CN115216064A - Carbon fiber reinforced graphene plate and preparation method thereof - Google Patents

Carbon fiber reinforced graphene plate and preparation method thereof Download PDF

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Publication number
CN115216064A
CN115216064A CN202210862690.6A CN202210862690A CN115216064A CN 115216064 A CN115216064 A CN 115216064A CN 202210862690 A CN202210862690 A CN 202210862690A CN 115216064 A CN115216064 A CN 115216064A
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film
heating
carbon fiber
flame
base film
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CN115216064B (en
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金永明
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Zhejiang Wanjianuan Intelligent Technology Co ltd
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Zhejiang Wanjianuan Intelligent Technology Co ltd
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    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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    • H—ELECTRICITY
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    • H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
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Abstract

The invention discloses a carbon fiber reinforced graphene plate and a preparation method thereof, the graphene plate sequentially comprises a curing sheet, a heating film, a curing sheet, a shielding film and a curing sheet from bottom to top, the heating film is prepared by punching a plurality of hexagonal through holes which are uniformly distributed on a heating base film by using the heating base film and raw materials, and riveting conductive copper foil on the periphery of the heating base film in a riveting manner, the heating base film takes flame-retardant resin as a base material, the flame-retardant resin contains a large amount of sulfonate, can be decomposed into sulfate and sulfite salt flame-retardant substances at high temperature, can effectively resist flame, and simultaneously magnesium hydroxide in composite carbon fibers can release a large amount of water vapor at high temperature to rapidly cool, so that the flame-retardant effect is further improved, the surface of the heating base film contains a layer of nano silicon dioxide, and can be matched with the original flame-retardant components of the heating base film during combustion to rapidly form a compact carbon layer, so that open flame can be effectively isolated from being contacted with the film, and the rapid flame-retardant effect is achieved.

Description

Carbon fiber reinforced graphene plate and preparation method thereof
Technical Field
The invention relates to the technical field of graphene material preparation, in particular to a carbon fiber reinforced graphene plate and a preparation method thereof.
Background
The carbon fiber paper can be widely applied to energy materials, electromagnetic wave shielding materials, anti-static packaging materials and heating materials. Acoustic materials, adsorption separation materials, aerospace materials and the like. The carbon fiber non-woven paper is made up by using synthetic fiber, conductive phase carbon fiber and fibrous adhesive, and adopting the processes of water-phase dispersion by using high-molecular polymer dispersing agent, defibering and mixing, and adopting wet-process non-woven fabric forming process. The carbon fiber planar heating material has the characteristics of light weight, uniform heating, safety, reliability and high thermal efficiency, and is a novel carbon fiber planar heating material. The electrical property is stable, and the power attenuation phenomenon can not appear after long-time electrification. Alternating current and direct current power supplies from 12V to 380V can be used, and the heating temperature can be from 30 ℃ to over 800 ℃; has high mechanical strength, good flexibility, good air permeability and temperature resistance, is convenient for cutting and processing, and can be made into heating materials with various shapes. Has physiotherapy and health promotion effects, and can be made into electric heating picture, wall heating, floor heating, electric heating plate, antistatic package, electromagnetic wave shielding, electric heating clothing, cushion, electric blanket, physiotherapy pad, etc. With the continuous improvement of the composite technology, the application field of the carbon fiber paper is necessarily further widened.
Disclosure of Invention
The invention aims to provide a carbon fiber reinforced graphene plate and a preparation method thereof, and solves the problems that the graphene plate is poor in flame retardant effect and general in mechanical property at the present stage.
The purpose of the invention can be realized by the following technical scheme:
the utility model provides a carbon fiber reinforced graphene board, includes curing piece, heating film, curing piece, shielding film, curing piece from bottom to top in proper order.
Further, the curing sheet is prepared by the following steps:
mixing nano-cellulose, graphene and deionized water, carrying out ultrasonic treatment for 30-40min under the condition of power of 800-1000W to obtain a mixed solution, filtering the mixed solution, carrying out compression molding on a substrate and drying to obtain a pretreated film, placing the pretreated film into a sealed dryer, placing the sealed dryer into a beaker filled with excessive perfluorodecyl trimethoxy silane, and carrying out heat preservation treatment for 40-50min under the condition of temperature of 250-260 ℃ to obtain a cured sheet.
Further, the mass ratio of the nanocellulose to the graphene is 3.
