CN113354920A - High-temperature-resistance epoxy aramid fiber insulating layer, molded part and preparation method thereof - Google Patents

High-temperature-resistance epoxy aramid fiber insulating layer, molded part and preparation method thereof Download PDF

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CN113354920A
CN113354920A CN202110555291.0A CN202110555291A CN113354920A CN 113354920 A CN113354920 A CN 113354920A CN 202110555291 A CN202110555291 A CN 202110555291A CN 113354920 A CN113354920 A CN 113354920A
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aramid fiber
epoxy resin
temperature
parts
epoxy
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CN113354920B (en
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杜旻
黄洪驰
师强
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Sichuan Dongcai Technology Group Co Ltd
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Sichuan Dongcai Technology Group Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29BPREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B15/00Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00
    • B29B15/08Pretreatment of the material to be shaped, not covered by groups B29B7/00 - B29B13/00 of reinforcements or fillers
    • B29B15/10Coating or impregnating independently of the moulding or shaping step
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28Shaping operations therefor
    • B29C70/40Shaping or impregnating by compression not applied
    • B29C70/42Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C70/00Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
    • B29C70/04Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
    • B29C70/28Shaping operations therefor
    • B29C70/54Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
    • B29C70/545Perforating, cutting or machining during or after moulding
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2363/00Characterised by the use of epoxy resins; Derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2463/00Characterised by the use of epoxy resins; Derivatives of epoxy resins
    • C08J2463/02Polyglycidyl ethers of bis-phenols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2463/00Characterised by the use of epoxy resins; Derivatives of epoxy resins
    • C08J2463/04Epoxynovolacs
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2477/00Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2477/10Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids

Abstract

The invention discloses a high-temperature-resistant epoxy aramid fiber insulating layer, a molded part and a preparation method thereof, and is characterized in that: the high temperature resistant epoxy aramid fiber insulating layer and the molded part are composite materials prepared by hot press molding one or more layers of overlapped high temperature resistant epoxy aramid fiber-fabric prepreg; the high-temperature-resistant epoxy aramid fiber-fabric prepreg is formed by impregnating aramid fiber-fabric with an epoxy adhesive and then baking the impregnated aramid fiber-fabric with a semi-cured product; the high-temperature-resistant epoxy adhesive consists of epoxy resin, modified epoxy resin, a filler, a curing agent, a solvent and an accelerant. The invention is suitable for the fields of various engineering equipment, electrical equipment, corrosion-resistant appliances, new energy automobiles and the like with special purposes (aviation, aerospace, high-performance ships, bulletproof, stab-resistant and military industry) with higher requirements on temperature resistance, and has high reliability, good performance and strong practicability.

Description

High-temperature-resistance epoxy aramid fiber insulating layer, molded part and preparation method thereof
Technical Field
The invention belongs to an insulating layer, a molded part and preparation thereof, and relates to a high-temperature-resistant epoxy aramid fiber insulating layer, a molded part and preparation methods thereof. The high-temperature-resistance epoxy aramid fiber insulating layer and the die-pressed part prepared by the invention are particularly suitable for application in the fields of various engineering equipment, electrical equipment, corrosion-resistant appliances, new energy automobiles and the like with special purposes (aviation, aerospace, high-performance ships, bulletproof, stab-resistant and military industry) and provide better reliability.
Background
Aramid fiber has unique excellent properties such as high mechanical strength, high strength modulus, wear resistance, low conductivity, creepage resistance, no warpage, no delamination and the like, and is widely applied to the fields of various engineering equipment, electrical equipment, corrosion-resistant appliances, new energy automobiles and the like with special purposes (aviation, aerospace, high-performance ships, bulletproof, stab resistance and military industry), so that the demand on high-performance aramid fiber products, particularly aramid fiber (insulation) layers and molded products used in high-temperature, high-humidity, high-current and high-strength environments, is more and more urgent. In recent years, although there has been an increasing research on aramid fibers, there has been little research on aramid fiber composite products, particularly aramid fiber (insulation) layers and molded products. In the fields of various engineering equipment, electrical equipment, corrosion-resistant appliances, new energy automobiles and the like with special purposes (aviation, aerospace, high-performance ships, bulletproof, stab resistance and military industry), when an epoxy aramid fiber (insulating) layer and a molded part are used in environments of high voltage, high temperature (especially above C level), high humidity and the like, the requirements that the normal state (room temperature) reaches more than or equal to 550MPa, the ultrahigh bending strength is more than or equal to 330MPa under the high-temperature working condition (the temperature is 230 ℃) and the high humidity resistance (namely, the temperature is 121 ℃, the bending strength retention rate of 96h under the environment with the humidity of 100% reaches more than 50% at the normal temperature and more than or equal to 275MPa) and the excellent toughness (namely, the shearing strength is more than or equal to 25MPa) are met. In the prior art, no literature report which can simultaneously meet the use requirements is found.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a high-temperature-resistant epoxy aramid fiber insulating layer, a molded part and a preparation method thereof. Therefore, the high temperature resistant epoxy aramid fiber insulating layer, the die-pressed part and the preparation method thereof can realize that the ultrahigh bending strength of the part is more than 330MPa at the temperature of 230 ℃, the bending strength retention rate of 96h at the temperature of 121 ℃ and the humidity of 100% reaches more than 50% (more than 275MPa) at normal temperature, the shear strength is more than or equal to 25MPa, and the use requirements in the fields of various engineering equipment, electrical equipment, corrosion-resistant appliances, new energy automobiles and the like with special purposes (aviation, aerospace, high-performance ships, bulletproof, stab-resistant and military industry) can be met.
