine powder of hemp stalk core, chitosan, and sophora biosurfactant to the modified polyamic acid and mixes them evenly, and then performs vacuum degassing to improve the spinnability of the spinning solution; then, a wet spinning process is adopted to extrude the spinning solution into a mixed coagulation bath and perform solvent replacement to obtain a modified polyamic acid hydrogel fiber with a stable three-dimensional cross-linked structure; finally, supercritical drying and hot stretching are performed to obtain polyimide aerogel fibers; at the same time, various process parameters are controlled so that the polyimide aerogel fibers have a rich porous structure to ensure that the comprehensive performance of the aerogel fabric is more excellent.

[0022] Preferably, the volume ratio of the spinning solution to the mixed coagulation bath is 1:10-20.

[0023] By adopting the above-mentioned technical solution, the present application controls the volume ratio of the spinning solution to the mixed coagulation bath within a certain range during the wet spinning process, so that the structure of the modified polyamic acid hydrogel fiber formed is more compact, thereby making the comprehensive performance of the polyimide aerogel fiber more excellent; at the same time, it can save resources and has positive significance for sustainable development.

[0024] Preferably, the mixed coagulation bath is obtained by mixing water, acetone and ethyl acetate in a volume ratio of 3-6:1-5:1.

[0025] By adopting the above-mentioned technical solution, the mixed coagulation bath of the present application is obtained by mixing water, acetone and ethyl acetate. During the solvent replacement process, the three have different polarities and different replacement capabilities. The three work together to ensure that the porous structure of the polyimide aerogel fiber can be smoothly formed, so that the thermal insulation and warmth performance of the polyimide aerogel fiber is significantly enhanced.

[0026] Preferably, the supercritical carbon dioxide drying pressure is 8.5-9 MPa, the temperature is 40-50° C., and the drying time is 10-15 h; the hot stretching temperature is 380-450° C., and the winding speed is 1-2 m / min.

[0027] By adopting the above technical solution, the present application controls the process parameters of supercritical carbon dioxide drying and thermal stretching within a certain range, so that the porous structure formed by the final polyimide aerogel fiber can not only play a role in heat insulation and warmth preservation, but also effectively ensure that the aerogel fiber has excellent mechanical properties.

[0028] Preferably, the thermal insulation and warming aerogel fabric is prepared by the following method:

[0029] First, polyimide aerogel fiber, coffee carbon fiber and wool fiber are blended in a mass ratio of 5-6:1-2:1 to obtain yarn; then the yarn is woven to obtain heat-insulating and warming aerogel fabric.

[0030] By adopting the above-mentioned technical scheme, the present application controls the mass ratio of polyimide aerogel fiber, coffee carbon fiber and wool fiber within a certain range for blending to obtain warp yarn, weaves the yarn, and controls various process parameters to prepare thermal insulating and warming aerogel fabric. The preparation method of the thermal insulating and warming aerogel fabric of the present application has simple steps, low cost, and is suitable for industrial production. The obtained thermal insulating and warming aerogel fabric has excellent thermal insulating and warming properties and mechanical properties, and has broad application prospects.

[0031] In summary, this application has the following beneficial effects:

[0032] 1. The thermal insulation and thermal insulation aerogel fabric of the present application is composed of polyimide aerogel fiber, coffee carbon fiber and wool fiber, so that the thermal insulation and thermal insulation aerogel fabric has significant thermal insulation and thermal insulation performance, as well as excellent mechanical properties, and has broad application prospects.

[0033] 2. The polyimide aerogel fiber of the present application includes modified polyamic acid, ultrafine hemp stalk core powder, chitosan, and sophorolipid. The components interact with each other, so that the mechanical properties of the prepared polyimide aerogel fiber are significantly improved.

[0034] 3. The raw materials of the modified polyamic acid of the present application include surface-modified nano-silica, 4,4-diaminodiphenyl ether, pyromellitic anhydride, melamine, etc., and the surface of the nano-silica is modified with bis(4-aminophenoxy)dimethylsilane, so that the mechanical properties and thermal insulation properties of the prepared polyimide aerogel fiber are enhanced.