Further, the heat-generating base film is prepared by the following steps:
step A1: uniformly mixing benzhydryl alcohol, DMF and N-bromosuccinimide, stirring for 5-7h at the rotation speed of 150-200r/min and the temperature of 20-25 ℃, extracting with trichloromethane, filtering to remove filter residue, distilling the filtrate to remove a solvent, uniformly mixing a substrate, 4-methoxyphenylboronic acid, tetrakis (triphenylphosphine) palladium, dioxane and potassium carbonate, and carrying out reflux reaction for 8-10h at the temperature of 105-110 ℃ to prepare an intermediate 1;
the reaction process is as follows:
Figure BDA0003757311560000021
step A2: uniformly mixing the intermediate 1, cyanuric chloride, tetrahydrofuran and sodium hydroxide, reacting for 6-8h at the rotation speed of 150-200r/min and the temperature of 0-5 ℃, adding 3-aminopropyl sodium sulfonate, heating to the temperature of 80-90 ℃, continuing to react for 8-10h to obtain an intermediate 2, mixing the intermediate 2 and dichloromethane, introducing nitrogen for protection, stirring and dropwise adding boron tribromide at the rotation speed of 200-300r/min and the temperature of 0-3 ℃, and reacting for 5-7h to obtain an intermediate 3;
step A3: uniformly mixing the intermediate 3, 4' -dibromobenzophenone and diphenyl sulfone, stirring for 5-10min at the rotation speed of 200-300r/min and at the temperature of 130-140 ℃, adding sodium carbonate and potassium carbonate, heating to the temperature of 180-220 ℃, reacting for 2-3h, heating to the temperature of 250-260 ℃, reacting for 1-2h, adding acetone, settling, refluxing for 30-40min, and finally drying in vacuum to obtain the flame-retardant resin;
step A4: uniformly mixing the flame-retardant resin and the composite carbon fiber, performing mould pressing for 10-15min at the temperature of 380-385 ℃ and the pressure of 2-3MPa, uniformly mixing tetraethoxysilane and deionized water, adjusting the pH value to 6, soaking the film in the mixture at the temperature of 60-65 ℃, taking out the film after soaking for 30-40min, and drying the film to obtain the heating base film.
Further, the dosage ratio of the benzhydrol, the DMF, the N-bromosuccinimide, the 4-methoxyphenylboronic acid, the tetrakis (triphenylphosphine) palladium, the dioxane and the potassium carbonate in the step A1 is 0.1mol, 30ml, 0.22mol.
Further, the molar ratio of the intermediate 1, cyanuric chloride and 3-aminopropyl sodium sulfonate in the step A2 is 1.
Further, the mass ratio of the intermediate 3, 4' -dibromobenzophenone, diphenyl sulfone, sodium carbonate and potassium carbonate in step A3 is 10.35.
Further, the dosage of the composite carbon fiber in the step A4 is 25-35% of the mass of the flame-retardant resin, and the dosage ratio of the ethyl orthosilicate to the deionized water is 1g.
The composite carbon fiber is prepared by the following steps:
step B1: placing carbon fibers into a muffle furnace, roasting for 30-40min at the temperature of 400-450 ℃, adding the carbon fibers into a sodium hydroxide solution, soaking for 1-1.5h, filtering and drying to obtain pretreated carbon fibers, dispersing the pretreated carbon fibers in deionized water, adding KH550, stirring for 20-30min at the rotation speed of 600-800r/min and the temperature of 30-35 ℃, filtering and drying to obtain modified carbon fibers;
and step B2: dispersing magnesium hydroxide in deionized water, adding KH560, stirring at 600-800r/min and 30-35 deg.C for 20-30min, filtering, oven drying, dispersing filter cake and modified carbon fiber in deionized water, reacting at 200-300r/min and alkaline pH for 2-3h, filtering, and oven drying to obtain the composite carbon fiber.
Further, the mass fraction of the sodium hydroxide solution in the step B1 is 10%, and the dosage of the KH550 is 5-8% of the mass of the pretreated carbon fiber.
Further, the dosage of KH560 in the step B2 is 5-8% of the mass of the magnesium hydroxide, and the mass ratio of the filter cake to the modified carbon fiber is 1.
The shielding film is prepared by the following steps:
adding carbon fibers into a vacuum tube type sintering furnace, placing a copper substrate in the middle of a quartz tube, adding a ferrocene ethanol solution into a liquid input pump, vacuumizing, introducing nitrogen, heating at the speed of 10 ℃/min, conveying the ferrocene ethanol solution to a reaction area when the temperature is 1100-1150 ℃, reacting for 20-30min, and stripping the copper substrate to obtain the shielding film.
