Preparation Process of Fireproof and Safe Carbon Fiber Silk Heating Wall Cloth

Abstract

The present invention relates to the technical field of composite materials, specifically to the preparation process of a fire-safe carbon fiber filament heating wall cloth. In the present invention, a modified material is scattered on the surface of a carbon fiber cloth for preheating to obtain a single-layer carbon fiber cloth, and then multiple layers of the single-layer carbon fiber cloth are laminated, and hot pressing and hot curing are carried out in sequence to obtain the preparation process of the fire-safe carbon fiber filament heating wall cloth. Among them, the modified material is prepared from raw materials such as phthalonitrile resin, flame retardant, curing agent, and hollow glass microspheres. The preparation process of the fire-safe carbon fiber filament heating wall cloth prepared by the present invention not only has good conductive heating performance, but also has excellent flame retardant performance and aging resistance performance, effectively ensuring its quality and quality.

Description

Technical Field

[0001] The present invention relates to the technical field of composite materials, and specifically to a preparation process of a fire-safe carbon fiber filament heating wall covering. Background Art

[0002] Wall coverings, also known as "wall fabrics", are fabrics pasted on walls. Most of the existing wall coverings use cotton cloth as the base cloth, and printing or embossing is applied on the base cloth, or some are woven with large jacquards. Most of the current wall coverings only have the single function of decoration and beauty, with a single function and it is difficult to meet the various needs of consumers such as sterilization and heating.

[0003] In the patent document with the application number "CN201510142382.6" and the name "A preparation method of a flexible high-conductive composite carbon fiber cloth", it is recorded that "using pure natural cellulose cotton cloth as a precursor, carbon nanotubes and / or graphene are uniformly compounded with the precursor by an impregnation method, and then the fabric fibers are carbonized by high-temperature heat treatment in a protective atmosphere, and a strong bonding force is generated between the carbon fiber interface and the compounded carbon nanotubes or graphene. During the carbonization process, strong bonding is formed between the carbon fibers and the carbon nanotubes and / or graphene to form a coaxial composite carbon fiber cloth. The present invention uses different treatment temperatures, treatment times and nano-carbon compounding amounts to regulate the structure and properties of the composite material, and this flexible high-conductive composite carbon fiber cloth solves the problem that ordinary carbon materials cannot have both flexibility, high specific surface area and high conductivity."

[0004] Although the carbon fiber filament heating wall covering manufactured by the above patent document has advantages such as conductive heating, its own flame retardant performance is relatively insufficient and still needs further improvement. Based on this, the present invention provides a preparation process of a fire-safe carbon fiber filament heating wall covering to solve the above-mentioned technical problems! Summary of the Invention

[0005] The purpose of the present invention is to provide a preparation process of a fire-safe carbon fiber filament heating wall covering. The prepared fire-safe carbon fiber filament heating wall covering not only has good conductive heating performance, but also has excellent flame retardant performance and aging resistance performance, effectively ensuring its quality and quality.

[0006] To achieve the above purpose, the present invention provides the following technical solutions:

[0007] The present invention provides a preparation process of a fire-safe carbon fiber filament heating wall covering, and the preparation process of the carbon fiber filament heating wall covering is as follows:

[0008] Step 1: Prepare carbon fiber cloth;

[0009] The preparation process of the carbon fiber cloth is as follows:

[0010] A suitable amount of nanosilver is placed in fluorosilicic acid at a dosage ratio of 0.08 to 0.12 g / mL, and stirred at 120 to 140 r / min for 8 to 10 hours. After centrifugation, the upper layer solution is taken and evaporated to dryness to obtain a base material;

[0011] A suitable amount of base material and polyethylene oxide are fully mixed at a mass ratio of 1:0.3-0.5 to obtain a mixture, and then the mixture is placed in deionized water at a dosage ratio of 0.02-0.06 g / mL and mixed, and then the precursor fiber is obtained by electrospinning at 25-30° C.;

[0012] The obtained precursor fiber is heated to 210-230° C. at a first heating rate and kept warm for 100-120 min. The obtained product is heated to 710-720° C. at a second heating rate under a nitrogen atmosphere and kept warm for 65-75 min to obtain carbon fiber filaments. The carbon fiber filaments are then used as wefts and warps to interweave into a cloth to obtain a carbon fiber cloth.