The content of the invention is as follows: a high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, characterized by: the high-temperature-resistant epoxy aramid fiber insulating layer and the molded part are composite materials (namely the high-temperature-resistant epoxy aramid fiber insulating layer and the molded part) prepared by hot-press molding one or more layers of overlapped high-temperature-resistant epoxy aramid fiber-fabric prepreg;
the high-temperature-resistant epoxy aramid fiber-fabric prepreg is formed by impregnating aramid fiber-fabric with an epoxy adhesive and baking (removing part of solvent in the aramid fiber-fabric) the aramid fiber-fabric prepreg with a semi-cured material;
the aramid fiber-fabric is aramid fiber plaid (product production providing enterprises can be DuPont, Japanese emperor, Chengdou Luchen new material science and technology Co., Ltd.), aramid fiber twill (product production providing enterprises can be David science and technology Co., Ltd., Shantou Mingda textile Co., Ltd., Jiangsu Kangdun new material Co., Ltd.), aramid fiber plaid (product production providing enterprises can be David science and technology Co., Ltd., Shanshu Ming Da textile Co., Ltd., Jiangsu Kangdun new material, etc.), aramid fiber satin (product production providing enterprises can be Jiangyin Kong Ying Jia textile Co., Yixing Jie Chuang carbon fiber product Co., Yixing Hua constant high performance fiber weaving Co., Ltd., etc.), aramid fiber stitch-knitted felt (product production providing enterprises can be Zhejiang David Wei environmental protection Yongsu Co., Ltd., etc.) One or a mixture of more than two of aramid fiber continuous felt (product production providing enterprises can be from Wed, Zhejiang, etc.), aramid fiber composite cloth (product production providing enterprises can be from Wed, Zhejiang, etc.), and aramid fiber composite felt (product production providing enterprises can be from Wed, Zhejiang, etc.);
the high-temperature-resistant epoxy adhesive comprises the following components in parts by weight: 12-45 parts of epoxy resin, 5-35 parts of modified epoxy resin, 1-61 parts of filler, 6-34 parts of curing agent, 9.5-201 parts of solvent and 0.01-0.18 part of accelerator;
the epoxy resin is one or a mixture of more than two of bisphenol fluorene epoxy resin (DGEBF for short), bis-o-cresol fluorene epoxy resin (DGEMBF for short) and bis-di-o-cresol fluorene epoxy resin (DGEDMFF for short), and the chemical structural formulas of the epoxy resin are respectively shown as the following formulas:
Figure BDA0003076952800000021
bisphenol fluorene epoxy resin (DGEBF for short) molecular structural formula
Figure BDA0003076952800000031
Molecular structural formula of bis-o-cresol fluorene epoxy resin (DGEMBF for short)
Figure BDA0003076952800000032
Molecular structural formula of bis-di-o-cresol fluorene epoxy resin (DGEDMFF for short)
The modified epoxy resin is bisphenol A type epoxy resin (product production providing company and brand may be DER-383 of Dow, DER-331 of Dow, E-51 of Baling, CYD-128 of Baling, etc.), bisphenol F type epoxy resin (product production providing company and brand may be EPON-862 of Hansen Miji, NPEF-170 of Nanya epoxy resin (Kunshan), etc.), alicyclic epoxy resin (product production providing company and brand may be TDE-85 of Hubei Xinrunder chemical Co., Ltd., CEL2021P of DAICEL, UVR-6110 of DOW, CY-179 of Hunan, etc.), glycidyl amine type epoxy resin (product production providing company and brand may be AG: Shanghai synthetic resin research institute, etc.), (product production providing company and brand may be DE-383 of Shanghai, etc.), Biphenyl type epoxy resin (product manufacturing and providing enterprises and brands may be BPNE3501LL/9781 of Jiangshan materials science and technology Limited in Hunan), phenol type novolac epoxy resin (product manufacturing and providing enterprises and brands may be NPPN-638S of Nanasia epoxy resin (Kunshan) Limited, EPON 154 of Hansen Mitsukuji materials group in USA, DPNH9501 of Jiangshan materials science and technology Limited in Hunan, etc.), o-cresol type novolac epoxy resin (product manufacturing and providing enterprises and brands may be N-XP of Japan ink corporation, CNE202 of Taiwan Changchun resin factory, NPCN-704/703 of Nanasia epoxy resin (Kunshan) Limited, etc.), bisphenol A novolac type epoxy resin (product manufacturing and providing enterprises and brands may be BNE200 of Taiwan Changchun resin factory, F-51 of Shanghai Satsu chemical technology Limited in China, etc.), bisphenol A novolac type epoxy resin (product manufacturing and brands may be BNE200 of Taiwan China, F-51 of Shanghai Katsu technology Limited in China, etc.), One or a mixture of two or more of resorcinol type epoxy resin (product production providing company and brand may be ERISYS RDGE-H of Jia Dida chemical Co., Ltd., YF-554 of Guangzhou Yifu chemical materials Co., Ltd.), epoxy resin of dicyclopentadiene or dicycladiene and phenol-formaldehyde polycondensation resin (product production providing company and brand may be NPNE1501 of Hunan Jiasheng Material science and technology Co., Ltd., DNE260 of Jinninghuaka resin Co., Ltd., DNE280A75 of Tiangao New technology Co., Ltd.), isocyanate modified epoxy resin (product production providing company and brand may be A-IME AER4152 of Jiangsai chemical Co., Ltd., SEB-350 of SHIN-A T & C, etc.), and hydantoin type epoxy resin (product production providing company and brand may be Whitman electronic material Co., Whitman, HY-070, etc.) An agent;
the curing agent is a mixture of two or more of 4, 4-diaminodiphenylmethane, 4-diaminodiphenylsulfone and diamine fluorene, wherein the chemical structural formula of the diamine fluorene is as follows:
Figure BDA0003076952800000041
the filler is one or a mixture of more than two of aluminum hydroxide, aluminum oxide, boehmite, magnesium hydroxide, silicon micropowder, montmorillonite, kaolin, fumed silica, silicon dioxide micropowder, graphene, hydrotalcite and talcum powder;
the accelerant is one or a mixture of more than two of 2-methylimidazole, 2-ethyl-4-methylimidazole, N-dimethylbenzylamine, boron trifluoride ethylamine, triethylamine, hexamethyltetramine and aluminum acetylacetonate;
the solvent is one or a mixture of more than two of toluene, xylene, ethylene glycol dimethyl ether, ethylene glycol ethyl ether acetate, propylene glycol methyl ether, methyl ethyl ketone, cyclohexanone, methyl acetate, butanone, acetone, N-dimethylformamide and ethanol.
The invention comprises the following steps: in the high-temperature-resistant epoxy aramid fiber-fabric prepreg: the weight percentage of the semi-cured substance is 15-55%, and the weight percentage of the aramid fiber-fabric is 45-85%.
The invention comprises the following steps: the bending strength of the high-temperature-resistant epoxy aramid fiber insulating layer and the molded part (namely the prepared composite material) is greater than 330MPa at the temperature of 230 ℃, the bending strength retention rate of 96h (h) at the temperature of 121 ℃ and the humidity of 100% reaches more than 50% at normal temperature, namely more than 275MPa, and the shear strength is more than or equal to 25 MPa.