The mass fraction of the ferrocene ethanol solution is 10-13%.
A preparation method of a carbon fiber reinforced graphene plate specifically comprises the following steps:
step S1: cutting the curing sheet, the heating base film and the shielding film to required sizes, punching a plurality of hexagonal through holes which are uniformly distributed on the cut heating base film, and riveting the periphery of the heating base film with a conductive copper foil in a riveting manner to obtain the heating film;
step S2: sequentially placing a curing sheet, a heating film, a curing sheet, a shielding film and a curing sheet from bottom to top, coating polyethylene glycol 200 between adjacent films, and performing high-temperature tabletting for 20-30min under the conditions that the temperature is 300-310 ℃ and the pressure is 2-3MPa to obtain the carbon fiber reinforced graphene plate.
The invention has the beneficial effects that: the carbon fiber reinforced graphene plate prepared by the invention sequentially comprises a curing sheet, a heating film, a curing sheet, a shielding film and a curing sheet from bottom to top, wherein the curing sheet is prepared by compounding graphene and nano-cellulose serving as raw materials, a pretreatment film is prepared by performing vapor deposition on the pretreatment film by using perfluorodecyl trimethoxysilane, a hydrophobic film is formed on the surface of the film, the heating effect of the graphene plate is ensured not to be influenced by a damp environment, the mechanical performance of the prepared graphene plate is greatly improved by compounding the cellulose and the graphene, the heating film is prepared by punching a plurality of uniformly distributed hexagonal through holes on the heating base film by using the heating base film and the raw materials, and riveting a conductive copper foil on the periphery of the heating base film in a riveting manner, so that the heating film can uniformly dissipate heat, the thermal efficiency is improved, and the conductive copper foil is riveted by using the riveting manner, the method comprises the steps of enabling conductive copper to be in close contact with a heating substrate to ensure that current is uniformly distributed, avoiding the use of an adhesive, avoiding the possibility of aging due to overlong time, treating the heating base film by using benzhydryl alcohol as a raw material through N-bromosuccinimide, then reacting the diphenyl carbinol with 4-methoxyphenylboronic acid to obtain an intermediate 1, controlling the temperature of the intermediate 1 and cyanuric chloride to enable one chlorine atom site on the cyanuric chloride to react with hydroxyl on the intermediate 1, adding 3-aminopropyl sodium sulfonate, heating to react with the remaining two chlorine atom sites to obtain an intermediate 2, removing ether from the intermediate 2 through boron tribromide to obtain an intermediate 3, polymerizing the intermediate 3 and 4,4' -dibromobenzophenone to form polyether-ether-ketone to obtain flame-retardant resin, carrying out high-temperature mould pressing on the flame-retardant resin and composite carbon fibers, and soaking the flame-retardant resin and the composite carbon fibers through ethyl orthosilicate to obtain the heating base film, after the surface of the carbon fiber is pretreated, KH550 treatment is carried out again to graft a large amount of amino on the surface of the carbon fiber, modified carbon fiber is prepared, magnesium hydroxide is treated by KH560 to graft a large amount of epoxy groups on the surface of the magnesium hydroxide, and the magnesium hydroxide is grafted with the modified carbon fiber in an alkaline environment to prepare the composite carbon fiber.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A carbon fiber reinforced graphene plate sequentially comprises a curing sheet, a heating film, a curing sheet, a shielding film and a curing sheet from bottom to top;
the carbon fiber reinforced graphene plate is prepared by the following steps:
step S1: cutting the curing sheet, the heating base film and the shielding film to required sizes, punching a plurality of hexagonal through holes which are uniformly distributed on the cut heating base film, and riveting the periphery of the heating base film with a conductive copper foil in a riveting manner to obtain the heating film;
step S2: the curing sheet, the heating film, the curing sheet, the shielding film and the curing sheet are sequentially placed from bottom to top, polyethylene glycol 200 is coated between adjacent films, and high-temperature tabletting is carried out for 20min under the conditions that the temperature is 300 ℃ and the pressure is 2MPa to obtain the carbon fiber reinforced graphene plate.