[0013] Step 2: Spreading the modified material on the surface of the carbon fiber cloth for preheating to obtain a single-layer carbon fiber cloth;

[0014] The preheating temperature is 180-190°C and the time is 50-60 minutes

[0015] The modified material is composed of the following raw materials in parts by weight: 20 to 30 parts of phthalonitrile resin, 3 to 6 parts of flame retardant, 3 to 5 parts of curing agent and 6 to 10 parts of hollow glass microspheres;

[0016] The preparation process of the modified material is as follows:

[0017] Accurately weigh the phthalonitrile resin, flame retardant, curing agent and hollow glass microspheres; place the phthalonitrile resin, flame retardant, curing agent and hollow glass microspheres in a stirring device and mix them thoroughly to obtain a modified material;

[0018] Step 3: stack multiple single-layer carbon fiber cloths, perform hot pressing and heat curing in sequence, and obtain a preparation process for fire-proof and safe carbon fiber wire heating wall cloth.

[0019] Furthermore, the first heating rate is 1-2°C / min, and the second heating rate is 3-5°C / min.

[0020] Furthermore, the preparation process of the flame retardant is as follows:

[0021] Disperse an appropriate amount of modified powder in N,N-dimethylformamide by ultrasonic for 20 - 30 min according to the dosage ratio of 0.002 - 0.008 g / mL, add maleic anhydride thereto, and treat it for 22 - 24 h under the conditions of nitrogen atmosphere, 230 - 330 r / min, and 80 - 84 °C. After centrifugation, wash it with deionized water 2 - 4 times, and dry it to constant weight at 50 - 60 °C to obtain the first material;

[0022] Disperse an appropriate amount of the first material in N,N-dimethylformamide by ultrasonic for 20 - 30 min according to the dosage ratio of 0.006 - 0.012 g / mL, add 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide thereto, and treat it for 22 - 24 h under the conditions of nitrogen atmosphere, 230 - 330 r / min, and 125 - 135 °C. After suction filtration, wash it with absolute ethanol and deionized water 2 - 4 times respectively, and dry it to constant weight at 50 - 60 °C to obtain the second material;

[0023] Disperse an appropriate amount of the second material in N,N-dimethylformamide by ultrasonic for 20 - 30 min according to the dosage ratio of 0.006 - 0.012 g / mL, add triglycidyl isocyanurate thereto, and treat it for 22 - 24 h under the conditions of nitrogen atmosphere, 230 - 330 r / min, and 150 - 155 °C. After suction filtration, wash it with absolute ethanol and deionized water 2 - 4 times respectively, and dry it to constant weight at 50 - 60 °C to obtain the flame retardant.

[0024] Furthermore, the preparation process of the modified powder is as follows:

[0025] Disperse an appropriate amount of brucite in deionized water by ultrasonic according to the dosage ratio of 0.02 - 0.12 g / mL, and then treat it for 30 - 40 min under the conditions of 60 - 70 °C and 220 - 240 r / min to obtain a suspension;

[0026] Place an appropriate amount of aqueous amino sulfonic acid solution in the suspension according to the mass ratio of 0.008 - 0.012:1, treat it for 300 - 320 min under the conditions of nitrogen atmosphere and 70 - 80 °C, after suction filtration, wash it with deionized water 2 - 4 times, vacuum dry it to constant weight at 50 - 60 °C, and pulverize it to 100 - 200 meshes to obtain the modified powder.

[0027] Furthermore, the addition amount of maleic anhydride is 0.14% - 0.34% of the mass of the modified powder.

[0028] Furthermore, the addition amount of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is 0.36% - 0.46% of the mass of the first material.

[0029] Further, the addition amount of the triglycidyl isocyanurate is 0.13% to 0.23% of the mass of the first material.

