Preparation process of fireproof safe carbon fiber heating wall cloth

Abstract

The invention relates to the technical field of composite materials, in particular to a preparation process of fireproof safe carbon fiber filament heating wall cloth. The preparation process comprises the following steps: dispersing a modified material on the surface of carbon fiber cloth, preheating to obtain single-layer carbon fiber cloth, stacking multiple layers of single-layer carbon fiber cloth, and sequentially carrying out hot pressing and thermocuring to obtain the fireproof safe carbon fiber filament heating wall cloth, the modified material is prepared from the following raw materials: phthalonitrile resin, a flame retardant, a curing agent, hollow glass beads and the like. According to the preparation process of the fireproof safe carbon fiber heating wall cloth, the fireproof safe carbon fiber heating wall cloth not only has better conductive heating performance, but also has excellent flame retardance and aging resistance, and the quality of the fireproof safe carbon fiber heating wall cloth is effectively guaranteed.

Description

Technical Field

[0001] The invention relates to the technical field of composite materials, in particular to a preparation process of fireproof and safe carbon fiber heating wall cloth. Background Art

[0002] Wall cloth, also known as "wall cloth", is pasted on the wall fabric. In the prior art, most wall cloths are made of cotton cloth as the base cloth, and printed or embossed on the base cloth, and some are woven with large jacquard. Most of the current wall cloths only have the effect of decoration and beauty, and the function is single, which is difficult to meet the needs of consumers for sterilization, heating and other aspects.

[0003] In the patent document with application number "CN201510142382.6" and titled "A method for preparing a flexible and highly conductive composite carbon fiber cloth", it is recorded that "pure natural cellulose cotton cloth is used as a precursor, and 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 under a protective atmosphere, and a strong binding force is generated between the carbon fiber interface and the composite carbon nanotubes or graphene. During the carbonization process, a strong bond is formed between the carbon fiber and the carbon nanotubes and / or graphene to form a coaxial composite carbon fiber cloth. The present invention utilizes different processing temperatures, processing times and nano-carbon composite amounts to regulate the structure and properties of the composite material. The flexible and highly conductive composite carbon fiber cloth solves the problem that ordinary carbon materials cannot have flexibility, high specific surface area and high conductivity at the same time."

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

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

[0006] To achieve the above object, the present invention provides the following technical solutions: The present invention provides a preparation process of a fireproof and safe carbon fiber heating wall cloth. 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: Spreading the modified material on the surface of the carbon fiber cloth for preheating 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 a preparation process for fire-proof and safe carbon fiber wire heating wall cloth.

[0007] Furthermore, the first heating rate is 1-2°C / min, and the second heating rate is 3-5°C / min.

[0008] Furthermore, 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, maleic anhydride is added thereto, 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; Place an appropriate amount of the first material in N,N-dimethylformamide at a dosage ratio of 0.006-0.012 g / mL and ultrasonically disperse for 20-30 min, add 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide thereto, treat for 22-24 h in a nitrogen atmosphere at 230-330 r / min and 125-135° C., filter, wash with anhydrous ethanol and deionized water for 2-4 times, respectively, and dry at 50-60° C. to constant weight to obtain a second material; An appropriate amount of the second material is placed in N,N-dimethylformamide at a dosage ratio of 0.006-0.012 g / mL and ultrasonically dispersed for 20-30 minutes, triglycidyl isocyanurate is added thereto, and treated for 22-24 hours under nitrogen atmosphere, 230-330 r / min, and 150-155° C. After filtration, the material is washed with anhydrous ethanol and deionized water for 2-4 times respectively, and dried at 50-60° C. to constant weight to obtain a flame retardant.

[0009] Furthermore, 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 aminosulfonic acid aqueous solution is placed in the suspension at a mass ratio of 0.008-0.012:1, and treated for 300-320 minutes under a nitrogen atmosphere at 70-80°C. After suction filtration, the suspension is washed with deionized water for 2-4 times, vacuum dried at 50-60°C to constant weight, and crushed to 100-200 meshes to obtain a modified powder.

[0010] Furthermore, the amount of maleic anhydride added is 0.14% to 0.34% of the mass of the modified powder.

[0011] Furthermore, the addition amount of the 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is 0.36% to 0.46% of the mass of the first material.

[0012] Furthermore, the added amount of triglycidyl isocyanurate is 0.13% to 0.23% of the mass of the first material.

[0013] Furthermore, the curing agent is any one of ethylenediamine, hexamethylenediamine and maleic anhydride.