The curing sheet is prepared by the following steps:
mixing nano-cellulose, graphene and deionized water, carrying out ultrasonic treatment for 30min under the condition of power of 800W to prepare a mixed solution, filtering the mixed solution, carrying out compression molding and drying on a substrate to prepare a pretreated film, placing the pretreated film in a sealed dryer, putting the sealed dryer into a beaker filled with excessive perfluorodecyl trimethoxy silane, and carrying out heat preservation treatment for 40min under the condition of temperature of 250 ℃ to prepare a cured sheet.
The mass ratio of the nano-cellulose to the graphene is 3.
The heating basal membrane is prepared by the following steps:
step A1: uniformly mixing benzhydryl alcohol, DMF (dimethyl formamide) and N-bromosuccinimide, stirring for 5 hours at the rotation speed of 150r/min and the temperature of 20 ℃, extracting with trichloromethane, filtering to remove filter residues, distilling the filtrate to remove a solvent, uniformly mixing a substrate, 4-methoxyphenylboronic acid, tetrakis (triphenylphosphine) palladium, dioxane and potassium carbonate, and carrying out reflux reaction for 8 hours at the temperature of 105 ℃ to prepare an intermediate 1;
step A2: uniformly mixing the intermediate 1, cyanuric chloride, tetrahydrofuran and sodium hydroxide, reacting for 6 hours at the rotation speed of 150r/min and the temperature of 0 ℃, adding 3-aminopropyl sodium sulfonate, heating to the temperature of 80 ℃, continuing to react for 8 hours to obtain an intermediate 2, mixing the intermediate 2 with dichloromethane, introducing nitrogen for protection, stirring and dropwise adding boron tribromide at the rotation speed of 200r/min and the temperature of 0 ℃, and reacting for 5 hours to obtain an intermediate 3;
step A3: uniformly mixing the intermediate 3, 4' -dibromobenzophenone and diphenyl sulfone, stirring for 5min at the rotation speed of 200r/min and the temperature of 130 ℃, adding sodium carbonate and potassium carbonate, heating to the temperature of 180 ℃, reacting for 2h, heating to the temperature of 250 ℃, reacting for 1h, adding acetone, settling and refluxing for 30min, and finally, drying in vacuum to obtain the flame-retardant resin;
step A4: uniformly mixing the flame-retardant resin and the composite carbon fiber, performing mould pressing for 10min at the temperature of 380 ℃ and the pressure of 2MPa, uniformly mixing tetraethoxysilane and deionized water, adjusting the pH value to 6, soaking the film in the mixture at the temperature of 60 ℃, taking out the film after soaking for 30min, and drying to obtain the heating base film.
The dosage ratio of the benzhydrol, the DMF, the N-bromosuccinimide, the 4-methoxyphenylboronic acid, the tetrakis (triphenylphosphine) palladium, the dioxane and the potassium carbonate in the step A1 is 0.1 mol.
The molar ratio of the intermediate 1, cyanuric chloride and 3-aminopropyl sodium sulfonate in the step A2 is 1, and the dosage ratio of the intermediate 2, dichloromethane and boron tribromide is 0.01mol.
The mass ratio of the intermediate 3, 4' -dibromobenzophenone, diphenyl sulfone, sodium carbonate and potassium carbonate in the step A3 is (10.35).
The using amount of the composite carbon fiber in the step A4 is 25% of the mass of the flame-retardant resin, and the using amount ratio of the tetraethoxysilane to the deionized water is 1g.
The composite carbon fiber is prepared by the following steps:
step B1: placing carbon fibers into a muffle furnace, roasting for 30min at the temperature of 400 ℃, adding the carbon fibers into a sodium hydroxide solution, soaking for 1h, filtering and drying to obtain pretreated carbon fibers, dispersing the pretreated carbon fibers into deionized water, adding KH550, stirring for 20min at the rotation speed of 600r/min and the temperature of 30 ℃, filtering and drying to obtain modified carbon fibers;
and step B2: dispersing magnesium hydroxide in deionized water, adding KH560, stirring for 20min at the rotation speed of 600r/min and the temperature of 30 ℃, filtering and drying, dispersing filter cakes and modified carbon fibers in deionized water, reacting for 2h at the rotation speed of 200r/min and the pH value of alkalinity, filtering and drying to obtain the composite carbon fiber.
The mass fraction of the sodium hydroxide solution in the step B1 is 10%, and the using amount of the KH550 is 5% of the mass of the pretreated carbon fibers.
The dosage of KH560 in the step B2 is 5% of the mass of the magnesium hydroxide, and the mass ratio of the filter cake to the modified carbon fiber is 1.