[0030] Further, the curing agent is selected from any one of ethylenediamine, hexamethylenediamine, and maleic anhydride.

[0031] Further, the number of laminated layers is 2 to 10 layers, the temperature of the thermal curing is 200 to 220 °C, and the time is 4 to 6 h.

[0032] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0033] In the present invention, the modified material is dispersed on the surface of the carbon fiber cloth for preheating to obtain a single-layer carbon fiber cloth, and then multiple single-layer carbon fiber cloths are laminated, and hot pressing and thermal curing are carried out in sequence to obtain a preparation process of a fire-safe carbon fiber filament heating wall cloth. Among them, the modified material is prepared from phthalonitrile resin, flame retardant, curing agent, hollow glass microspheres, etc. The preparation process of the fire-safe carbon fiber filament heating wall cloth prepared by the present invention not only has good conductive heating performance, but also has excellent flame retardant performance and aging resistance performance, effectively ensuring its quality and quality. The preparation process of the fire-safe carbon fiber filament heating wall cloth provided by the present invention has a broader market prospect and is more suitable for popularization. Specific Embodiments

[0034] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the scope of protection of the present invention.

[0035] Example 1: This example provides a preparation process of a fire-safe carbon fiber filament heating wall cloth. The preparation process of the carbon fiber filament heating wall cloth is as follows:

[0036] Step 1: Prepare carbon fiber cloth;

[0037] The preparation process of the carbon fiber cloth is as follows:

[0038] An appropriate amount of nano-silver is placed in fluosilicic acid at a dosage ratio of 0.08 g / mL, stirred for 8 h under the condition of 120 r / min, and after centrifugal separation, the upper layer solution is taken and evaporated to dryness to obtain a base material;

[0039] An appropriate amount of the base material and polyethylene oxide are fully mixed at a mass ratio of 1:0.3 to obtain a mixed material, and then the obtained mixed material is placed in deionized water at a dosage ratio of 0.02 g / mL and mixed, and then electrospun at 25 °C to obtain a precursor fiber;

[0040] The obtained precursor fiber is heated to 210°C at a first heating rate and kept warm for 100 minutes. The obtained product is heated to 710°C at a second heating rate under a nitrogen atmosphere and kept warm for 65 minutes to obtain carbon fiber filaments. The carbon fiber filaments are then used as weft and warp to interweave into a cloth to obtain carbon fiber cloth.

[0041] The first heating rate is 1°C / min, and the second heating rate is 3°C / min.

[0042] Step 2: Spreading the modified material on the surface of the carbon fiber cloth for preheating to obtain a single-layer carbon fiber cloth;

[0043] Preheating temperature is 180℃, time is 50min

[0044] The modified material is composed of the following raw materials in parts by weight: 20 parts of phthalonitrile resin, 3 parts of flame retardant, 3 parts of curing agent and 6 parts of hollow glass microspheres;

[0045] In this embodiment, it should be noted that the hollow glass microspheres were purchased from Hebei Huanhe Mineral Products Co., Ltd.

[0046] The preparation process of the modified material is as follows:

[0047] Accurately weigh the phthalonitrile resin, flame retardant, curing agent and hollow glass microspheres; place the phthalonitrile resin, flame retardant, curing agent and hollow glass microspheres in a stirring device and mix them thoroughly to obtain a modified material.

[0048] Among them, the preparation process of the flame retardant is as follows:

[0049] An appropriate amount of the modified powder was placed in N,N-dimethylformamide at a dosage ratio of 0.002 g / mL and ultrasonically dispersed for 20 min, maleic anhydride was added thereto, and the mixture was treated for 22 h under a nitrogen atmosphere, 230 r / min, and 80° C. After centrifugation, the mixture was washed twice with deionized water and dried at 50° C. to constant weight to obtain a first material;

[0050] An appropriate amount of the first material was placed in N,N-dimethylformamide at a dosage ratio of 0.006 g / mL and ultrasonically dispersed for 20 min, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide was added thereto, and the mixture was treated for 22 h under a nitrogen atmosphere at 230 r / min and 125° C. After suction filtration, the mixture was washed twice with anhydrous ethanol and deionized water respectively, and dried at 50° C. to constant weight to obtain a second material;