Another aspect of the invention is: a preparation method of a high-temperature-resistant epoxy aramid fiber insulating layer and a molded part is characterized by comprising the following steps:
a. preparing a high-temperature-resistant epoxy adhesive:
(a) preparing materials: taking raw materials of the components according to the weight ratio of 12-45 parts of epoxy resin, 5-35 parts of modified epoxy resin, 1-61 parts of filler, 6-34 parts of curing agent, 9.5-201 parts of solvent and 0.01-0.18 part of accelerator;
the epoxy resin is one or a mixture of more than two of bisphenol fluorene epoxy resin (DGEBF for short), bis-o-cresol fluorene epoxy resin (DGEMBF for short) and bis-di-o-cresol fluorene epoxy resin (DGEDMFF for short), and the chemical structural formulas of the epoxy resin are respectively shown as the following formulas:
Figure BDA0003076952800000051
bisphenol fluorene epoxy resin (DGEBF for short) molecular structural formula
Figure BDA0003076952800000052
Molecular structural formula of bis-o-cresol fluorene epoxy resin (DGEMBF for short)
Figure BDA0003076952800000053
Molecular structural formula of bis-di-o-cresol fluorene epoxy resin (DGEDMFF for short)
The modified epoxy resin is bisphenol A type epoxy resin (product production providing company and brand may be DER-383 of Dow, DER-331 of Dow, E-51 of Baling, CYD-128 of Baling, etc.), bisphenol F type epoxy resin (product production providing company and brand may be EPON-862 of Hansen Miji, NPEF-170 of Nanya epoxy resin (Kunshan), etc.), alicyclic epoxy resin (product production providing company and brand may be TDE-85 of Hubei Xinrunder chemical Co., Ltd., CEL2021P of DAICEL, UVR-6110 of DOW, CY-179 of Hunan, etc.), glycidyl amine type epoxy resin (product production providing company and brand may be AG: Shanghai synthetic resin research institute, etc.), (product production providing company and brand may be DE-383 of Shanghai, etc.), Biphenyl type epoxy resin (product manufacturing and providing enterprises and brands may be BPNE3501LL/9781 of Jiangshan materials science and technology Limited in Hunan), phenol type novolac epoxy resin (product manufacturing and providing enterprises and brands may be NPPN-638S of Nanasia epoxy resin (Kunshan) Limited, EPON 154 of Hansen Mitsukuji materials group in USA, DPNH9501 of Jiangshan materials science and technology Limited in Hunan, etc.), o-cresol type novolac epoxy resin (product manufacturing and providing enterprises and brands may be N-XP of Japan ink corporation, CNE202 of Taiwan Changchun resin factory, NPCN-704/703 of Nanasia epoxy resin (Kunshan) Limited, etc.), bisphenol A novolac type epoxy resin (product manufacturing and providing enterprises and brands may be BNE200 of Taiwan Changchun resin factory, F-51 of Shanghai Satsu chemical technology Limited in China, etc.), bisphenol A novolac type epoxy resin (product manufacturing and brands may be BNE200 of Taiwan China, F-51 of Shanghai Katsu technology Limited in China, etc.), One or a mixture of two or more of resorcinol type epoxy resin (product production providing company and brand may be ERISYS RDGE-H of Jia Dida chemical Co., Ltd., YF-554 of Guangzhou Yifu chemical materials Co., Ltd.), epoxy resin of dicyclopentadiene or dicycladiene and phenol-formaldehyde polycondensation resin (product production providing company and brand may be NPNE1501 of Hunan Jiasheng Material science and technology Co., Ltd., DNE260 of Jinninghuaka resin Co., Ltd., DNE280A75 of Tiangao New technology Co., Ltd.), isocyanate modified epoxy resin (product production providing company and brand may be A-IME AER4152 of Jiangsai chemical Co., Ltd., SEB-350 of SHIN-A T & C, etc.), and hydantoin type epoxy resin (product production providing company and brand may be Whitman electronic material Co., Whitman, HY-070, etc.) An agent;
the curing agent is a mixture of two or more of 4, 4-diaminodiphenylmethane, 4-diaminodiphenylsulfone and diamine fluorene, wherein the chemical structural formula of the diamine fluorene is as follows:
Figure BDA0003076952800000061
the filler is one or a mixture of more than two of aluminum hydroxide, aluminum oxide, boehmite, magnesium hydroxide, silicon micropowder, montmorillonite, kaolin, fumed silica, silicon dioxide micropowder, graphene, hydrotalcite and talcum powder;
the accelerant is one or a mixture of more than two of 2-methylimidazole, 2-ethyl-4-methylimidazole, N-dimethylbenzylamine, boron trifluoride ethylamine, triethylamine, hexamethyltetramine and aluminum acetylacetonate;
the solvent is one or a mixture of more than two of toluene, xylene, ethylene glycol dimethyl ether, ethylene glycol ethyl ether acetate, propylene glycol methyl ether, methyl ethyl ketone, cyclohexanone, methyl acetate, butanone, acetone, N-dimethylformamide and ethanol;
(b) adding the epoxy resin, the modified epoxy resin and the filler in the formula amount in the step (a) into a glue preparation tank at room temperature, stirring for 0.5-2 hours at the temperature of 55-115 ℃, adding a curing agent, stirring for 1-4 hours at the temperature of 100-145 ℃, cooling, adding a solvent, fully and uniformly dispersing, adding an accelerator to adjust the forming time of the glue solution, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the epoxy adhesive under the condition of a 210 ℃ hot plate when the forming time is 440-530 seconds to obtain the high-temperature-resistant epoxy adhesive;
b. preparing high-temperature-resistant epoxy aramid fiber-fabric prepreg:
dipping the aramid fiber-fabric into the high-temperature-resistant epoxy adhesive in the step a through a gluing machine (which can be a horizontal or vertical gluing machine), and baking the aramid fiber-fabric through a baking channel of the gluing machine, wherein the baking channel of the gluing machine is 24m long and is divided into 4 sections and 6m in each section, the baking temperature range is 70-175 ℃, the speed of the gluing machine is 7-21 m/min, and the high-temperature-resistant epoxy aramid fiber-fabric prepreg is prepared after baking;
the aramid fiber-fabric is aramid fiber plaid (product production providing enterprises can be DuPont, Japanese emperor, Chengdou Luchen new material science and technology Co., Ltd.), aramid fiber twill (product production providing enterprises can be David science and technology Co., Ltd., Shantou Mingda textile Co., Ltd., Jiangsu Kangdun new material Co., Ltd.), aramid fiber plaid (product production providing enterprises can be David science and technology Co., Ltd., Shanshu Ming Da textile Co., Ltd., Jiangsu Kangdun new material, etc.), aramid fiber satin (product production providing enterprises can be Jiangyin Kong Ying Jia textile Co., Yixing Jie Chuang carbon fiber product Co., Yixing Hua constant high performance fiber weaving Co., Ltd., etc.), aramid fiber stitch-knitted felt (product production providing enterprises can be Zhejiang David Wei environmental protection Yongsu Co., Ltd., etc.) One or a mixture of more than two of aramid fiber continuous felt (product production providing enterprises can be from Wed, Zhejiang, etc.), aramid fiber composite cloth (product production providing enterprises can be from Wed, Zhejiang, etc.), and aramid fiber composite felt (product production providing enterprises can be from Wed, Zhejiang, etc.);
c. and (3) pressing the high-temperature-resistant epoxy aramid fiber insulating layer and a molded part:
cutting the high temperature resistant epoxy aramid fiber-fabric prepreg prepared in the step b into a required shape and size according to the drawing (process) requirements of the high temperature resistant epoxy aramid fiber insulating layer and a molded part, placing one or more layers of the cut high temperature resistant epoxy aramid fiber-fabric prepreg on a stainless steel mold (with two surfaces coated with a release agent), sending the high temperature resistant epoxy aramid fiber-fabric prepreg to a hot press (which can be a common hot press or a vacuum hot press) with a hot plate, controlling the temperature to be 140-250 ℃ and the pressure to be 5-30 MPa for hot press molding, and determining the hot press molding time to be 0.5-30 h according to the thickness of a molded structural part, thus preparing the high temperature resistant epoxy aramid fiber insulating layer and the molded part.