[0035] 4. The preparation method of the thermal insulation and thermal insulation aerogel fabric of the present application is simple, the preparation cost is low, and it is suitable for industrial production. The prepared thermal insulation and thermal insulation aerogel fabric has excellent performance, which expands the application range of the thermal insulation and thermal insulation aerogel fabric. DETAILED DESCRIPTION

[0036] The present application is further described in detail below with reference to the embodiments.

[0037] Preparation Examples 1-5 provide methods for preparing surface-modified nano-silica.

[0038] Preparation Example 1

[0039] Surface-modified nano-silica is prepared by the following method:

[0040] 10 kg of nano-silica, 1 kg of bis(4-aminophenoxy)dimethylsilane, and 30 kg of toluene were mixed, stirred at a speed of 1100 r / min for 10 minutes, and then heated under reflux at 60° C. for 8 hours while continuously introducing nitrogen. After the reaction, the mixture was filtered, washed, and dried to obtain surface-modified nano-silica.

[0041] Preparation Example 2

[0042] Surface-modified nano-silica is prepared by the following method:

[0043] 12 kg of nano-silica, 1.5 kg of bis(4-aminophenoxy)dimethylsilane, and 37 kg of toluene were mixed, stirred at a speed of 1200 r / min for 8 minutes, and then heated under reflux at 65° C. for 7.5 hours while continuously introducing nitrogen. After the reaction, the mixture was filtered, washed, and dried to obtain surface-modified nano-silica.

[0044] Preparation Example 3

[0045] Surface-modified nano-silica is prepared by the following method:

[0046] 15 kg of nano-silica, 2 kg of bis(4-aminophenoxy)dimethylsilane, and 45 kg of toluene were mixed, stirred at a speed of 1300 r / min for 7 minutes, and then heated under reflux at 70° C. for 7 hours while continuously introducing nitrogen. After the reaction, the mixture was filtered, washed, and dried to obtain surface-modified nano-silica.

[0047] Preparation Example 4

[0048] Surface-modified nano-silica is prepared by the following method:

[0049] 18 kg of nano-silica, 2.5 kg of bis(4-aminophenoxy)dimethylsilane, and 54 kg of toluene were mixed, stirred at a speed of 1400 r / min for 6 minutes, and then heated under reflux at 75°C for 6.5 hours while continuously introducing nitrogen. After the reaction, the mixture was filtered, washed, and dried to obtain surface-modified nano-silica.

[0050] Preparation Example 5

[0051] Surface-modified nano-silica is prepared by the following method:

[0052] 20 kg of nano-silica, 3 kg of bis(4-aminophenoxy)dimethylsilane, and 60 kg of toluene were mixed, stirred at a speed of 1500 r / min for 5 minutes, and then heated under reflux at 80°C for 6 hours while continuously introducing nitrogen. After the reaction, the mixture was filtered, washed, and dried to obtain surface-modified nano-silica.

[0053] Preparation Examples 6-10 and Comparative Preparation Examples 1 and 2 are modified polyamic acids and preparation methods thereof.

[0054] Preparation Example 6

[0055] Modified polyamic acid, including the following raw materials: 10 kg surface-modified nano-silica, 20 kg 4,4-diaminodiphenyl ether, 20 kg pyromellitic anhydride, 40 kg melamine, 60 kg N-methylpyrrolidone;

[0056] Among them, the surface-modified nano-silica is prepared in Example 1;

[0057] Modified polyamic acid is prepared by the following method:

[0058] 4,4-Diaminodiphenyl ether and surface-modified nano-silica were added to N-methylpyrrolidone and stirred at a speed of 500 r / min for 20 minutes. Subsequently, pyromellitic anhydride and melamine were added and stirred for 60 minutes at the same stirring speed to obtain modified polyamic acid.