[0051] An appropriate amount of the second material was ultrasonically dispersed in N,N-dimethylformamide for 20 min at a dosage ratio of 0.006 g / mL, and triglycidyl isocyanurate was added thereto. It was treated for 22 h under the conditions of a nitrogen atmosphere, 230 r / min, and 150 °C. After suction filtration, it was washed twice with absolute ethanol and deionized water respectively, and dried to a constant weight at 50 °C to obtain a flame retardant.

[0052] Furthermore, the preparation process of the modified powder is as follows:

[0053] An appropriate amount of brucite was ultrasonically dispersed in deionized water at a dosage ratio of 0.02 g / mL, and then treated for 30 min under the conditions of 60 °C and 220 r / min to obtain a suspension;

[0054] An appropriate amount of aqueous amino sulfonic acid solution was placed in the suspension at a mass ratio of 0.008:1, and treated for 300 min under the conditions of a nitrogen atmosphere and 70 °C. After suction filtration, it was washed twice with deionized water, vacuum dried to a constant weight at 50 °C, and pulverized to 100 meshes to obtain the modified powder.

[0055] In addition, ethylenediamine was used as the curing agent.

[0056] In this example, it should be noted that the brucite was purchased from Shijiazhuang Oumeiya Mineral Products Co., Ltd.

[0057] Among them, the addition amount of maleic anhydride was 0.14% of the mass of the modified powder.

[0058] The addition amount of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide was 0.36% of the mass of the first material.

[0059] The addition amount of triglycidyl isocyanurate was 0.13% of the mass of the first material.

[0060] Step 3: Stack multiple single-layer carbon fiber cloths, and perform hot pressing and hot curing in sequence to obtain a preparation process for a fire-safe carbon fiber filament heating wall cloth.

[0061] Among them, the number of stacked layers was 2 layers, the temperature of hot curing was 200 °C, and the time was 4 h.

[0062] Example 2: The preparation process of the fire-safe carbon fiber filament heating wall cloth provided in this example was basically the same as that in Example 1, except that: the specific preparation method of the preparation process of the fire-safe carbon fiber filament heating wall cloth in this example was different; the specific preparation method of the preparation process of the fire-safe carbon fiber filament heating wall cloth in this example was as follows:

[0063] A preparation process for a fire-safe carbon fiber filament heating wall cloth, and the preparation process of the carbon fiber filament heating wall cloth is as follows:

[0064] Step 1, preparing carbon fiber cloth;

[0065] The preparation process of carbon fiber cloth is as follows:

[0066] An appropriate amount of nanosilver is placed in fluorosilicic acid at a dosage ratio of 0.1 g / mL, and stirred at 130 r / min for 9 hours. After centrifugation, the upper layer solution is taken and evaporated to dryness to obtain a base material;

[0067] A proper amount of base material and polyethylene oxide were fully mixed at a mass ratio of 1:0.4 to obtain a mixture, and the mixture was then placed in deionized water at a dosage ratio of 0.04 g / mL and mixed, and then electrospun at 27° C. to obtain precursor fibers;

[0068] The obtained precursor fiber was heated to 220°C at a first heating rate and kept warm for 110 minutes. The obtained product was heated to 715°C at a second heating rate under a nitrogen atmosphere and kept warm for 70 minutes to obtain carbon fiber filaments, which were then interwoven into cloth using the carbon fiber filaments as weft and warp to obtain carbon fiber cloth.

[0069] The first heating rate is 2°C / min, and the second heating rate is 4°C / min.

[0070] Step 2: Spreading the modified material on the surface of the carbon fiber cloth for preheating to obtain a single-layer carbon fiber cloth;

[0071] Preheating temperature is 185℃, time is 55min

[0072] The modified material is composed of the following raw materials in parts by weight: 25 parts of phthalonitrile resin, 4 parts of flame retardant, 4 parts of curing agent and 8 parts of hollow glass microspheres.