In another aspect of the invention: the high-temperature-resistant epoxy aramid fiber-fabric prepreg prepared in the step b is a high-temperature-resistant epoxy aramid fiber-fabric prepreg with a semi-cured product on an aramid fiber-fabric, wherein the high-temperature-resistant epoxy aramid fiber-fabric prepreg comprises the following components in percentage by weight: the weight percentage of the semi-cured substance is 15-55%, and the weight percentage of the aramid fiber-fabric is 45-85%.
In another aspect of the invention: the shape of the stainless steel mold in step c can be flat plate type, U-shaped, L-shaped or similar shape, and other special shapes.
In another aspect of the invention: and c, bending strength of the prepared high-temperature-resistant epoxy aramid fiber insulating layer and the molded part is larger than 330MPa at the temperature of 230 ℃, the bending strength retention rate of 96h (h) at the temperature of 121 ℃ and the humidity of 100% reaches more than 50% at normal temperature, namely more than 275MPa, and the shear strength is larger than or equal to 25 MPa.
Compared with the prior art, the invention has the following characteristics and beneficial effects:
(1) according to the invention, the matrix resin and all raw materials are long-term high-temperature resistant products, the high-temperature resistant epoxy aramid fiber insulating layer and the molded part can strictly meet the requirement of high mechanical strength at a use temperature of more than 230 ℃ for a long time, the bending strength at normal state is 617-634 MPa, the bending strength at 230 ℃ is 373-394 MPa, especially the strength retention ratio at high temperature and high humidity is higher, the bending strength at 230 ℃ is 373-394 MPa (the retention ratio is more than or equal to 60%), the bending strength at 121 ℃ and 100% humidity is 469-497 MPa (the retention ratio is more than or equal to 75%) after 96h, and the shear strength is 45-61 MPa. The technical problem that the bending strength retention rate of the epoxy aramid fiber composite material at the temperature of over 230 ℃ is more than or equal to 50 percent due to the self strength difference of the epoxy aramid fiber composite material is solved;
(2) the invention adopts the synergistic technology of the modified resin and the epoxy resin, so that the resin system of the modified resin and the epoxy resin simultaneously meets better toughness on the basis of resisting the use temperature of more than 200 ℃ for a long time, and particularly solves the technical problem that the bending strength retention rate is more than 75 percent at the temperature of 121 ℃ and the humidity of 100 percent after 96 hours, which cannot be achieved by the performance of the resin, in the aspects of moisture and heat resistance, and also greatly reduces the production cost of the product;
(3) the invention has simple preparation process, easy operation, excellent product quality, reduced cost, and capability of meeting the requirements of various engineering equipment, electrical equipment, corrosion-resistant appliances, new energy automobiles and other fields with special purposes (aviation, aerospace, high-performance ships, bulletproof, stab prevention, war industry) on high-temperature-resistant structural composite materials, and has obvious practical use value and application prospect and strong practicability.
Detailed Description
The following examples are intended to further illustrate the present invention and should not be construed as limiting the scope of the invention, which is intended to be covered by the claims appended hereto.
In the following examples, the amounts of each ingredient component material indicated as "parts" are parts by weight (e.g., both grams or kilograms).
Preparation of first part high-temperature-resistant epoxy adhesive
Example 1-1:
respectively adding 18 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 10 parts of glycidyl amine epoxy resin, 9 parts of biphenyl epoxy resin and 8 parts of silica powder into a glue preparation tank at room temperature, stirring for 0.75 hour at the temperature of 75 ℃, adding 4 parts of curing agent 4, 4-diaminodiphenyl sulfone and 3 parts of bisamine fluorene, stirring for 1.25 hours at the temperature of 100 ℃, adding 18 parts of xylene, fully and uniformly dispersing, adding 0.05 part of accelerant 2-ethyl-4-methylimidazole, adjusting the molding time of the glue solution, sampling, testing the molding time of the glue solution by a knife method (210 ℃ hot plate) for 496 seconds, and finishing the preparation of the glue solution.
Examples 1 to 2:
respectively adding 21 parts of bisphenol fluorene epoxy resin (DGEBF for short), 9 parts of alicyclic epoxy resin, 7 parts of phenol novolac epoxy resin and 16 parts of fumed silica into a glue preparation tank at room temperature, stirring for 0.5 hour at the temperature of 85 ℃, adding 7 parts of curing agent 4, 4-diaminodiphenylmethane and 6 parts of diamine fluorene, stirring for 1.75 hours at the temperature of 110 ℃, adding 26 parts of ethylene glycol dimethyl ether to fully and uniformly disperse the ethylene glycol dimethyl ether, adding 0.07 part of accelerator boron trifluoride ethylamine fluoride to adjust the molding time of the glue solution, sampling, testing the molding time of the glue solution (210 ℃) for 481 seconds by using a knife method, and finishing the preparation of the glue solution.