The shielding film is prepared by the following steps:
adding carbon fibers into a vacuum tube type sintering furnace, placing a copper substrate in the middle of a quartz tube, adding a ferrocene ethanol solution into a liquid input pump, vacuumizing, introducing nitrogen, heating at the speed of 10 ℃/min, conveying the ferrocene ethanol solution to a reaction area when the temperature is 1100 ℃, reacting for 20min, and stripping the copper substrate to obtain the shielding film.
Example 2
A carbon fiber reinforced graphene plate sequentially comprises a curing sheet, a heating film, a curing sheet, a shielding film and a curing sheet from bottom to top;
the carbon fiber reinforced graphene plate is prepared by the following steps:
step S1: cutting the curing sheet, the heating base film and the shielding film to required sizes, punching a plurality of hexagonal through holes which are uniformly distributed on the cut heating base film, and riveting the periphery of the heating base film with a conductive copper foil in a riveting manner to obtain the heating film;
step S2: placing a curing sheet, a heating film, a curing sheet, a shielding film and a curing sheet in sequence from bottom to top, coating polyethylene glycol 200 between adjacent membranes, and performing high-temperature tabletting for 25min under the conditions that the temperature is 305 ℃ and the pressure is 2.5MPa to obtain the carbon fiber reinforced graphene plate.
The curing sheet is prepared by the following steps:
mixing nano-cellulose, graphene and deionized water, carrying out ultrasonic treatment for 35min under the condition that the power is 900W to prepare a mixed solution, filtering the mixed solution, carrying out compression molding and drying on a substrate to prepare a pretreated film, placing the pretreated film into a sealed dryer, placing the sealed dryer into a beaker filled with excessive perfluorodecyl trimethoxy silane, and carrying out heat preservation treatment for 45min under the condition that the temperature is 255 ℃ to prepare a cured sheet.
The mass ratio of the nano-cellulose to the graphene is 3.
The heating basal membrane is prepared by the following steps:
step A1: uniformly mixing benzhydryl alcohol, DMF and N-bromosuccinimide, stirring for 6 hours at the rotation speed of 180r/min and the temperature of 23 ℃, extracting with trichloromethane, filtering to remove filter residues, distilling the filtrate to remove a solvent, uniformly mixing a substrate, 4-methoxyphenylboronic acid, tetrakis (triphenylphosphine) palladium, dioxane and potassium carbonate, and carrying out reflux reaction for 9 hours at the temperature of 108 ℃ to prepare an intermediate 1;
step A2: uniformly mixing the intermediate 1, cyanuric chloride, tetrahydrofuran and sodium hydroxide, reacting for 7 hours at the temperature of 3 ℃ at the rotation speed of 180r/min, adding 3-aminopropyl sodium sulfonate, heating to 85 ℃, continuing to react for 9 hours to obtain an intermediate 2, mixing the intermediate 2 with dichloromethane, introducing nitrogen for protection, stirring and dropwise adding boron tribromide at the rotation speed of 200r/min at the temperature of 3 ℃, and reacting for 6 hours to obtain an intermediate 3;
step A3: uniformly mixing the intermediate 3, 4' -dibromobenzophenone and diphenyl sulfone, stirring for 8min at the rotation speed of 200r/min and the temperature of 135 ℃, adding sodium carbonate and potassium carbonate, heating to the temperature of 200 ℃, reacting for 2.5h, heating to the temperature of 255 ℃, reacting for 1.5h, adding acetone, settling and refluxing for 35min, and finally drying in vacuum to obtain the flame-retardant resin;
step A4: uniformly mixing the flame-retardant resin and the composite carbon fiber, molding for 15min at 385 ℃ and 2.5MPa, uniformly mixing tetraethoxysilane and deionized water, adjusting the pH value to 6, soaking the film at 60 ℃, taking out and drying after 35min of soaking, and thus obtaining the heating base film.
The use ratio of the benzhydryl alcohol, DMF, N-bromosuccinimide, 4-methoxyphenylboronic acid, tetrakis (triphenylphosphine) palladium, dioxane and potassium carbonate in the step A1 is 0.1 mol.
The molar ratio of the intermediate 1, cyanuric chloride and 3-aminopropyl sodium sulfonate in the step A2 is 1, and the dosage ratio of the intermediate 2, dichloromethane and boron tribromide is 0.01mol.