[0073] In this embodiment, it should be noted that the hollow glass microspheres were purchased from Hebei Huanhe Mineral Products Co., Ltd.

[0074] The preparation process of the modified material is as follows:

[0075] Accurately weigh the phthalonitrile resin, flame retardant, curing agent and hollow glass microspheres; place the phthalonitrile resin, flame retardant, curing agent and hollow glass microspheres in a stirring device and mix them thoroughly to obtain a modified material.

[0076] Among them, the preparation process of the flame retardant is as follows:

[0077] Disperse an appropriate amount of modified powder in N,N-dimethylformamide at a dosage ratio of 0.005 g / mL by ultrasonic treatment for 25 min, add maleic anhydride thereto, and treat it under the conditions of a nitrogen atmosphere, 280 r / min, and 82 °C for 23 h. After centrifugation, wash it three times with deionized water, and dry it to a constant weight at 55 °C to obtain the first material;

[0078] Disperse an appropriate amount of the first material in N,N-dimethylformamide at a dosage ratio of 0.009 g / mL by ultrasonic treatment for 25 min, add 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide thereto, and treat it under the conditions of a nitrogen atmosphere, 280 r / min, and 130 °C for 23 h. After suction filtration, wash it three times with anhydrous ethanol and deionized water respectively, and dry it to a constant weight at 55 °C to obtain the second material;

[0079] Disperse an appropriate amount of the second material in N,N-dimethylformamide at a dosage ratio of 0.009 g / mL by ultrasonic treatment for 25 min, add triglycidyl isocyanurate thereto, and treat it under the conditions of a nitrogen atmosphere, 280 r / min, and 152 °C for 23 h. After suction filtration, wash it three times with anhydrous ethanol and deionized water respectively, and dry it to a constant weight at 55 °C to obtain the flame retardant.

[0080] Furthermore, the preparation process of the modified powder is as follows:

[0081] Disperse an appropriate amount of brucite in deionized water at a dosage ratio of 0.06 g / mL, and then treat it under the conditions of 65 °C and 230 r / min for 35 min to obtain a suspension;

[0082] Place an appropriate amount of aqueous amino sulfonic acid solution in the suspension at a mass ratio of 0.01:1, treat it under the conditions of a nitrogen atmosphere and 75 °C for 310 min, after suction filtration, wash it three times with deionized water, vacuum dry it to a constant weight at 55 °C, and pulverize it to 150 meshes to obtain the modified powder.

[0083] In addition, the curing agent is selected as hexamethylenediamine.

[0084] In this embodiment, it should be noted that the brucite is purchased from Shijiazhuang Oumeiya Mineral Products Co., Ltd.

[0085] Among them, the addition amount of maleic anhydride is 0.24% of the mass of the modified powder.

[0086] The addition amount of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is 0.41% of the mass of the first material.

[0087] The addition amount of triglycidyl isocyanurate is 0.18% of the mass of the first material.

[0088] Step 3: Stack multiple single-layer carbon fiber cloths, and perform hot pressing and hot curing in sequence to obtain a preparation process for a fire-safe carbon fiber filament heating wall cloth.

[0089] Among them, the number of stacked layers is 2 layers, the temperature of hot curing is 210 °C, and the time is 5 h.

[0090] Example 3: The preparation process for the fire-safe carbon fiber filament heating wall cloth provided in this example is basically the same as that in Example 1, except that: the specific preparation method of the preparation process for the fire-safe carbon fiber filament heating wall cloth in this example is different; the specific preparation method of the preparation process for the fire-safe carbon fiber filament heating wall cloth in this example is as follows:

[0091] A preparation process for a fire-safe carbon fiber filament heating wall cloth, and the preparation process of the carbon fiber filament heating wall cloth is as follows:

[0092] Step 1: Prepare carbon fiber cloth;

[0093] The preparation process of the carbon fiber cloth is as follows:

