CN114751762A - Method for preparing carbon fiber composite insulation board by using carbon fiber reclaimed materials - Google Patents
Method for preparing carbon fiber composite insulation board by using carbon fiber reclaimed materials Download PDFInfo
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- CN114751762A CN114751762A CN202210571216.8A CN202210571216A CN114751762A CN 114751762 A CN114751762 A CN 114751762A CN 202210571216 A CN202210571216 A CN 202210571216A CN 114751762 A CN114751762 A CN 114751762A
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- insulation board
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 92
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 91
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 238000009413 insulation Methods 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 238000003763 carbonization Methods 0.000 claims abstract description 13
- 239000011268 mixed slurry Substances 0.000 claims abstract description 11
- 238000007654 immersion Methods 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000010000 carbonizing Methods 0.000 claims abstract description 4
- 229920005989 resin Polymers 0.000 claims description 47
- 239000011347 resin Substances 0.000 claims description 47
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 26
- 239000000654 additive Substances 0.000 claims description 23
- 230000000996 additive effect Effects 0.000 claims description 23
- 239000007822 coupling agent Substances 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 13
- 239000004643 cyanate ester Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000004744 fabric Substances 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 239000002562 thickening agent Substances 0.000 claims description 4
- 235000010980 cellulose Nutrition 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- 150000004665 fatty acids Chemical class 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 229920006337 unsaturated polyester resin Polymers 0.000 claims description 3
- 150000002170 ethers Chemical class 0.000 claims description 2
- 239000000835 fiber Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000004064 recycling Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229920000159 gelatin Polymers 0.000 description 2
- 239000008273 gelatin Substances 0.000 description 2
- 235000019322 gelatine Nutrition 0.000 description 2
- 235000011852 gelatine desserts Nutrition 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000010786 composite waste Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007676 flexural strength test Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/524—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
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- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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Abstract
The invention discloses a method for preparing a carbon fiber composite insulation board by using a carbon fiber reclaimed material, which comprises the following steps of: crushing the recycled carbonized felt to obtain carbon fibers with the average length of 1-80 mm; cleaning and drying the ground carbon fibers to obtain crushed carbon fiber materials; mixing the carbon fiber crushed material and the pre-immersion liquid according to the proportion of 1: 1-3, and uniformly stirring to obtain carbon fiber preformed mixed slurry; injecting the carbon fiber pre-formed mixed slurry into a mold, and putting the mold into a drying oven for curing and forming to obtain a cured felt; and (4) demolding the cured felt, and carbonizing the cured felt in a carbonization furnace to obtain the carbon fiber composite insulation board. The carbon fiber composite insulation board prepared by using the carbon fiber reclaimed material can keep the density at 0.1-0.2g/cm3And has high strength and low heat conductivity coefficient.
Description
Technical Field
The invention relates to the field of material preparation, in particular to a method for preparing a carbon fiber composite insulation board by using a carbon fiber reclaimed material.
Background
With the vigorous development of carbon fiber and composite material industry, the reduction of the overall cost has become a consensus in the industry, and the worldwide waste carbon fiber composite material products are increasing year by year Recycling has become an important issue. The waste carbon fiber has extremely high recycling value and can be used for preparing high-performance composite materials again. The existing recovery method is usually a physical recovery method, namely, carbon fiber resin matrix composite waste is crushed and then mixed with an organic binder to prepare a carbon fiber product. The crushed carbon fibers do not have a woven net tire structure and are scattered crushed short fibers. In the prior art, one method is to control the density of the prepared composite material to be 0.1-0.2g/cm3But the structure strength is extremely low, the transportation and the machining cannot be met, and the recycling value is seriously influenced; another is compression molding method, the density of the prepared plate is controlled to be 0.3-0.7g/cm3It has higher bending strength, but the heat conductivity coefficient is more than 1W/m.k, and does not have good heat preservation performance.
Therefore, a method for preparing the carbon fiber composite insulation board by using the carbon fiber recycled material needs to be developed or changed, so that the prepared composite material board has higher strength and lower heat conductivity coefficient.