[0059] Preparation Example 7

[0060] Modified polyamic acid, including the following raw materials: 12 kg surface-modified nano-silica, 25 kg 4,4-diaminodiphenyl ether, 25 kg pyromellitic anhydride, 45 kg melamine, 65 kg N-methylpyrrolidone;

[0061] Among them, the surface-modified nano-silica is prepared in Example 2;

[0062] Modified polyamic acid is prepared by the following method:

[0063] 4,4-Diaminodiphenyl ether and surface-modified nano-silica were added to N-methylpyrrolidone and stirred at a speed of 600 r / min for 18 minutes. Subsequently, pyromellitic anhydride and melamine were added and stirred for 55 minutes at the same stirring speed to obtain modified polyamic acid.

[0064] Preparation Example 8

[0065] Modified polyamic acid, including the following raw materials: 15 kg surface-modified nano-silica, 30 kg 4,4-diaminodiphenyl ether, 30 kg pyromellitic anhydride, 50 kg melamine, 70 kg N-methylpyrrolidone;

[0066] Among them, the surface-modified nano-silica is prepared in Example 3;

[0067] Modified polyamic acid is prepared by the following method:

[0068] 4,4-Diaminodiphenyl ether and surface-modified nano-silica were added to N-methylpyrrolidone and stirred at a speed of 800 r / min for 15 minutes. Subsequently, pyromellitic anhydride and melamine were added and stirred for 45 minutes at the same stirring speed to obtain modified polyamic acid.

[0069] Preparation Example 9

[0070] Modified polyamic acid, including the following raw materials: 18 kg surface-modified nano-silica, 35 kg 4,4-diaminodiphenyl ether, 35 kg pyromellitic anhydride, 55 kg melamine, 75 kg N-methylpyrrolidone;

[0071] Among them, the surface-modified nano-silica is prepared in Example 4;

[0072] Modified polyamic acid is prepared by the following method:

[0073] 4,4-Diaminodiphenyl ether and surface-modified nano-silica were added to N-methylpyrrolidone and stirred at a speed of 900 r / min for 12 minutes. Subsequently, pyromellitic anhydride and melamine were added and stirred for 38 minutes at the same stirring speed to obtain modified polyamic acid.

[0074] Preparation Example 10

[0075] Modified polyamic acid, including the following raw materials: 20 kg surface-modified nano-silica, 40 kg 4,4-diaminodiphenyl ether, 40 kg pyromellitic anhydride, 60 kg melamine, 80 kg N-methylpyrrolidone;

[0076] Among them, the surface-modified nano-silica is prepared in Example 5;

[0077] Modified polyamic acid is prepared by the following method:

[0078] 4,4-Diaminodiphenyl ether and surface-modified nano-silica were added to N-methylpyrrolidone and stirred at a speed of 1000 r / min for 10 minutes. Subsequently, pyromellitic anhydride and melamine were added and stirred for 30 minutes at the same stirring speed to obtain modified polyamic acid.

[0079] Comparative Preparation Example 1

[0080] Comparative Preparation Example 1 is the same as Preparation Example 6, except that nano-silica is used to replace the surface-modified nano-silica.

[0081] Comparative Preparation Example 2

[0082] Comparative Preparation Example 2 is the same as Preparation Example 6, except that no surface-modified nano-silica is added.

[0083] Preparation Examples 11-15 and Comparative Preparation Examples 3-12 are polyimide aerogel fibers and preparation methods thereof.

[0084] Preparation Example 11

[0085] Polyimide aerogel fiber, including the following raw materials: 40kg modified polyamic acid, 10kg hemp stalk core ultrafine powder, 4kg chitosan, 1kg sophora biosurfactant;

[0086] Among them, the modified polyamic acid is Preparation Example 6;

[0087] Polyimide aerogel fiber is prepared by the following method:

[0088] S1. Add hemp stalk core ultrafine powder, chitosan, and sophorolipid to the modified polyamic acid, mix well, and then perform vacuum degassing for 20 minutes to obtain a spinning solution;

[0089] S2. Using a wet spinning process, the spinning solution obtained in step S1 was squeezed into a 10° C. mixing coagulation bath and subjected to solvent replacement for 8 hours to obtain modified polyamic acid hydrogel fibers;

[0090] The volume ratio of the spinning solution to the mixed coagulation bath is 1:10; the mixed coagulation bath is prepared by mixing water, acetone and ethyl acetate in a volume ratio of 3:1:1;

[0091] S3. The modified polyamic acid hydrogel fiber obtained in step S2 is dried by supercritical carbon dioxide at a pressure of 8.5 MPa, a temperature of 40° C., and a drying time of 10 h; then hot stretching is performed at a temperature of 380° C. and a winding speed of 1 m / min to obtain a polyimide aerogel fiber.