[0014] Furthermore, the number of the stacked layers is 2 to 10, the temperature of the thermal curing is 200 to 220° C., and the time is 4 to 6 hours.

[0015] Compared with the prior art, the present invention has the following beneficial effects: The present invention obtains a single-layer carbon fiber cloth by scattering a modified material on the surface of a carbon fiber cloth for preheating, and then stacking multiple layers of single-layer carbon fiber cloth, and sequentially performing hot pressing and heat curing to obtain a preparation process for a fireproof and safe carbon fiber silk heating wall cloth, wherein the modified material is prepared with phthalonitrile resin, flame retardant, curing agent and hollow glass microbeads as raw materials. The preparation process of the fireproof and safe carbon fiber silk 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, effectively ensuring its quality. The preparation process of the fireproof and safe carbon fiber silk heating wall cloth provided by the present invention has a broader market prospect and is more suitable for promotion. DETAILED DESCRIPTION

[0016] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0017] Embodiment 1: This embodiment provides a preparation process of a fireproof and safe carbon fiber heating wall cloth. The preparation process of the carbon fiber heating wall cloth is as follows: Step 1, preparing carbon fiber cloth; The preparation process of carbon fiber cloth is as follows: An appropriate amount of nanosilver is placed in fluorosilicic acid at a dosage ratio of 0.08 g / mL, and stirred at 120 r / min for 8 hours. After centrifugation, the upper layer solution is taken and evaporated to dryness to obtain a base material; A proper amount of base material and polyethylene oxide were fully mixed at a mass ratio of 1:0.3 to obtain a mixture, and the mixture was then placed in deionized water at a dosage ratio of 0.02 g / mL, and then electrospun at 25° C. to obtain a precursor fiber; 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.

[0018] The first heating rate is 1°C / min, and the second heating rate is 3°C / min.

[0019] Step 2: Spreading the modified material on the surface of the carbon fiber cloth for preheating to obtain a single-layer carbon fiber cloth; Preheating temperature is 180℃, time is 50min 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; In this embodiment, it should be noted that the hollow glass microspheres were purchased from Hebei Huanhe Mineral Products Co., Ltd.

[0020] 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.

[0021] Among them, the preparation process of the flame retardant is as follows: 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; 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; An appropriate amount of the second material was placed in N,N-dimethylformamide at a dosage ratio of 0.006 g / mL and ultrasonically dispersed for 20 minutes. Triglycidyl isocyanurate was added thereto, and the mixture was treated for 22 hours under nitrogen atmosphere, 230 r / min, and 150° C. After filtration, the mixture was washed twice with anhydrous ethanol and deionized water respectively, and dried at 50° C. to constant weight to obtain a flame retardant.

[0022] Further, the preparation process of the modified powder is as follows: An appropriate amount of brucite was ultrasonically dispersed in deionized water at a dosage ratio of 0.02 g / mL, and then treated at 60°C and 220 r / min for 30 min to obtain a suspension; An appropriate amount of aminosulfonic acid aqueous solution was placed in the suspension at a mass ratio of 0.008:1, and treated for 300 minutes under a nitrogen atmosphere at 70°C. After filtration, the suspension was washed twice with deionized water, dried under vacuum at 50°C to constant weight, and crushed to 100 mesh to obtain a modified powder.

[0023] In addition, ethylenediamine is selected as the curing agent.

[0024] In this embodiment, it should be noted that brucite was purchased from Shijiazhuang Oumeiya Mineral Products Co., Ltd.

[0025] Among them, the addition amount of maleic anhydride is 0.14% of the mass of the modified powder.

[0026] The added amount of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is 0.36% of the mass of the first material.

[0027] The added amount of triglycidyl isocyanurate is 0.13% of the mass of the first material.

[0028] 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.

[0029] The number of stacked layers is 2, the thermal curing temperature is 200° C., and the time is 4 hours.

[0030] Example 2: The preparation process of the fireproof safety carbon fiber 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 of the fireproof safety carbon fiber heating wall cloth in this example is different; the specific preparation method of the preparation process of the fireproof safety carbon fiber heating wall cloth in this example is as follows: A preparation process of a fireproof and safe carbon fiber heating wall cloth, the preparation process of the carbon fiber heating wall cloth is as follows: Step 1, preparing carbon fiber cloth; The preparation process of carbon fiber cloth is as follows: 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; 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; 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.

[0031] The first heating rate is 2°C / min, and the second heating rate is 4°C / min.

[0032] Step 2: Spreading the modified material on the surface of the carbon fiber cloth for preheating to obtain a single-layer carbon fiber cloth; Preheating temperature is 185℃, time is 55min 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.