Disclosure of Invention
Based on the above, in order to solve the problems of low strength or high heat conductivity coefficient of the carbon fiber composite insulation board prepared by the carbon fiber reclaimed material method, the invention provides a method for preparing the carbon fiber composite insulation board by the carbon fiber reclaimed material method, and the specific technical scheme is as follows:
A method for preparing a carbon fiber composite insulation board by using a carbon fiber reclaimed material comprises the following steps:
crushing the recycled carbonized felt to obtain carbon fibers with the average length of 1-80 mm;
cleaning and drying the ground carbon fibers to obtain carbon fiber crushed materials;
mixing the carbon fiber crushed material with the pre-immersion liquid according to the proportion of 1: 1-3, and uniformly stirring to obtain carbon fiber pre-forming mixed slurry;
injecting the carbon fiber pre-forming mixed slurry into a mold, and putting the mold into a drying oven for curing and forming to obtain a cured felt;
demoulding the curing felt, and carbonizing the curing felt in a carbonization furnace to obtain a carbon fiber composite insulation board;
the pre-immersion liquid comprises coupling agent resin mixed liquid and additive water solution;
the coupling agent resin mixed solution comprises resin and a silane coupling agent;
the mass ratio of the coupling agent resin mixed solution to the additive aqueous solution is 1: 2-30;
the mass ratio of the resin to the silane coupling agent is 1: 1-5;
the mass percentage of the additive in the additive water solution is 1-3%;
the density of the carbon fiber composite insulation board is 0.1-0.2g/cm3。
Further, the resin includes one or more of a cyanate ester resin, an unsaturated polyester resin, and a urethane resin.
Further, the additive comprises one or more of cellulose, fatty alcohol, fatty acid, ether, polyacrylate and associative polyurethane thickener.
Further, the cleaning is ultrasonic cleaning.
Further, the drying temperature is 150-200 ℃, and the drying time is 4-6 h.
Furthermore, the stirring speed is 300-1500 r/min.
Further, the curing temperature is 100-200 ℃, and the curing time is 6-12 h.
Further, the carbonization temperature is 1000-1800 ℃, and the carbonization atmosphere is vacuum or inert gas.
Furthermore, a demolding material polytetrafluoroethylene woven cloth is attached to the inside of the mold.
Further, the demolding time is 0.5-3 min.
The method comprises the following steps of crushing the recycled carbonized felt to obtain the carbon fiber which is a scattered short carbon fiber; the crushed carbon fibers do not have a woven net tire structure, and the added silane coupling agent can improve the dispersibility and the adhesive force of the carbon fibers in resin, so that the added short carbon fibers can be regularly arranged and gathered into a net tire-like structure in liquid resin. The net-like tire structure can greatly reduce the heat conductivity coefficient of the manufactured carbon fiber composite insulation board, achieves the effect that the heat conductivity coefficient is less than or equal to 0.5W/m.k, and has good insulation effect. On the other hand, the carbon fiber composite insulation board is often required to be processed into shapes suitable for different thermal fields, so the bonding strength of the product is obvious to the product importance. The addition of the silane coupling agent can not only reduce the density, but also ensure that the horizontal compressive strength of the prepared carbon fiber composite insulation board is more than or equal to 0.5Mpa, so that the carbon fiber composite board has wider usability.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to embodiments thereof. It should be understood that the detailed description and specific examples, while indicating the scope of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In one embodiment of the invention, a method for preparing a carbon fiber composite insulation board by using a carbon fiber reclaimed material comprises the following steps:
crushing the recycled carbonized felt to obtain carbon fibers with the average length of 1-80 mm;
cleaning and drying the ground carbon fibers to obtain carbon fiber crushed materials;
mixing the carbon fiber crushed material with the pre-immersion liquid according to the proportion of 1: 1-3, and uniformly stirring to obtain carbon fiber pre-forming mixed slurry;
Injecting the carbon fiber pre-formed mixed slurry into a mold, and putting the mold into a drying oven for curing and forming to obtain a cured felt;
demolding the cured felt, and carbonizing the cured felt in a carbonization furnace to obtain a carbon fiber composite insulation board;
the pre-immersion liquid comprises coupling agent resin mixed liquid and additive water solution;
the coupling agent resin mixed solution comprises resin and a silane coupling agent;
the mass ratio of the coupling agent resin mixed solution to the additive aqueous solution is 1: 2-30;
the mass ratio of the resin to the silane coupling agent is 1: 1-5;
the mass percentage of the additive in the additive water solution is 1-3%;
the density of the carbon fiber composite insulation board is 0.1-0.2g/cm3。
Preferably, the length of the carbon fiber is 5-30 mm. Further preferably, the length of the carbon fiber is 10-20 mm.
Preferably, the mass ratio of the carbon fiber crushed material to the pre-impregnation liquid is 1: 1 to 2. Further preferably, the mass ratio of the carbon fiber crushed material to the pre-impregnation liquid is 1: 1.5 to 2.