[0092] Preparation Example 12

[0093] Polyimide aerogel fiber, including the following raw materials: 45kg modified polyamic acid, 10.5kg hemp stalk core ultrafine powder, 5kg chitosan, 1.2kg sophora biosurfactant;

[0094] Among them, the modified polyamic acid is Preparation Example 7;

[0095] Polyimide aerogel fiber is prepared by the following method:

[0096] S1. Add hemp stalk core ultrafine powder, chitosan, and sophorolipid to the modified polyamic acid, mix well, and then vacuum degas for 25 minutes to obtain a spinning solution;

[0097] S2. Using a wet spinning process, the spinning solution obtained in step S1 was squeezed into a 12° C. mixing coagulation bath and subjected to solvent replacement for 9 hours to obtain modified polyamic acid hydrogel fibers;

[0098] The volume ratio of the spinning solution to the mixed coagulation bath is 1:12; the mixed coagulation bath is prepared by mixing water, acetone and ethyl acetate in a volume ratio of 4:2:1;

[0099] S3. The modified polyamic acid hydrogel fiber obtained in step S2 is dried by supercritical carbon dioxide at a pressure of 8.7 MPa, a temperature of 42° C., and a drying time of 11 h; then hot stretching is performed at a temperature of 390° C. and a winding speed of 1.2 m / min to obtain a polyimide aerogel fiber.

[0100] Preparation Example 13

[0101] Polyimide aerogel fiber, including the following raw materials: 50kg modified polyamic acid, 11kg hemp stalk core ultrafine powder, 6kg chitosan, 1.5kg sophora biosurfactant;

[0102] Among them, the modified polyamic acid is Preparation Example 8;

[0103] Polyimide aerogel fiber is prepared by the following method:

[0104] S1. Add hemp stalk core ultrafine powder, chitosan, and sophorolipid to the modified polyamic acid, mix well, and then vacuum degas for 30 minutes to obtain a spinning solution;

[0105] S2. Using a wet spinning process, the spinning solution obtained in step S1 was squeezed into a 15° C. mixing coagulation bath and solvent replacement was performed for 10 hours to obtain modified polyamic acid hydrogel fibers;

[0106] The volume ratio of the spinning solution to the mixed coagulation bath is 1:15; the mixed coagulation bath is prepared by mixing water, acetone and ethyl acetate in a volume ratio of 5:3:1;

[0107] S3. The modified polyamic acid hydrogel fiber obtained in step S2 is dried by supercritical carbon dioxide at a pressure of 8.8 MPa, a temperature of 45° C., and a drying time of 13 h; then hot stretching is performed at a temperature of 420° C. and a winding speed of 1.5 m / min to obtain a polyimide aerogel fiber.

[0108] Preparation Example 14

[0109] Polyimide aerogel fiber, including the following raw materials: 55kg modified polyamic acid, 11.5kg hemp stalk core ultrafine powder, 7kg chitosan, 1.8kg sophora biosurfactant;

[0110] Among them, the modified polyamic acid is Preparation Example 9;

[0111] Polyimide aerogel fiber is prepared by the following method:

[0112] S1. Add hemp stalk core ultrafine powder, chitosan, and sophorolipid to the modified polyamic acid, mix well, and then vacuum degas for 35 minutes to obtain a spinning solution;

[0113] S2. Using a wet spinning process, the spinning solution obtained in step S1 was squeezed into a mixing coagulation bath at 18° C. and solvent replacement was performed for 9 hours to obtain modified polyamic acid hydrogel fibers;

[0114] The volume ratio of the spinning solution to the mixed coagulation bath is 1:18; the mixed coagulation bath is prepared by mixing water, acetone and ethyl acetate in a volume ratio of 5:4:1;

[0115] S3. The modified polyamic acid hydrogel fiber obtained in step S2 is dried by supercritical carbon dioxide at a pressure of 8.9 MPa, a temperature of 48° C., and a drying time of 11 h; then hot drawing is performed at a temperature of 420° C. and a winding speed of 1.8 m / min to obtain a polyimide aerogel fiber.