The mass ratio of the intermediate 3, 4' -dibromobenzophenone, the diphenyl sulfone, the sodium carbonate and the potassium carbonate in the step A3 is 10.35.
The dosage of the composite carbon fiber in the step A4 is 30% of the mass of the flame-retardant resin, and the dosage ratio of the ethyl orthosilicate to the deionized water is 1g.
The composite carbon fiber is prepared by the following steps:
step B1: placing carbon fibers into a muffle furnace, roasting for 35min at the temperature of 430 ℃, adding the carbon fibers into a sodium hydroxide solution, soaking for 1.3h, filtering and drying to obtain pretreated carbon fibers, dispersing the pretreated carbon fibers into deionized water, adding KH550, stirring for 25min at the rotation speed of 600r/min and the temperature of 35 ℃, filtering and drying to obtain modified carbon fibers;
and step B2: dispersing magnesium hydroxide in deionized water, adding KH560, stirring for 25min at the rotation speed of 600r/min and the temperature of 35 ℃, filtering and drying, dispersing filter cakes and modified carbon fibers in deionized water, reacting for 3h at the rotation speed of 200r/min and the pH value of alkalinity, filtering and drying to obtain the composite carbon fiber.
The mass fraction of the sodium hydroxide solution in the step B1 is 10%, and the dosage of KH550 is 6% of the mass of the pretreated carbon fiber.
The dosage of KH560 in the step B2 is 7% of the mass of the magnesium hydroxide, and the mass ratio of the filter cake to the modified carbon fiber is 1.
The shielding film is prepared by the following steps:
adding carbon fibers into a vacuum tube type sintering furnace, placing a copper substrate in the middle of a quartz tube, adding a ferrocene ethanol solution into a liquid input pump, vacuumizing, introducing nitrogen, heating at the speed of 10 ℃/min, conveying the ferrocene ethanol solution to a reaction area when the temperature is 1120 ℃, reacting for 25min, and stripping the copper substrate to obtain the shielding film.
Example 3
A carbon fiber reinforced graphene plate sequentially comprises a curing sheet, a heating film, a curing sheet, a shielding film and a curing sheet from bottom to top;
the carbon fiber reinforced graphene plate is prepared by the following steps:
step S1: cutting the curing sheet, the heating base film and the shielding film to required sizes, punching a plurality of hexagonal through holes which are uniformly distributed on the cut heating base film, and riveting the periphery of the heating base film with a conductive copper foil in a riveting manner to obtain the heating film;
step S2: the curing sheet, the heating film, the curing sheet, the shielding film and the curing sheet are sequentially placed from bottom to top, polyethylene glycol 200 is coated between adjacent films, and high-temperature tabletting is carried out for 30min under the conditions that the temperature is 310 ℃ and the pressure is 3MPa to obtain the carbon fiber reinforced graphene plate.
The curing sheet is prepared by the following steps:
mixing nano-cellulose, graphene and deionized water, carrying out ultrasonic treatment for 40min under the condition that the power is 1000W to prepare a mixed solution, filtering the mixed solution, carrying out compression molding on a substrate and drying to prepare a pretreated film, placing the pretreated film into a sealed dryer, placing the sealed dryer into a beaker filled with excessive perfluorodecyl trimethoxy silane, and carrying out heat preservation treatment for 50min under the condition that the temperature is 260 ℃ to prepare a cured sheet.
The mass ratio of the nano-cellulose to the graphene is 3.
The heating base film is prepared by the following steps:
step A1: uniformly mixing benzhydryl alcohol, DMF (dimethyl formamide) and N-bromosuccinimide, stirring for 7 hours at the rotation speed of 200r/min and the temperature of 25 ℃, extracting with trichloromethane, filtering to remove filter residues, distilling the filtrate to remove a solvent, uniformly mixing a substrate, 4-methoxyphenylboronic acid, tetrakis (triphenylphosphine) palladium, dioxane and potassium carbonate, and carrying out reflux reaction for 10 hours at the temperature of 110 ℃ to prepare an intermediate 1;
step A2: uniformly mixing the intermediate 1, cyanuric chloride, tetrahydrofuran and sodium hydroxide, reacting for 8 hours at the rotation speed of 200r/min and the temperature of 5 ℃, adding 3-aminopropyl sodium sulfonate, heating to the temperature of 90 ℃, continuing to react for 10 hours to obtain an intermediate 2, mixing the intermediate 2 and dichloromethane, introducing nitrogen for protection, stirring and dropwise adding boron tribromide at the rotation speed of 300r/min and the temperature of 3 ℃, and reacting for 7 hours to obtain an intermediate 3;
step A3: uniformly mixing the intermediate 3, 4' -dibromobenzophenone and diphenyl sulfone, stirring for 10min at the rotation speed of 300r/min and the temperature of 140 ℃, adding sodium carbonate and potassium carbonate, heating to the temperature of 220 ℃, reacting for 3h, heating to the temperature of 260 ℃, reacting for 2h, adding acetone, settling and refluxing for 40min, and finally, drying in vacuum to obtain the flame-retardant resin;
step A4: uniformly mixing the flame-retardant resin and the composite carbon fiber, molding for 15min at 385 ℃ and 3MPa, uniformly mixing tetraethoxysilane and deionized water, adjusting the pH value to 6, soaking the film at 65 ℃ for 40min, taking out and drying to obtain the heating base film.