[0094] Place an appropriate amount of nano-silver in fluosilicic acid according to a dosage ratio of 00.12 g / mL, stir for 10 h under the condition of 140 r / min, after centrifugal separation, take the upper layer solution, and after evaporation to dryness, obtain a base material;

[0095] Fully mix an appropriate amount of the base material and polyethylene oxide according to a mass ratio of 1:0.5 to obtain a mixture, and then place the obtained mixture in deionized water according to a dosage ratio of 0.06 g / mL and mix, and then obtain a precursor fiber by electrospinning under the condition of 30 °C;

[0096] Heat the obtained precursor fiber to 230 °C at a first heating rate and keep it for 120 min. The obtained product is heated to 720 °C at a second heating rate in a nitrogen atmosphere and kept for 75 min to obtain carbon fiber filaments, and then use the carbon fiber filaments as weft and warp to interweave into a cloth shape to obtain carbon fiber cloth.

[0097] Among them, the first heating rate is 2 °C / min, and the second heating rate is 5 °C / min.

[0098] Step 2: Spread the modifier on the surface of the carbon fiber cloth for preheating to obtain a single-layer carbon fiber cloth;

[0099] The preheating temperature is 190 °C, and the time is 60 min

[0100] The modifier is composed of the following raw materials in parts by weight: 30 parts of phthalonitrile resin, 6 parts of flame retardant, 5 parts of curing agent, and 10 parts of hollow glass microspheres.

[0101] In this embodiment, it should be noted that the hollow glass microspheres were purchased from Hebei Huanhe Mineral Products Co., Ltd.

[0102] The preparation process of the modified material is as follows:

[0103] Accurately weigh the phthalonitrile resin, flame retardant, curing agent and hollow glass microspheres; place the phthalonitrile resin, flame retardant, curing agent and hollow glass microspheres in a stirring device and mix them thoroughly to obtain a modified material.

[0104] Among them, the preparation process of the flame retardant is as follows:

[0105] An appropriate amount of the modified powder was placed in N,N-dimethylformamide at a dosage ratio of 0.008 g / mL and ultrasonically dispersed for 30 min, and maleic anhydride was added thereto, and the mixture was treated under nitrogen atmosphere, 330 r / min, and 84° C. for 24 h. After centrifugation, the mixture was washed with deionized water for 4 times, and dried at 60° C. to constant weight to obtain a first material;

[0106] An appropriate amount of the first material was placed in N,N-dimethylformamide at a dosage ratio of 0.012 g / mL and ultrasonically dispersed for 30 min, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide was added thereto, and the mixture was treated in a nitrogen atmosphere at 330 r / min and 135° C. for 24 h. After suction filtration, the mixture was washed with anhydrous ethanol and deionized water for 4 times respectively, and dried at 60° C. to constant weight to obtain a second material;

[0107] An appropriate amount of the second material was placed in N,N-dimethylformamide at a dosage ratio of 0.012 g / mL and ultrasonically dispersed for 30 minutes. Triglycidyl isocyanurate was added thereto, and the mixture was treated for 24 hours under nitrogen atmosphere, 330 r / min, and 155° C. After filtration, the mixture was washed with anhydrous ethanol and deionized water for 4 times respectively, and dried at 60° C. to constant weight to obtain a flame retardant.

[0108] Further, the preparation process of the modified powder is as follows:

[0109] An appropriate amount of brucite was ultrasonically dispersed in deionized water at a dosage ratio of 0.12 g / mL, and then treated at 70°C and 240 r / min for 40 min to obtain a suspension;

[0110] An appropriate amount of aminosulfonic acid aqueous solution was placed in the suspension at a mass ratio of 0.012:1, and treated for 320 minutes in a nitrogen atmosphere at 80°C. After filtration, the suspension was washed with deionized water for 4 times, vacuum dried at 60°C to constant weight, and crushed to 200 mesh to obtain a modified powder.

[0111] In addition, maleic anhydride is selected as the curing agent.

[0112] In this embodiment, it should be noted that brucite was purchased from Shijiazhuang Omeiya Mineral Products Co., Ltd.