[0116] Preparation Example 15

[0117] Polyimide aerogel fiber, including the following raw materials: 60kg modified polyamic acid, 12kg hemp stalk core ultrafine powder, 8kg chitosan, 2kg sophorolipid;

[0118] Among them, the modified polyamic acid is Preparation Example 10;

[0119] Polyimide aerogel fiber is prepared by the following method:

[0120] S1. Add hemp stalk core ultrafine powder, chitosan, and sophorolipid to the modified polyamic acid, mix well, and then vacuum degas for 40 minutes to obtain a spinning solution;

[0121] S2. Using a wet spinning process, the spinning solution obtained in step S1 was squeezed into a 20° C. mixing coagulation bath and subjected to solvent replacement for 8 hours to obtain modified polyamic acid hydrogel fibers;

[0122] The volume ratio of the spinning solution to the mixed coagulation bath is 1:20; the mixed coagulation bath is prepared by mixing water, acetone and ethyl acetate in a volume ratio of 6:5:1;

[0123] S3. The modified polyamic acid hydrogel fiber obtained in step S2 is dried by supercritical carbon dioxide at a pressure of 9 MPa, a temperature of 50° C., and a drying time of 15 h; then hot stretching is performed at a temperature of 450° C. and a winding speed of 2 m / min to obtain a polyimide aerogel fiber.

[0124] Comparative Preparation Example 3

[0125] Comparative Preparation Example 3 is the same as Preparation Example 11, except that the modified polyamic acid is the same as that in Comparative Preparation Example 1.

[0126] Comparative Preparation Example 4

[0127] Comparative Preparation Example 4 is the same as Preparation Example 11, except that the modified polyamic acid is the same as that in Comparative Preparation Example 2.

[0128] Comparative Preparation Example 5

[0129] Comparative Preparation Example 5 is the same as Preparation Example 11, except that the ultrafine hemp stalk core powder is not added.

[0130] Comparative Preparation Example 6

[0131] Comparative Preparation Example 6 is the same as Preparation Example 11, except that chitosan is not added.

[0132] Comparative Preparation Example 7

[0133] Comparative Preparation Example 7 is the same as Preparation Example 11, except that no sophorolipid is added.

[0134] Comparative Preparation Example 8

[0135] Comparative Preparation Example 8 is the same as Preparation Example 11, except that the volume ratio of the spinning solution to the mixed coagulation bath is 1:5.

[0136] Comparative Preparation Example 9

[0137] Comparative Preparation Example 9 is the same as Preparation Example 11, except that the volume ratio of the spinning solution to the mixed coagulation bath is 1:30.

[0138] Comparative Preparation Example 10

[0139] Comparative Preparation Example 10 is the same as Preparation Example 11, except that the mixed coagulation bath is obtained by mixing water and acetone in a volume ratio of 3:2.

[0140] Comparative Preparation Example 11

[0141] Comparative Preparation Example 11 is the same as Preparation Example 11, except that the mixed coagulation bath is obtained by mixing water and ethyl acetate in a volume ratio of 4:1.

[0142] Comparative Preparation Example 12

[0143] Comparative Preparation Example 12 is the same as Preparation Example 11, except that the mixed coagulation bath is obtained by mixing acetone and ethyl acetate in a volume ratio of 1:4.

[0144] Examples 1-5 provide a thermal insulation and warming aerogel fabric.