Examples 1 to 3:
at room temperature, 12 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 3 parts of biphenyl epoxy resin, 2 parts of bisphenol A epoxy resin and 9 parts of montmorillonite are respectively added into a glue preparation tank, stirred for 0.75 hour at the temperature of 55 ℃, added with 4 parts of curing agent 4, 4-diaminodiphenyl sulfone and 4 parts of bisamine fluorene, stirred for 1 hour at the temperature of 105 ℃, added with 9.5 parts of cyclohexanone to be fully and uniformly dispersed, added with 0.01 part of accelerant triethylamine to adjust the molding time of glue solution, sampled, and tested by a knife method for the molding time (210 ℃) of 486 seconds, thus finishing the preparation of the glue solution.
Examples 1 to 4:
at room temperature, 23 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 7 parts of epoxy resin of dicyclopentadiene or dicyclo-diene and phenolic aldehyde polycondensation resin, 2 parts of o-cresol type phenolic aldehyde epoxy resin and 22 parts of boehmite are respectively added into a glue preparation tank, after stirring for 1.05 hours at the temperature of 90 ℃, 10 parts of curing agent 4, 4-diaminodiphenyl sulfone and 8 parts of diamine fluorene are added, stirring is carried out for 1.05 hours at the temperature of 115 ℃, 28 parts of N, N-dimethylformamide is added, after the N, N-dimethylformamide is fully and uniformly dispersed, 0.14 part of accelerator hexamethyltetramine is added to adjust the forming time of glue solution, sampling is carried out, the forming time (210 ℃ hot plate) 465 seconds of the glue solution is tested by using a knife method, and the glue solution is prepared.
Examples 1 to 5:
respectively adding 16 parts of bis-o-cresol fluorene epoxy resin (DGEDMBF for short), 6 parts of isocyanate modified epoxy resin, 5 parts of resorcinol epoxy resin and 1 part of talcum powder into a glue preparation tank at room temperature, stirring for 1.25 hours at 70 ℃, adding 2 parts of curing agent 4, 4-diaminodiphenyl sulfone and 4 parts of diamine fluorene, stirring for 2 hours at 110 ℃, adding 12 parts of dimethylbenzene to fully and uniformly disperse, adding 0.11 part of accelerator N, N-dimethylbenzylamine to adjust the forming time of glue solution, sampling, testing the forming time of the glue solution by a knife method (210 ℃ hot plate) for 502 seconds, and finishing the preparation of the glue solution.
Examples 1 to 6:
at room temperature, 25 parts of bis-o-cresol fluorene epoxy resin (DGEDMBF for short), 11 parts of biphenyl epoxy resin, 10 parts of bisphenol F epoxy resin and 32 parts of graphene are respectively added into a glue preparation tank, after stirring for 1.25 hours at the temperature of 95 ℃, 11 parts of curing agent 4, 4-diaminodiphenylmethane and 11 parts of bisamine fluorene are added, stirring is carried out for 2.35 hours at the temperature of 115 ℃, 68 parts of butanone is added, after the materials are fully and uniformly dispersed, 0.12 part of accelerant aluminum acetylacetonate is added to adjust the forming time of glue solution, sampling is carried out, the forming time (210 ℃ hot plate) of the glue solution is tested by a knife method for 478 seconds, and the glue solution is prepared.
Examples 1 to 7:
respectively adding 19 parts of bis-o-cresol fluorene epoxy resin (DGEDMBF for short), 13 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 4 parts of phenol novolac epoxy resin, 9 parts of alicyclic epoxy resin and 28 parts of silicon micro powder into a glue preparation tank at room temperature, stirring for 1.5 hours at the temperature of 85 ℃, adding 5 parts of curing agent 4, 4-diaminodiphenylmethane and 17 parts of diamine fluorene, stirring for 1.65 hours at the temperature of 135 ℃, adding 42 parts of propylene glycol methyl ether, fully dispersing uniformly, adding 0.11 part of accelerator aluminum acetylacetonate to adjust the forming time of the glue solution, sampling, testing the forming time of the glue solution (210 ℃ hot plate) for 525 seconds by using a knife method, and finishing the preparation of the glue solution.
Examples 1 to 8:
at room temperature, 19 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 10 parts of bisphenol fluorene epoxy resin (DGEBF for short), 7 parts of glycidyl amine epoxy resin, 5 parts of bisphenol F epoxy resin, 17 parts of talcum powder and 8 parts of silicon micropowder are respectively added into a glue preparation tank, after stirring for 2 hours at the temperature of 85 ℃, 8 parts of curing agent 4, 4-diaminodiphenyl sulfone and 12 parts of diamine fluorene are added, stirring for 2.5 hours at the temperature of 125 ℃, 50 parts of toluene and 41 parts of methyl acetate are added, after the materials are fully dispersed uniformly, 0.14 part of accelerant 2-ethyl-4-methylimidazole is added to adjust the forming time of the glue solution, sampling is carried out, the forming time (210 ℃)477 seconds of the glue solution is tested by a knife method, and the glue solution is prepared by a hot plate.
Examples 1 to 9:
at room temperature, 27 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 7 parts of bisphenol fluorene epoxy resin (DGEBF for short), 8 parts of epoxy resin of dicyclopentadiene or dicyclodiene and phenolic polycondensation resin, 9 parts of resorcinol type epoxy resin, 17 parts of boehmite and 21 parts of talcum powder are respectively added into a glue preparation tank, after stirring for 2 hours at the temperature of 115 ℃, 5 parts of curing agent 4, 4-diaminodiphenylmethane and 11 parts of diamine fluorene are added, stirring for 3 hours at the temperature of 130 ℃, 95 parts of xylene and 84 parts of alcohol are added, after the mixture is fully dispersed uniformly, 0.13 part of accelerant 2-methylimidazole is added to adjust the molding time of the glue solution, sampling is carried out, the molding time of the glue solution (210 ℃ hot plate) is tested by a knife method for 472 seconds, and the glue solution is prepared.
Examples 1 to 10:
respectively adding 24 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 15 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 14 parts of bisphenol F type epoxy resin, 10 parts of isocyanate modified epoxy resin, 18 parts of kaolin and 19 parts of fumed silica into a glue preparation tank at room temperature, stirring for 2 hours at the temperature of 95 ℃, adding 11 parts of curing agent 4, 4-diaminodiphenyl sulfone and 19 parts of diamine fluorene, stirring for 3.5 hours at the temperature of 145 ℃, adding 71 parts of propylene glycol methyl ether and 45 parts of toluene, fully and uniformly dispersing, adding 0.15 part of accelerator 2-ethyl-4-methylimidazole, adjusting the molding time of the glue solution, sampling, testing the molding time of the glue solution (210 ℃) by using a knife method for 440 seconds, and preparing the glue solution by a hot plate.