[0113] Among them, the addition amount of maleic anhydride is 0.34% of the mass of the modified powder.

[0114] The addition amount of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is 0.46% of the mass of the first material.

[0115] The addition amount of triglycidyl isocyanurate is 0.23% of the mass of the first material.

[0116] Step 3: Stack multiple single-layer carbon fiber cloths, and perform hot pressing and hot curing in sequence to obtain a preparation process for a fire-safe carbon fiber filament heating wall cloth.

[0117] Among them, the number of stacked layers is 2 layers, the temperature of hot curing is 220 °C, and the time is 6 h.

[0118] Comparative Example 1: The difference from Example 1 is that in this example, an equal amount of commercially available carbon fiber cloth (Shaanxi Tianheng Aerospace New Materials Co., Ltd.) is used to replace the carbon fiber cloth in Example 1.

[0119] Comparative Example 2: The difference from Example 1 is that this example does not contain a flame retardant.

[0120] Performance test: The carbon fiber filament heating wall cloth samples provided in Examples 1 to 3 and Comparative Examples 1 to 2 are respectively marked as Examples 1 to 3 and Comparative Examples 1 to 2; and the following tests are respectively carried out on the relevant performances of the carbon fiber filament heating wall cloths provided in Examples 1 to 3 and Comparative Examples 1 to 2:

[0121] 1. Conductivity test: The test method is to use the four-probe method to test the sheet resistance of each group of carbon fiber filament heating wall cloths (8 cm long, 7.5 cm wide, and 0.8 mm thick).

[0122] 2. Fire resistance test: The test method is GB8624-2012.

[0123] 3. Aging resistance test: Aging for 2000 h under ultraviolet light, and testing the tensile strength retention rate.

[0124] The obtained test data are recorded in Tables 1 to 3 below.

[0125]

[0126]

[0127]

[0128] By comparing and analyzing the relevant data in Tables 1 to 2, it can be seen that the preparation process of the fire-safe carbon fiber filament heating wall cloth prepared by the present invention not only has good electrothermal performance, but also has excellent flame retardancy and aging resistance, effectively ensuring its quality and quality. This shows that the preparation process of the fire-safe carbon fiber filament heating wall cloth provided by the present invention has a broader market prospect and is more suitable for popularization.

[0129] In the description of this specification, the description referring to terms such as "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in a suitable manner in any one or more embodiments or examples.

[0130] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific embodiments described. Obviously, many modifications and variations can be made according to the content of this specification. These embodiments are selected and specifically described in this specification to better explain the principles and practical applications of the present invention, so that those skilled in the art can well understand and utilize the present invention. The present invention is only limited by the claims and their full scope and equivalents.

Claims

1. Preparation process of a fire-safe carbon fiber filament heating wall covering, characterized in that, The preparation process of the carbon fiber heating wall cloth is as follows: Step 1, preparing carbon fiber cloth; The preparation process of the carbon fiber cloth is as follows: A suitable amount of nanosilver is placed in fluorosilicic acid at a dosage ratio of 0.08 to 0.12 g / mL, and stirred at 120 to 140 r / min for 8 to 10 hours. After centrifugation, the upper layer solution is taken and evaporated to dryness to obtain a base material; A suitable amount of base material and polyethylene oxide are fully mixed at a mass ratio of 1:0.3-0.5 to obtain a mixture, and then the mixture is placed in deionized water at a dosage ratio of 0.02-0.06 g / mL and mixed, and then the precursor fiber is obtained by electrospinning at 25-30° C.; The obtained precursor fiber is heated to 210-230° C. at a first heating rate and kept warm for 100-120 min. The obtained product is heated to 710-720° C. at a second heating rate under a nitrogen atmosphere and kept warm for 65-75 min to obtain carbon fiber filaments. The carbon fiber filaments are then used as wefts and warps to interweave into a cloth to obtain a carbon fiber cloth. Step 2: dispersing the modified material on the surface of the carbon fiber cloth and preheating it to obtain a single-layer carbon fiber cloth; The preheating temperature is 180-190°C and the time is 50-60 minutes; The modified material is composed of the following raw materials in parts by weight: 20 to 30 parts of phthalonitrile resin, 3 to 6 parts of flame retardant, 3 to 5 parts of curing agent and 6 to 10 parts of hollow glass microspheres; The preparation process of the modified material is as follows: Accurately weigh the phthalonitrile resin, flame retardant, curing agent and hollow glass microspheres; place the phthalonitrile resin, flame retardant, curing agent and hollow glass microspheres in a stirring device and mix them thoroughly to obtain a modified material; Step 3: stack multiple single-layer carbon fiber cloths, perform hot pressing and heat curing in sequence, and obtain fireproof and safe carbon fiber wire heating wall cloth.