[0145] Example 1

[0146] A heat-insulating and warming aerogel fabric is prepared by the following method:

[0147] First, 5kg of polyimide aerogel fiber, 1kg of coffee carbon fiber, and 1kg of wool fiber are mixed, and then the yarn is obtained through the processes of wool mixing, cotton plucking, cotton blending, cotton opening, cotton carding, drawing, friction spinning and winding. Then, the yarn is obtained through the processes of warping, drawing-in, weaving, finishing and packaging to obtain the thermal insulation and warming aerogel fabric.

[0148] Among them, the polyimide aerogel fiber is Preparation Example 11.

[0149] Example 2

[0150] A heat-insulating and warming aerogel fabric is prepared by the following method:

[0151] First, 5.2 kg of polyimide aerogel fiber, 1.2 kg of coffee carbon fiber, and 1 kg of wool fiber are mixed, and then the yarn is obtained through the processes of wool mixing, cotton plucking, blending, cotton opening, carding, drawing, friction spinning and winding. Then, the yarn is obtained through the processes of warping, drawing-in, weaving, finishing and packaging to obtain the thermal insulation and warming aerogel fabric.

[0152] Among them, the polyimide aerogel fiber is Preparation Example 12.

[0153] Example 3

[0154] A heat-insulating and warming aerogel fabric is prepared by the following method:

[0155] First, 5.5 kg of polyimide aerogel fiber, 1.5 kg of coffee carbon fiber, and 1 kg of wool fiber are mixed, and then the yarn is obtained through the processes of wool mixing, cotton plucking, blending, cotton opening, carding, drawing, friction spinning and winding. Then, the yarn is obtained through the processes of warping, drawing-in, weaving, finishing and packaging to obtain the thermal insulation and warming aerogel fabric.

[0156] Among them, the polyimide aerogel fiber is Preparation Example 13.

[0157] Example 4

[0158] A heat-insulating and warming aerogel fabric is prepared by the following method:

[0159] First, 5.8 kg of polyimide aerogel fiber, 1.8 kg of coffee carbon fiber, and 1 kg of wool fiber are mixed, and then go through the processes of wool mixing, cotton plucking, cotton blending, cotton opening, cotton carding, drawing, friction spinning and winding to obtain yarn; then go through the processes of warping, drawing-in, weaving, finishing and packaging to obtain thermal insulation and warming aerogel fabric;

[0160] Among them, the polyimide aerogel fiber is Preparation Example 14.

[0161] Example 5

[0162] A heat-insulating and warming aerogel fabric is prepared by the following method:

[0163] First, 6kg of polyimide aerogel fiber, 2kg of coffee carbon fiber, and 1kg of wool fiber are mixed, and then go through the processes of wool mixing, cotton plucking, cotton blending, cotton opening, cotton carding, drawing, friction spinning and winding to obtain yarn; then through the processes of warping, drawing-in, weaving, finishing and packaging to obtain thermal insulation and warming aerogel fabric;

[0164] Among them, the polyimide aerogel fiber is Preparation Example 15.

[0165] In order to verify the performance of the thermal insulation and warming aerogel fabrics in Examples 1-5 of the present application, the applicant set up comparative examples 1-10, which are as follows:

[0166] Comparative Example 1

[0167] Comparative Example 1 is the same as Example 1, except that the polyimide aerogel fiber is prepared as Comparative Preparation Example 3.

[0168] Comparative Example 2

[0169] Comparative Example 2 is the same as Example 1, except that the polyimide aerogel fiber is prepared as Comparative Preparation Example 4.

[0170] Comparative Example 3

[0171] Comparative Example 3 is the same as Example 1, except that the polyimide aerogel fiber is prepared as Comparative Preparation Example 5.

[0172] Comparative Example 4

[0173] Comparative Example 4 is the same as Example 1, except that the polyimide aerogel fiber is prepared as Comparative Preparation Example 6.

[0174] Comparative Example 5

[0175] Comparative Example 5 is the same as Example 1, except that the polyimide aerogel fiber is prepared as Comparative Example 7.

[0176] Comparative Example 6

[0177] Comparative Example 6 is the same as Example 1, except that the polyimide aerogel fiber is prepared as Comparative Example 8.