Examples 1 to 11:
respectively adding 10 parts of bis-o-cresol fluorene epoxy resin (DGEMBF), 16 parts of bisphenol fluorene epoxy resin (DGEBF), 12 parts of glycidyl amine epoxy resin, 7 parts of hydantoin epoxy resin, 18 parts of kaolin and 14 parts of hydrotalcite into a glue preparation tank at room temperature, stirring for 1.75 hours at the temperature of 85 ℃, adding 14 parts of curing agent 4, 4-diaminodiphenyl sulfone and 10 parts of diamine fluorene, stirring for 3 hours at the temperature of 125 ℃, adding 43 parts of N, N-dimethylformamide and 81 parts of propylene glycol methyl ether, fully dispersing uniformly, adding 0.06 part of accelerator hexamethyl tetramine to adjust the molding time of the glue solution, sampling, testing the molding time of the glue solution by a knife method (210 ℃ hot plate) for 451 seconds, and finishing the preparation of the glue solution.
Examples 1 to 12:
at room temperature, 19 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 12 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 15 parts of glycidyl amine type epoxy resin, 11 parts of alicyclic epoxy resin, 16 parts of magnesium hydroxide and 26 parts of montmorillonite are respectively added into a glue preparation tank, after stirring for 1.75 hours at the temperature of 95 ℃, 7 parts of curing agent 4, 4-diaminodiphenylmethane and 25 parts of diamine fluorene are added, stirring is carried out for 2.75 hours at the temperature of 135 ℃, 78 parts of cyclohexanone and 58 parts of N, N-dimethylformamide are added, after the materials are fully dispersed uniformly, 0.13 part of accelerant 2-methylimidazole is added to adjust the molding time of the glue solution, sampling is carried out, the molding time (210 ℃) of the glue solution is tested by using a knife method for 530 seconds, and the glue solution is prepared by a hot plate.
Examples 1 to 13:
at room temperature, 23 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 12 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 12 parts of biphenyl epoxy resin, 5 parts of bisphenol F epoxy resin, 24 parts of graphene and 16 parts of montmorillonite are respectively added into a glue preparation tank, after stirring for 1.25 hours at the temperature of 95 ℃, 8 parts of curing agent 4, 4-diaminodiphenylmethane and 22 parts of bisamine fluorene are added, stirring is carried out for 3 hours at the temperature of 120 ℃, 27 parts of N, N-dimethylformamide and 61 parts of acetone are added, after the materials are fully dispersed uniformly, 0.17 part of accelerant 2-ethyl-4-methylimidazole is added to adjust the molding time of the glue solution, sampling is carried out, the molding time of the glue solution is tested by a knife method (210 ℃) for 476 seconds by a hot plate, and the glue solution is prepared.
Examples 1 to 14:
at room temperature, 29 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 12 parts of bisphenol fluorene epoxy resin (DGEBF for short), 7 parts of glycidyl amine epoxy resin, 8 parts of bisphenol F epoxy resin, 8 parts of o-cresol novolac epoxy resin, 16 parts of boehmite, 19 parts of magnesium hydroxide and 12 parts of hydrotalcite are respectively added into a glue preparation tank, stirred for 1.65 hours at the temperature of 100 ℃, added with 12 parts of curing agent 4, 4-diaminodiphenyl sulfone and 16 parts of diamine fluorene, stirred for 1.25 hours at the temperature of 135 ℃, added with 116 parts of ethylene glycol dimethyl ether and 47 parts of cyclohexanone to be fully and uniformly dispersed, added with 0.09 part of accelerator N, N-dimethylbenzylamine to adjust the molding time of the glue solution, sampled, the glue solution molding time (210 ℃ hot plate) tested by a knife method is 505 seconds, and the glue solution is prepared.
Examples 1 to 15:
at room temperature, 13 parts of bisphenol fluorene epoxy resin (DGEBF for short), 20 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 5 parts of glycidyl amine epoxy resin, 4 parts of isocyanate modified epoxy resin, 5 parts of bisphenol A epoxy resin, 11 parts of magnesium hydroxide, 8 parts of kaolin and 7 parts of silicon micropowder are respectively added into a glue preparation tank, stirred for 1.25 hours at 105 ℃, added with 8 parts of curing agent 4, 4-diaminodiphenylmethane and 18 parts of diamine fluorene, stirred for 3.25 hours at 125 ℃, added with 52 parts of propylene glycol methyl ether and 21 parts of butanone, fully and uniformly dispersed, added with 0.08 part of accelerator triethylamine to adjust the forming time of the glue solution, sampled, and tested by a method for the forming time (210 ℃ hot plate) 483 seconds, namely the glue solution is completely prepared.
Examples 1 to 16:
respectively adding 19 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 16 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 23 parts of glycidylamine epoxy resin, 5 parts of o-cresol novolac epoxy resin, 4 parts of alicyclic epoxy resin, 18 parts of montmorillonite, 14 parts of aluminum hydroxide and 20 parts of fumed silica into a glue preparation tank at room temperature, stirring at 95 ℃ for 0.85 hour, adding 12 parts of curing agent 4, 4-diaminodiphenylmethane and 19 parts of diamine fluorene, stirring at 120 ℃ for 3 hours, adding 45 parts of ethylene glycol dimethyl ether and 18 parts of xylene, fully and uniformly dispersing, adding 0.18 part of boron trifluoride ethylamine as an accelerator to adjust the forming time of the glue solution, sampling, and testing the forming time of the glue solution by a method (210 ℃ hot plate) for 453 seconds to finish the preparation of the glue solution.
Examples 1 to 17:
respectively adding 22 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 11 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 10 parts of bisphenol fluorene epoxy resin (DGEBF for short), 11 parts of alicyclic epoxy resin, 15 parts of resorcinol epoxy resin, 9 parts of epoxy resin of dicyclopentadiene or dicycladiene and phenolic aldehyde polycondensation resin, 21 parts of boehmite, 17 parts of hydrotalcite and 23 parts of fumed silica into a glue preparation tank at room temperature, stirring for 2 hours at the temperature of 110 ℃, adding 9 parts of curing agent 4, 4-diaminodiphenylmethane, 15 parts of diamine fluorene and 10 parts of 4, 4-diaminodiphenylsulfone, stirring for 2.75 hours at the temperature of 140 ℃, adding 74 parts of methyl acetate and 48 parts of N, N-dimethylformamide, fully and uniformly dispersing, adding 0.11 part of accelerator 2-ethyl-4-methylimidazole to adjust the forming time of glue solution, sampling, and testing the molding time (210 ℃ hot plate) of the glue solution by using a knife method for 479 seconds to finish the preparation of the glue solution.