[0033] In this embodiment, it should be noted that the hollow glass microspheres were purchased from Hebei Huanhe Mineral Products Co., Ltd.

[0034] 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.

[0035] Among them, the preparation process of the flame retardant is as follows: An appropriate amount of the modified powder was placed in N,N-dimethylformamide at a dosage ratio of 0.005 g / mL and ultrasonically dispersed for 25 min, maleic anhydride was added thereto, and the mixture was treated for 23 h under nitrogen atmosphere, 280 r / min, and 82° C. After centrifugation, the mixture was washed with deionized water for 3 times and dried at 55° C. to constant weight to obtain a first material; An appropriate amount of the first material was placed in N,N-dimethylformamide at a dosage ratio of 0.009 g / mL and ultrasonically dispersed for 25 min, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide was added thereto, and the mixture was treated for 23 h under a nitrogen atmosphere at 280 r / min and 130° C. After suction filtration, the mixture was washed with anhydrous ethanol and deionized water for 3 times respectively, and dried at 55° C. to constant weight to obtain a second material; An appropriate amount of the second material was placed in N,N-dimethylformamide at a dosage ratio of 0.009 g / mL and ultrasonically dispersed for 25 minutes. Triglycidyl isocyanurate was added thereto, and the mixture was treated for 23 hours under nitrogen atmosphere, 280 r / min, and 152° C. After filtration, the mixture was washed three times with anhydrous ethanol and deionized water respectively, and dried at 55° C. to constant weight to obtain a flame retardant.

[0036] Further, the preparation process of the modified powder is as follows: An appropriate amount of brucite was ultrasonically dispersed in deionized water at a dosage ratio of 0.06 g / mL, and then treated at 65°C and 230 r / min for 35 min to obtain a suspension; An appropriate amount of aminosulfonic acid aqueous solution was placed in the suspension at a mass ratio of 0.01:1, and treated for 310 minutes under a nitrogen atmosphere at 75°C. After filtration, the suspension was washed with deionized water for 3 times, dried in a vacuum at 55°C to a constant weight, and crushed to 150 mesh to obtain a modified powder.

[0037] In addition, hexamethylenediamine is selected as the curing agent.

[0038] In this embodiment, it should be noted that brucite was purchased from Shijiazhuang Oumeiya Mineral Products Co., Ltd.

[0039] Among them, the addition amount of maleic anhydride is 0.24% of the mass of the modified powder.

[0040] The added amount of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is 0.41% of the mass of the first material.

[0041] The added amount of triglycidyl isocyanurate is 0.18% of the mass of the first material.

[0042] 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.

[0043] The number of stacked layers is 2, the thermal curing temperature is 210° C., and the time is 5 hours.

[0044] Example 3: The preparation process of the fireproof safety carbon fiber 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 of the fireproof safety carbon fiber heating wall cloth in this example is different; the specific preparation method of the preparation process of the fireproof safety carbon fiber heating wall cloth in this example is as follows: A preparation process of a fireproof and safe carbon fiber heating wall cloth, the preparation process of the carbon fiber heating wall cloth is as follows: Step 1, preparing carbon fiber cloth; The preparation process of carbon fiber cloth is as follows: An appropriate amount of nanosilver is placed in fluorosilicic acid at a dosage ratio of 0.0012 g / mL, and stirred at 140 r / min for 10 h. After centrifugation, the upper layer solution is taken and evaporated to dryness to obtain a base material; A proper amount of base material and polyethylene oxide were fully mixed at a mass ratio of 1:0.5 to obtain a mixture, and the mixture was then placed in deionized water at a dosage ratio of 0.06 g / mL, and then electrospun at 30° C. to obtain a precursor fiber; The obtained precursor fiber is heated to 230°C at a first heating rate and kept warm for 120 minutes. The obtained product is heated to 720°C at a second heating rate under a nitrogen atmosphere and kept warm for 75 minutes to obtain carbon fiber filaments, which are then interwoven into a cloth using the carbon fiber filaments as weft and warp to obtain carbon fiber cloth.

[0045] The first heating rate is 2°C / min, and the second heating rate is 5°C / min.

[0046] Step 2: Spreading the modified material on the surface of the carbon fiber cloth for preheating to obtain a single-layer carbon fiber cloth; Preheating temperature is 190℃, time is 60min The modified material 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.

[0047] In this embodiment, it should be noted that the hollow glass microspheres were purchased from Hebei Huanhe Mineral Products Co., Ltd.

[0048] 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.