Preferably, the mass ratio of the coupling agent resin mixed solution to the additive aqueous solution is 1: 2-20. More preferably, the mass ratio of the coupling agent resin mixed solution to the additive aqueous solution is 1: 3-5.
Preferably, the mass ratio of the resin to the silane coupling agent is 1: 2 to 4. Further preferably, the mass ratio of the resin to the silane coupling agent is 1: 2.5 to 3.
In one embodiment, the resin comprises one or more of a cyanate ester resin, an unsaturated polyester resin, and a urethane resin. Preferably, the resin is a cyanate ester resin.
In one embodiment, the additive comprises one or more of celluloses, fatty alcohols, fatty acids, ethers, polyacrylates, and associative polyurethane thickeners. Preferably, the additive is a thickener. Further preferably, the additive is gelatin.
In one embodiment, the cleaning is ultrasonic cleaning.
In one embodiment, the drying temperature is 150-200 ℃, and the drying time is 4-6 h.
In one embodiment, the stirring speed is 300-1500 r/min.
In one embodiment, the curing temperature is 100-200 ℃, and the curing time is 6-12 h.
In one embodiment, the carbonization temperature is 1000-1800 ℃, and the carbonization atmosphere is vacuum or inert gas.
In one embodiment, the demolding material polytetrafluoroethylene woven cloth is attached to the inside of the mold.
In one embodiment, the demolding time is 0.5-3 min.
When the silane coupling agent is added into the resin, the coupling agent can improve the bonding strength of the resin, so that the strength of the carbon fiber composite insulation board product is improved. The silane coupling agent works on the principle that it itself has two groups: one group can be combined with the bonded framework material, and the other group can be combined with the high polymer material or the adhesive, so that a chemical bond with higher strength is formed on the bonding interface, and the bonding strength is greatly improved. In the invention, the crushed carbon fibers need to be introduced into a surface treating agent serving as a framework material, and the conventional resin solution is added independently, so that the requirements of high strength and low heat conduction cannot be met simultaneously. The addition of the silane coupling agent can reduce the addition of resin and prepare the low-heat-conduction high-strength recycled carbon fiber composite insulation board. The experiment shows that: when the mass ratio of the resin to the silane coupling agent is 1: 1-5 hours, the carbon fibers are uniformly suspended in the slurry, the fibers of the prepared carbon fiber composite insulation board are in the best transverse tidy arrangement state, and the fibers are in the woven shape similar to a tire net in a transverse cutting mode. When the mass ratio of the resin to the silane coupling agent is lower than 1: 5, the fibers cannot be arranged in order, and the cut surface is spiral and has a gap. When no silane coupling agent is added, the high-strength low-heat-conductivity carbon fiber composite insulation board cannot be prepared, and the powder falling phenomenon exists.
The coupling agent resin mixed solution and the additive aqueous solution have better mixing and using effects, and the silane coupling agent and the additive aqueous solution can uniformly suspend the crushed carbon fibers and the resin in the mixed solution when being mixed and used, so that the crushed carbon fibers can be uniformly suspended in the mixed solution, and the suspended periphery still keeps the system stable in the curing process due to the uniform dispersion and wrapping of the resin system, thereby playing a tire-like net weaving shape, and further ensuring that the carbon fiber composite insulation board product has high strength and low thermal conductivity.
Embodiments of the present invention will be described in detail below with reference to specific examples.
Example 1:
the recovered polyacrylonitrile carbon felt was ground to obtain ground carbon fibers having an average length of 10 mm. And ultrasonically cleaning and drying the ground carbon fibers at the drying temperature of 200 ℃ for 6 hours to obtain clean carbon fiber ground materials. Mixing cyanate ester resin and silane coupling agent according to the mass ratio of 1:2 to obtain a coupling agent resin mixed solution. 5 parts by weight of gelatin were dissolved in 20 parts by weight of water to form an aqueous additive solution. And mixing the coupling agent resin mixed solution and the additive aqueous solution according to the mass ratio of 1:3 to form a pre-immersion liquid. Mixing clean carbon fiber crushed material with pre-immersion liquid according to the proportion of 1: 1.65, and uniformly stirring to obtain the carbon fiber preformed mixed slurry. And (3) injecting the carbon fiber pre-forming mixed slurry into a mold, and internally attaching a demolding material polytetrafluoroethylene woven cloth to facilitate demolding. And placing the carbon-carbon fiber pre-formed mixed slurry and the forming mold into a drying oven for curing and forming to obtain the cured felt. The curing temperature is 160 ℃, and the curing time is 8 h. And (3) demolding the cured felt, and then sending the cured felt into a vacuum carbonization furnace for carbonization at the carbonization temperature of 1700 ℃ to obtain the carbon fiber composite insulation board.