Examples 1 to 18:
respectively adding 19 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 6 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 15 parts of bisphenol fluorene epoxy resin (DGEBF for short), 11 parts of isocyanate modified epoxy resin, 8 parts of hydantoin epoxy resin, 15 parts of glycidyl amine type epoxy resin, 16 parts of kaolin, 9 parts of graphene and 23 parts of talcum powder into a glue preparation tank at room temperature, stirring for 1.65 hours at the temperature of 105 ℃, adding 9 parts of curing agent 4, 4-diaminodiphenylmethane, 13 parts of diamine fluorene and 11 parts of 4, 4-diaminodiphenylsulfone, stirring for 2.25 hours at the temperature of 135 ℃, adding 84 parts of cyclohexanone and 102 parts of xylene, fully and uniformly dispersing, adding 0.12 part of accelerator hexamethyltetramine to adjust the forming time of the glue solution, sampling, and testing the forming time of the glue solution (210 ℃ hot plate) for 449 seconds by using a knife method to finish the preparation of the glue solution.
Examples 1 to 19:
respectively adding 14 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 11 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 13 parts of bisphenol fluorene epoxy resin (DGEBF for short), 3 parts of epoxy resin of dicyclopentadiene or dicyclic diene and phenolic aldehyde polycondensation resin, 4 parts of o-cresol novolac epoxy resin, 3 parts of alicyclic epoxy resin, 2 parts of glycidyl amine epoxy resin, 12 parts of fumed silica, 18 parts of aluminum oxide and 8 parts of magnesium hydroxide into a glue preparation tank at room temperature, stirring for 1.25 hours at 110 ℃, adding 5 parts of curing agent 4, 4-diaminodiphenylmethane, 14 parts of diamine fluorene and 9 parts of 4, 4-diaminodiphenylsulfone, stirring for 1.75 hours at 135 ℃, adding 56 parts of methyl ethyl ketone, 71 parts of butanone and 41 parts of alcohol, fully dispersing uniformly, adding 0.12 parts of accelerant aluminum acetylacetonate, 0.12 parts of accelerant, and the like, And (3) adjusting the forming time of the glue solution by 0.04 part of hexamethyltetramine, sampling, and testing the forming time (210 ℃ hot plate) of the glue solution for 485 seconds by using a knife method to finish the preparation of the glue solution.
Examples 1 to 20:
respectively adding 17 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 8 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 17 parts of bisphenol fluorene epoxy resin (DGEBF for short), 5 parts of epoxy resin of dicyclopentadiene or dicyclic diene and phenolic aldehyde polycondensation resin, 4 parts of biphenyl epoxy resin, 3 parts of o-cresol novolac epoxy resin, 4 parts of bisphenol A epoxy resin, 16 parts of graphene, 7 parts of aluminum hydroxide and 19 parts of boehmite into a glue preparation tank at room temperature, stirring at 105 ℃ for 1.5 hours, adding 7 parts of curing agent 4, 4-diaminodiphenylmethane, 9 parts of bisaminofluorene and 3 parts of 4, 4-diaminodiphenylsulfone, stirring at 135 ℃ for 2 hours, adding 83 parts of xylene, 51 parts of propylene glycol monomethyl ether and 67 parts of acetone, fully dispersing uniformly, adding 0.04 part of accelerant 2-ethyl-4-methylimidazole, and the like, 0.07 part of boron trifluoride ethylamine, adjusting the forming time of the glue solution, sampling, and testing the forming time (210 ℃ hot plate) of the glue solution for 490 seconds by using a knife method to finish the preparation of the glue solution.
Examples 1 to 21:
respectively adding 23 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 11 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 11 parts of bisphenol fluorene epoxy resin (DGEBF for short), 8 parts of bisphenol A novolac epoxy resin, 7 parts of isocyanate modified epoxy resin, 8 parts of alicyclic epoxy resin, 11 parts of epoxy resin of dicyclopentadiene or dicyclic diene and novolac polycondensation resin, 14 parts of hydrotalcite, 24 parts of montmorillonite and 19 parts of silicon micropowder into a glue preparation tank at room temperature, stirring for 1.25 hours at the temperature of 115 ℃, adding 9 parts of curing agent 4, 4-diaminodiphenylmethane, 13 parts of diamine fluorene and 12 parts of 4, 4-diaminodiphenylsulfone, stirring for 4 hours at the temperature of 130 ℃, adding 84 parts of methyl acetate, 32 parts of N, N-dimethylformamide and 81 parts of butanone, fully dispersing uniformly, adding 0.12 part of accelerant 2-methylimidazole, 0.12 part of methyl imidazole, methyl ethyl ketone and sodium benzoate, 0.05 part of aluminum acetylacetonate is used for adjusting the forming time of the glue solution, sampling is carried out, the forming time (210 ℃ hot plate) of the glue solution is tested for 507 seconds by a knife method, and the glue solution is prepared.
Preparation of second part high temperature-resistant epoxy aramid fiber-fabric prepreg
1. Basic processes of examples 2-1 to 2-21:
a. selecting a high-temperature-resistant epoxy adhesive:
the first part of the high temperature resistant epoxy adhesive prepared in the embodiments 1-1 to 1-21 is selected correspondingly in the embodiments 2-1 to 2-21;
b. preparation of high-temperature-resistant epoxy aramid fiber-fabric prepreg
Coating the fiber-fabric (aramid fiber checkered cloth, aramid fiber twill cloth, aramid fiber plain cloth, aramid fiber satin cloth, aramid fiber stitch-bonded felt, aramid fiber continuous felt, aramid fiber composite cloth and aramid fiber composite felt) with the high-temperature-resistant epoxy adhesive in the step a through a horizontal or vertical gluing machine, and baking the fiber-fabric through a baking channel of the gluing machine, wherein the baking channel of the gluing machine is 24m long and is divided into 4 sections and 6m in each section, the baking temperature range is 70-175 ℃, and the speed of the gluing machine is 7-21 m/min, so that the high-temperature-resistant epoxy aramid fiber-fabric prepreg is prepared; the indexes of the fiber-fabric prepreg are as follows: the fluidity is 18 mm-34 mm, the content of soluble resin is more than or equal to 95 percent, and the content of volatile matters is less than or equal to 2 percent.