[0049] Among them, the preparation process of the flame retardant is as follows: 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; 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; 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.

[0050] Further, the preparation process of the modified powder is as follows: 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; 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.

[0051] In addition, maleic anhydride is selected as the curing agent.

[0052] In this embodiment, it should be noted that brucite was purchased from Shijiazhuang Oumeiya Mineral Products Co., Ltd.

[0053] Among them, the addition amount of maleic anhydride is 0.34% of the mass of the modified powder.

[0054] The added amount of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is 0.46% of the mass of the first material.

[0055] The added amount of triglycidyl isocyanurate is 0.23% of the mass of the first material.

[0056] 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.

[0057] The number of stacked layers is 2, the thermal curing temperature is 220° C., and the time is 6 hours.

[0058] Comparative Example 1: The difference from Example 1 is that an equal amount of commercially available carbon fiber cloth (Shaanxi Tianheng Aerospace New Materials Co., Ltd.) is used in this example to replace the carbon fiber cloth in Example 1.

[0059] Comparative Example 2: The difference from Example 1 is that this example does not contain a flame retardant.

[0060] Performance test: The carbon fiber heating wall cloth samples provided in Examples 1 to 3 and Comparative Examples 1 to 2 are marked as Examples 1 to 3 and Comparative Examples 1 to 2, respectively; and the relevant properties of the carbon fiber heating wall cloth provided in Examples 1 to 3 and Comparative Examples 1 to 2 are tested as follows: 1. Conductive test: The test method is to use the four-probe method to test the square resistance of each group of carbon fiber heating wall cloth (length 8cm, width 7.5cm, thickness 0.8mm).

[0061] 2. Fire test: The test method is GB8624-2012.

[0062] 3. Aging resistance test: Aging under UV light for 2000h, testing the tensile strength retention rate.

[0063] The obtained test data are recorded in Tables 1 to 3 below.

[0064]

[0065]

[0066]

[0067] By comparing and analyzing the relevant data in Tables 1 and 2, it can be seen that the preparation process of the fireproof safety carbon fiber wire 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, which effectively guarantees its quality. This shows that the preparation process of the fireproof safety carbon fiber wire heating wall cloth provided by the present invention has a broader market prospect and is more suitable for promotion.

[0068] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0069] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. The preparation process of fireproof and safe carbon fiber heating wall cloth is 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: Spreading the modified material on the surface of the carbon fiber cloth for preheating 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 a preparation process for fire-proof and safe carbon fiber wire heating wall cloth.

2. The preparation process of the fireproof safety carbon fiber 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 safety carbon fiber 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, maleic anhydride is added thereto, 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; Place an appropriate amount of the first material in N,N-dimethylformamide at a dosage ratio of 0.006-0.012 g / mL and ultrasonically disperse for 20-30 min, add 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide thereto, treat for 22-24 h in a nitrogen atmosphere at 230-330 r / min and 125-135° C., filter, wash with anhydrous ethanol and deionized water for 2-4 times, respectively, and dry at 50-60° C. to constant weight to obtain a second material; An appropriate amount of the second material is placed in N,N-dimethylformamide at a dosage ratio of 0.006-0.012 g / mL and ultrasonically dispersed for 20-30 minutes, triglycidyl isocyanurate is added thereto, and treated for 22-24 hours under nitrogen atmosphere, 230-330 r / min, and 150-155° C. After filtration, the material is washed with anhydrous ethanol and deionized water for 2-4 times respectively, and dried at 50-60° C. to constant weight to obtain a flame retardant.

4. The preparation process of the fireproof safety carbon fiber heating wall cloth according to claim 3 is characterized in that: 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 aminosulfonic acid aqueous solution is placed in the suspension at a mass ratio of 0.008-0.012:1, and treated for 300-320 minutes under a nitrogen atmosphere at 70-80°C. After suction filtration, the suspension is washed with deionized water for 2-4 times, vacuum dried at 50-60°C to constant weight, and crushed to 100-200 meshes to obtain a modified powder.

5. The preparation process of the fireproof safety carbon fiber heating wall cloth according to claim 3 is characterized in that: The amount of maleic anhydride added is 0.14% to 0.34% of the mass of the modified powder.

6. The preparation process of the fireproof and safe carbon fiber heating wall cloth according to claim 3, characterized in that: The added amount of the 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is 0.36% to 0.46% of the mass of the first material.

7. The preparation process of the fireproof and safe carbon fiber heating wall cloth according to claim 3, characterized in that: The added amount of triglycidyl isocyanurate is 0.13% to 0.23% of the mass of the first material.

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

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

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