Example 2
The same as example 1, except that the mass ratio of the cyanate ester resin to the silane coupling agent was 1: 2.5.
Example 3
The same as in example 1, except that the mass ratio of the cyanate ester resin to the silane coupling agent was 1: 4.
Example 4
The same as in example 1, except that the mass ratio of the cyanate ester resin to the silane coupling agent was 1: 5.
Example 5
The same as example 1, except that the mass ratio of the cyanate ester resin to the silane coupling agent was 1: 1.
Comparative example 1
The same as in example 1, except that no silane coupling agent was added.
The test method comprises the following steps:
1. the density test method comprises the following steps: the density was tested according to national standard GBT 6343-2009.
2. The flexural strength test method comprises the following steps: and testing the flexural strength by using a universal tensile testing machine.
3. The heat conductivity coefficient test method comprises the following steps: the samples were tested for thermal conductivity using a thermal conductivity meter.
Table 1:
the carbon fiber composite insulation board obtained by the method is uniform in texture, the test densities of the carbon fiber composite insulation board are the same when the carbon fiber composite insulation board is cut at different places, and the fibers are arranged in order. From the data of examples 1 to 5, it can be seen that when a silane coupling agent is added to the process and the mass ratio of resin to silane coupling agent is 1: when the density is 1-5 hours, the density of the obtained carbon fiber composite insulation board is 0.1-0.2g/cm 3The heat conductivity coefficient is kept between 0.22 and 0.50W/m.k, and the heat preservation effect is good; the breaking strength reaches 0.5-1.2 MPa, the strength is high, and the requirements of carrying and machining can be met. As can be seen from the data of comparative example 1, the density of the system of the present method is 0.3g/cm when no silane coupling agent is added3The thermal conductivity coefficient is 1.8W/m.k, which is not in line with the thermal conductivity coefficient range of the thermal insulation material; the breaking strength is as low as 0.1MPa, and the requirement of practical application is not met.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The method for preparing the carbon fiber composite insulation board by using the carbon fiber reclaimed material is characterized by comprising the following steps of:
crushing the recycled carbonized felt to obtain carbon fibers with the average length of 1-80 mm;
cleaning and drying the ground carbon fibers to obtain crushed carbon fiber materials;
mixing the carbon fiber crushed material and the pre-immersion liquid according to the proportion of 1: 1-3, and uniformly stirring to obtain carbon fiber preformed mixed slurry;
injecting the carbon fiber pre-formed mixed slurry into a mold, and putting the mold into a drying oven for curing and forming to obtain a cured felt;
demolding the cured felt, and carbonizing the cured felt in a carbonization furnace to obtain a carbon fiber composite insulation board;
the pre-immersion liquid comprises coupling agent resin mixed liquid and additive water solution;
the coupling agent resin mixed solution comprises resin and a silane coupling agent;
the mass ratio of the coupling agent resin mixed solution to the additive aqueous solution is 1: 2-30;
the mass ratio of the resin to the silane coupling agent is 1: 1-5;
the mass percentage of the additive in the additive water solution is 1-3%.
2. The method of claim 1, wherein the resin comprises one or more of a cyanate ester resin, an unsaturated polyester resin, and a urethane resin.
3. The method of claim 1, wherein the additive comprises one or more of celluloses, fatty alcohols, fatty acids, ethers, polyacrylates, and associative polyurethane thickeners.
4. The method of claim 1, wherein the cleaning is ultrasonic cleaning.
5. The method according to claim 1, wherein the drying temperature is 150-200 ℃ and the drying time is 4-6 h.
6. The method of claim 1, wherein the stirring speed is 300 to 1500 r/min.
7. The method according to claim 1, wherein the curing temperature is 100 to 200 ℃ and the curing time is 6 to 12 hours.
8. The method according to claim 1, wherein the temperature of the carbonization is 1000 to 1800 ℃, and the atmosphere of the carbonization is vacuum or inert gas.
9. The method of claim 1, wherein a release material polytetrafluoroethylene woven cloth is attached to the inside of the mold.
10. The method according to claim 1, wherein the demolding time is 0.5 to 3 min.
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