2. The preparation process of the fireproof and safe carbon fiber filament heating wall cloth according to claim 1, characterized in that, The first heating rate is 1-2°C / min, and the second heating rate is 3-5°C / min.

3. The preparation process of the fireproof and safe carbon fiber filament heating wall cloth according to claim 1, characterized in that, The preparation process of the flame retardant is as follows: An appropriate amount of modified powder is placed in N,N-dimethylformamide at a dosage ratio of 0.002-0.008 g / mL and ultrasonically dispersed for 20-30 min, and maleic anhydride is added thereto, wherein the amount of maleic anhydride added is 0.14%-0.34% of the mass of the modified powder, and the mixture is treated for 22-24 h in a nitrogen atmosphere at 230-330 r / min and 80-84° C. After centrifugation, the mixture is washed with deionized water for 2-4 times, and dried at 50-60° C. to constant weight to obtain a first material; The preparation process of the modified powder is as follows: An appropriate amount of brucite is ultrasonically dispersed in deionized water at a dosage ratio of 0.02 to 0.12 g / mL, and then treated at 60 to 70° C. and 220 to 240 r / min for 30 to 40 minutes to obtain a suspension; An appropriate amount of aqueous sulfamic acid solution was placed in the suspension according to a mass ratio of 0.008 to 0.012:1, and treated under a nitrogen atmosphere at 70 to 80 °C for 300 to 320 min. After suction filtration, it was washed 2 to 4 times with deionized water, vacuum dried at 50 to 60 °C to constant weight, and pulverized to 100 to 200 mesh to obtain the modified powder. An appropriate amount of the first material was ultrasonically dispersed in N,N-dimethylformamide for 20 to 30 min according to a dosage ratio of 0.006 to 0.012 g / mL. 9,10-Dihydro-9-oxa-10-phosphaphenanthrene-10-oxide was added thereto, and the addition amount of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide was 0.36% to 0.46% of the mass of the first material. It was treated under a nitrogen atmosphere at 230 to 330 r / min and 125 to 135 °C for 22 to 24 h. After suction filtration, it was washed 2 to 4 times with absolute ethanol and deionized water respectively, and dried to constant weight at 50 to 60 °C to obtain the second material. An appropriate amount of the second material was ultrasonically dispersed in N,N-dimethylformamide for 20 to 30 min according to a dosage ratio of 0.006 to 0.012 g / mL. Triglycidyl isocyanurate was added thereto, and the addition amount of triglycidyl isocyanurate was 0.13% to 0.23% of the mass of the first material. It was treated under a nitrogen atmosphere at 230 to 330 r / min and 150 to 155 °C for 22 to 24 h. After suction filtration, it was washed 2 to 4 times with absolute ethanol and deionized water respectively, and dried to constant weight at 50 to 60 °C to obtain the flame retardant.

4. The preparation process of the fireproof and safe carbon fiber filament heating wall cloth according to claim 1, characterized in that, The curing agent is selected from any one of ethylenediamine, hexamethylenediamine, and maleic anhydride.

5. The preparation process of the fireproof and safe carbon fiber filament heating wall cloth according to claim 1, characterized in that, The number of stacked layers is 2 to 10 layers, the temperature of thermal curing is 200 to 220 °C, and the time is 4 to 6 h.

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