[0178] Comparative Example 7

[0179] Comparative Example 7 is the same as Example 1, except that the polyimide aerogel fiber is prepared as Comparative Example 9.

[0180] Comparative Example 8

[0181] Comparative Example 8 is the same as Example 1, except that the polyimide aerogel fiber is prepared as Comparative Example 10.

[0182] Comparative Example 9

[0183] Comparative Example 9 is the same as Example 1, except that the polyimide aerogel fiber is prepared as Comparative Example 11.

[0184] Comparative Example 10

[0185] Comparative Example 10 is the same as Example 1, except that the polyimide aerogel fiber is prepared as Comparative Preparation Example 12.

[0186] The main properties of the thermal insulation and warming aerogel fabrics in Examples 1-5 and Comparative Examples 1-10 of the present application were tested respectively, and the following result parameters were obtained, as shown in Table 1:

[0187] Mechanical properties test: Tensile strength test was carried out on a universal tensile testing machine according to ASTM D638; the tensile test rate was 45 mm / min;

[0188] Thermal insulation performance test: A flat-plate fabric thermal insulation tester is used for testing. According to the requirements of GB / T11048-1989 "Test method for thermal insulation performance of textiles", the standard human body temperature is set at 36.7°C, and the thermal insulation rate and heat transfer coefficient are calculated by a microcomputer using the constant temperature difference heat dissipation method.

[0189] Table 1:

[0190] Tensile strength / N Insulation rate / % <![CDATA[Heat transfer coefficient / W·m -2 ·℃ -1 > Example 1 142 86.3 18.5 Example 2 165 88.6 17.2 Example 3 174 91.5 15.5 Example 4 182 93.4 15.1 Example 5 175 92.6 16.3 Comparative Example 1 111 80.1 24.3 Comparative Example 2 89 72.2 34.7 Comparative Example 3 103 75.3 32.5 Comparative Example 4 118 81.2 22.6 Comparative Example 5 135 83.8 21.5 Comparative Example 6 108 79.2 23.6 Comparative Example 7 134 83.1 19.4 Comparative Example 8 110 78.9 22.6 Comparative Example 9 105 80.3 21.0 Comparative Example 10 101 77.5 23.6

[0191] From the data shown in Table 1 above, it can be seen that the thermal insulation and warming aerogel fabrics prepared in Examples 1-5 of the present application have a large tensile strength, a thermal insulation rate of more than 85%, and a heat transfer coefficient of 20 W·m -2 ℃ -1 The performance of the thermal insulation and thermal insulation aerogel fabrics prepared in Examples 1-5 is much better than that of Comparative Examples 1-10, indicating that the thermal insulation and thermal insulation aerogel fabrics of the present application have excellent mechanical properties and strong thermal insulation and thermal insulation functions.

[0192] It can be seen from Example 1 and Comparative Examples 1 and 2 that the polyimide aerogel fiber in Example 1 of the present application is prepared by Preparation Example 11, and the modified polyamic acid in Preparation Example 11 is prepared by Preparation Example 6. The raw materials of Preparation Example 6 contain surface-modified nano-silica, and the surface-modified nano-silica is prepared by bis(4-aminophenoxy)dimethylsilane-modified nano-silica. Compared with Comparative Examples 1 and 2, the mechanical properties and thermal insulation properties of the thermal insulation aerogel fabric prepared in Example 1 are better.

[0193] It can be seen from Example 1 and Comparative Examples 3-5 that the polyimide aerogel fiber in Example 1 of the present application is prepared by Preparation Example 11. In addition to the main raw material modified polyamic acid, Preparation Example 11 also includes hemp stalk core ultrafine powder, chitosan, and sophora biosurfactant. Compared with Comparative Examples 3-5, the comprehensive performance of the thermal insulation and warmth aerogel fabric prepared in Example 1 is better than that of Comparative Examples 3-5, indicating that the hemp stalk core ultrafine powder, chitosan, sophora biosurfactant and modified polyamic acid interact with each other and synergistically enhance the effect, so that the final aerogel fabric has significant mechanical properties and thermal insulation and warmth properties.