The use ratio of the benzhydryl alcohol, DMF, N-bromosuccinimide, 4-methoxyphenylboronic acid, tetrakis (triphenylphosphine) palladium, dioxane and potassium carbonate in the step A1 is 0.1 mol.
The molar ratio of the intermediate 1, cyanuric chloride and 3-aminopropyl sodium sulfonate in the step A2 is 1, and the dosage ratio of the intermediate 2, dichloromethane and boron tribromide is 0.01mol.
The mass ratio of the intermediate 3, 4' -dibromobenzophenone, the diphenyl sulfone, the sodium carbonate and the potassium carbonate in the step A3 is 10.35.
The dosage of the composite carbon fiber in the step A4 is 35% of the mass of the flame-retardant resin, and the dosage ratio of the ethyl orthosilicate to the deionized water is 1g.
The composite carbon fiber is prepared by the following steps:
step B1: placing carbon fibers into a muffle furnace, roasting for 40min at the temperature of 450 ℃, adding the carbon fibers into a sodium hydroxide solution, soaking for 1.5h, filtering and drying to obtain pretreated carbon fibers, dispersing the pretreated carbon fibers into deionized water, adding KH550, stirring for 30min at the rotation speed of 800r/min and the temperature of 35 ℃, filtering and drying to obtain modified carbon fibers;
and step B2: dispersing magnesium hydroxide in deionized water, adding KH560, stirring for 30min at the rotation speed of 800r/min and the temperature of 35 ℃, filtering and drying, dispersing filter cakes and modified carbon fibers in deionized water, reacting for 3h at the rotation speed of 300r/min and the pH value of alkalinity, filtering and drying to obtain the composite carbon fiber.
The mass fraction of the sodium hydroxide solution in the step B1 is 10%, and the using amount of the KH550 is 8% of the mass of the pretreated carbon fibers.
The dosage of KH560 in the step B2 is 5-8% of the mass of the magnesium hydroxide, and the mass ratio of the filter cake to the modified carbon fiber is 1.
The shielding film is prepared by the following steps:
adding carbon fibers into a vacuum tube type sintering furnace, placing a copper substrate in the middle of a quartz tube, adding a ferrocene ethanol solution into a liquid input pump, vacuumizing, introducing nitrogen, heating at the speed of 10 ℃/min, conveying the ferrocene ethanol solution to a reaction area when the temperature is 1150 ℃, reacting for 30min, and stripping the copper substrate to obtain the shielding film.
The graphene plates prepared in examples 1 to 3 were subjected to performance testing, and the test results are shown in the following table;
water resistance: the graphene plate is soaked in water to observe whether water seepage occurs or not, leakage current in a wet state is detected, and alternating current with the frequency of 50Hz and 5000V is applied to test the electrical strength of the graphene plate.
Mechanical strength: according to the standard of GB4706.1-2005, scratch with the fingernail at the uniform velocity of 200mm/s along the electric heat membrane surface, the scratch should pass current-carrying strip and heating resistor area, the test nail is 30 degrees with the horizontal direction and the angle, the force of exerting pressure on the test nail is 10N, carry on the test of electrical strength again after the test, apply the alternating current test voltage of the frequency of 50Hz,5000V, for 1 minute.
Flame retardancy the flame retardancy grade was tested according to the experimental method of GB 4706.8-2003-30.102.
Figure BDA0003757311560000141
From the table, it can be known that the carbon fiber reinforced graphene boards prepared in examples 1 to 3 have good waterproof effect, excellent mechanical properties and good flame retardancy.