[0194] It can be seen from Example 1 and Comparative Examples 6 and 7 that the polyimide aerogel fiber in Example 1 of the present application is prepared by Preparation Example 11, and the volume ratio of the spinning solution to the mixed coagulation bath in Preparation Example 11 is 1:10. Compared with Comparative Examples 6 and 7, the tensile strength and thermal insulation rate of the aerogel fabric prepared in Example 1 are higher than those of Comparative Examples 6 and 7, and the comprehensive performance of the aerogel fabric is better.

[0195] It can be seen from Example 1 and Comparative Examples 8-10 that the polyimide aerogel fiber in Example 1 of the present application is prepared by Preparation Example 11, and the mixed coagulation bath in Preparation Example 11 is obtained by mixing water, acetone and ethyl acetate in a volume ratio of 4:2:1; compared with Comparative Examples 8-10, the thermal insulation and mechanical properties of the aerogel fabric prepared in Example 1 are better.

[0196] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. A thermal insulation and warming aerogel fabric, characterized in that: The thermal insulation and warming aerogel fabric is composed of polyimide aerogel fiber, coffee carbon fiber and wool fiber; The polyimide aerogel fiber comprises the following raw materials in parts by weight: 40-60 parts of modified polyamic acid, 10-12 parts of ultrafine hemp stalk core powder, 4-8 parts of chitosan, and 1-2 parts of sophorolipid; The modified polyamic acid comprises the following raw materials in parts by weight: 10-20 parts of surface-modified nano-silica, 20-40 parts of 4,4-diaminodiphenyl ether, 20-40 parts of pyromellitic anhydride, 40-60 parts of melamine, and 60-80 parts of N-methylpyrrolidone; The modified polyamic acid is prepared by the following method: Add 4,4-diaminodiphenyl ether and surface-modified nano-silica to N-methylpyrrolidone, stir at a speed of 500-1000 r / min for 10-20 minutes, then add pyromellitic anhydride and melamine, maintain the same stirring speed, and continue stirring for 30-60 minutes to obtain modified polyamic acid; The surface-modified nano-silica is prepared by the following method: Nano-silica, bis(4-aminophenoxy)dimethylsilane, and toluene are mixed in a mass ratio of 10-20:1-3:30-60, stirred at a speed of 1100-1500 r / min for 5-10 minutes, and then heated under reflux at 60-80° C. for 6-8 hours while maintaining the same stirring speed and continuously introducing nitrogen. After the reaction is completed, the mixture is filtered, washed, and dried to obtain surface-modified nano-silica.

2. The heat-insulating and warming aerogel fabric according to claim 1, characterized in that: The polyimide aerogel fiber is prepared by the following method: S1. Add hemp stalk core ultrafine powder, chitosan, and sophorolipid to the modified polyamic acid, mix well, and then perform vacuum degassing for 20-40 minutes to obtain a spinning solution; S2. Using a wet spinning process, squeeze the spinning solution obtained in step S1 into a 10-20° C. mixing coagulation bath and perform solvent replacement for 8-12 hours to obtain modified polyamic acid hydrogel fibers; S3. The modified polyamic acid hydrogel fiber obtained in step S2 is dried with supercritical carbon dioxide and then thermally stretched to obtain polyimide aerogel fiber.

3. The heat-insulating and warming aerogel fabric according to claim 2, characterized in that: The volume ratio of the spinning solution to the mixed coagulation bath is 1:10-20.

4. The heat-insulating and warming aerogel fabric according to claim 2, characterized in that: The mixed coagulation bath is obtained by mixing water, acetone and ethyl acetate in a volume ratio of 3-6:1-5:

1.

5. The heat-insulating and warming aerogel fabric according to claim 1, characterized in that: The thermal insulation and warming aerogel fabric is prepared by the following method: First, polyimide aerogel fiber, coffee carbon fiber and wool fiber are blended in a mass ratio of 5-6:1-2:1 to obtain yarn; then the yarn is woven to obtain heat-insulating and warming aerogel fabric.