The foregoing is illustrative and explanatory only of the present invention, and it is intended that the present invention cover modifications, additions, or substitutions by those skilled in the art, without departing from the spirit of the invention or exceeding the scope of the claims.

Claims (8)

1. A carbon fiber reinforced graphene board is characterized in that: the heating film is arranged on the upper surface of the curing sheet;
the curing sheet is prepared by the following steps:
mixing nano-cellulose, graphene and deionized water, performing ultrasonic treatment to obtain a mixed solution, filtering the mixed solution, performing compression molding on a substrate, drying to obtain a pretreated film, placing the pretreated film in a sealed dryer, placing the sealed dryer into a beaker filled with excessive perfluorodecyl trimethoxy silane, and performing heat preservation treatment to obtain a cured sheet.
2. The carbon fiber-reinforced graphene sheet according to claim 1, wherein: the heating basal membrane is prepared by the following steps:
step A1: mixing and stirring benzhydryl alcohol, DMF and N-bromosuccinimide, extracting with trichloromethane, filtering to remove filter residues, distilling the filtrate to remove a solvent, mixing and refluxing a substrate, 4-methoxyphenylboronic acid, tetrakis (triphenylphosphine) palladium, dioxane and potassium carbonate to react to prepare an intermediate 1;
step A2: mixing the intermediate 1, cyanuric chloride, tetrahydrofuran and sodium hydroxide for reaction, adding 3-aminopropyl sodium sulfonate, heating for continuous reaction to obtain an intermediate 2, mixing the intermediate 2 with dichloromethane, introducing nitrogen for protection, stirring, dropwise adding boron tribromide, and reacting to obtain an intermediate 3;
step A3: mixing and stirring the intermediate 3, 4' -dibromo benzophenone and the diphenyl sulfone, adding sodium carbonate and potassium carbonate, heating to react again, adding acetone to settle and reflux, and finally drying in vacuum to obtain the flame-retardant resin;
step A4: and (3) uniformly mixing the flame-retardant resin and the composite carbon fiber, after mould pressing treatment, uniformly mixing tetraethoxysilane and deionized water, adjusting the pH value to soak the film in the mixture, taking out the film and drying the film to obtain the heating base film.
3. The carbon fiber-reinforced graphene sheet according to claim 2, wherein: the dosage ratio of the benzhydrol, the DMF, the N-bromosuccinimide, the 4-methoxyphenylboronic acid, the tetrakis (triphenylphosphine) palladium, the dioxane and the potassium carbonate in the step A1 is 0.1 mol.
4. The carbon fiber-reinforced graphene sheet according to claim 2, wherein: the molar ratio of the intermediate 1, cyanuric chloride and 3-aminopropyl sodium sulfonate in the step A2 is 1, and the dosage ratio of the intermediate 2, dichloromethane and boron tribromide is 0.01mol.
5. The carbon fiber reinforced graphene sheet according to claim 2, wherein: the mass ratio of the intermediate 3, 4' -dibromobenzophenone, diphenyl sulfone, sodium carbonate and potassium carbonate in the step A3 is (10.35).
6. The carbon fiber-reinforced graphene sheet according to claim 2, wherein: the dosage of the composite carbon fiber in the step A4 is 25-35% of the mass of the flame-retardant resin, and the dosage ratio of the ethyl orthosilicate to the deionized water is 1g.
7. The carbon fiber-reinforced graphene sheet according to claim 1, wherein: the shielding film is prepared by the following steps:
adding carbon fibers into a vacuum tube type sintering furnace, placing a copper substrate in the middle of a quartz tube, adding a ferrocene ethanol solution into a liquid input pump, pumping to vacuum, introducing nitrogen, heating, conveying the ferrocene ethanol solution to a reaction area, reacting, and stripping the copper substrate to obtain the shielding film.
8. The method for preparing the carbon fiber reinforced graphene plate according to claim 1, wherein the method comprises the following steps: the method specifically comprises the following steps:
step S1: cutting the curing sheet, the heating base film and the shielding film to required sizes, punching a plurality of hexagonal through holes which are uniformly distributed on the cut heating base film, and riveting the periphery of the heating base film with a conductive copper foil in a riveting manner to obtain the heating film;
step S2: from the bottom up places solidification piece, heating film, solidification piece, shielding film, solidification piece in proper order to coating polyethylene glycol 200 between adjacent diaphragm, the high temperature preforming makes carbon fiber reinforcement formula graphite alkene board.
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