2. The specific process parameters and test results of examples 2-1 to 2-21 are shown in Table 1 below:
table 1: the preparation process parameters of the high temperature resistant epoxy aramid fiber-fabric prepreg are as follows:
Figure BDA0003076952800000151
Figure BDA0003076952800000161
preparation of third part high temperature resistant epoxy aramid fiber insulating layer and mould pressing part
1. Basic Process for examples 3-1 to 3-21
a. High-temperature-resistant epoxy aramid fiber-fabric prepreg
The second part of the high temperature resistant epoxy aramid fiber-fabric prepreg prepared in the examples 2-1 to 2-21 is selected correspondingly in the examples 3-1 to 3-21 respectively;
b. and (3) pressing the high-temperature-resistant epoxy aramid fiber insulating layer and a molded part:
taking a high-temperature-resistant epoxy aramid fiber-fabric prepreg cut into a required shape and size according to the process requirements of a high-temperature-resistant epoxy aramid fiber insulating layer and a molded part, and placing the prepreg paving layer on a smooth stainless steel mold coated with a release agent on two sides, wherein the mold shape comprises: and (3) feeding the flat plate type, the U-shaped or other special shapes into a common hot press or a vacuum hot press with a hot plate, carrying out hot press molding under the conditions that the temperature is controlled to be 140-250 ℃ and the pressure is controlled to be 5-30 MPa, and determining the hot press molding time to be within the range of 0.5-30 h according to the thickness of a molded structural part to be 0.5-150 mm, thus obtaining the high-temperature-resistant epoxy aramid fiber insulating layer and the molded part.
2. Specific process parameters of examples 2-1 to 2-21 and technical performance test results of the high temperature-resistant epoxy aramid fiber insulating layer and the molded part product are respectively shown in the following tables 2 and 3:
table 2: the high temperature resistant epoxy aramid fiber insulating layer and the pressing technological parameters of the die pressing part are as follows:
Figure BDA0003076952800000171
table 3: the technical performance test results of the high-temperature-resistant epoxy aramid fiber insulating layer and the molded part are as follows:
Figure BDA0003076952800000172
Figure BDA0003076952800000181
note: (1) in the above table, the test values are the test results at room temperature and 50% ± 5% humidity, except that the test temperature and humidity of the bending strength are indicated.
(2) The technical performance test method comprises the following steps:
1) bending strength, shear strength: the determination is carried out according to the method specified in GB/T9341-2008;
2) water absorption: the measurement was carried out according to the method defined in GB/T1034-2008.
Example 4:
a high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, this insulating layer, mould pressing structural part are 2 layers of high temperature resistant epoxy aramid fiber-fabric prepreg that overlap and make composite material after hot briquetting;
the high-temperature-resistant epoxy aramid fiber-fabric prepreg is an aramid fiber-fabric impregnating material which is formed by impregnating aramid fiber-fabric with a high-temperature-resistant epoxy adhesive and then baking (removing part of solvent in the aramid fiber-fabric), wherein the aramid fiber-fabric impregnating material is provided with a semi-cured product, and the impregnating material comprises the following components in parts by weight: the weight percentage of the semi-cured product is 35 percent, and the weight percentage of the aramid fiber-fabric is 65 percent;
the high-temperature-resistant epoxy adhesive comprises the following components in parts by weight: 23 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 7 parts of epoxy resin of dicyclopentadiene or dicycladiene and phenolic aldehyde polycondensation resin, 2 parts of o-cresol novolac epoxy resin, 22 parts of boehmite, 10 parts of 4, 4-diaminodiphenyl sulfone, 8 parts of diamine fluorene, 28 parts of N, N-dimethylformamide and 0.14 part of hexamethyltetramine.
Example 5:
a high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, the insulating layer, mould pressing structural part are the composite material made after 50 layers of high temperature resistant epoxy aramid fiber-fabric prepreg that overlap is hot-pressed;
the high-temperature-resistant epoxy aramid fiber-fabric prepreg is an aramid fiber-fabric impregnating material which is formed by impregnating aramid fiber-fabric with a high-temperature-resistant epoxy adhesive and then baking (removing part of solvent in the aramid fiber-fabric), wherein the aramid fiber-fabric impregnating material is provided with a semi-cured product, and the impregnating material comprises the following components in parts by weight: the weight percentage of the semi-cured product is 25 percent, and the weight percentage of the aramid fiber-fabric is 75 percent;
the high-temperature-resistant epoxy adhesive comprises the following components in parts by weight: 16 parts of bis-o-cresol fluorene epoxy resin (DGEDMFF for short), 6 parts of isocyanate modified epoxy resin, 5 parts of resorcinol epoxy resin, 1 part of talcum powder, 2 parts of 4, 4-diaminodiphenyl sulfone, 4 parts of diamine fluorene, 12 parts of xylene and 0.11 part of N, N-dimethylbenzylamine.
Example 6:
a high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, the insulating layer, mould pressing structural part are the composite material that 300 layers of high temperature resistant epoxy aramid fiber-fabric prepreg that overlap are made after the hot briquetting;
the high-temperature-resistant epoxy aramid fiber-fabric prepreg is an aramid fiber-fabric impregnating material which is formed by impregnating aramid fiber-fabric with a high-temperature-resistant epoxy adhesive and then baking (removing part of solvent in the aramid fiber-fabric), wherein the aramid fiber-fabric impregnating material is provided with a semi-cured product, and the impregnating material comprises the following components in parts by weight: the weight percentage of the semi-cured substance is 15 percent, and the weight percentage of the aramid fiber-fabric is 85 percent;
the high-temperature-resistant epoxy adhesive comprises the following components in parts by weight: 25 parts of bis-di-o-cresol fluorene epoxy resin (DGEDMFF for short), 11 parts of biphenyl epoxy resin, 10 parts of bisphenol F epoxy resin, 32 parts of graphene, 11 parts of 4, 4-diaminodiphenylmethane, 11 parts of bisamine fluorene, 68 parts of butanone and 0.12 part of aluminum acetylacetonate.
Example 7:
a high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, the insulating layer, mould pressing structural part are the composite material that 200 layers of high temperature resistant epoxy aramid fiber-fabric prepreg that overlap are made after the hot briquetting;
the high-temperature-resistant epoxy aramid fiber-fabric prepreg is an aramid fiber-fabric impregnating material which is formed by impregnating aramid fiber-fabric with a high-temperature-resistant epoxy adhesive and then baking (removing part of solvent in the aramid fiber-fabric), wherein the aramid fiber-fabric impregnating material is provided with a semi-cured product, and the impregnating material comprises the following components in parts by weight: the weight percentage of the semi-cured product is 55 percent, and the weight percentage of the aramid fiber-fabric is 45 percent;
the high-temperature-resistant epoxy adhesive comprises the following components in parts by weight: 19 parts of bis-di-o-cresol fluorene epoxy resin (DGEDMFF for short), 13 parts of bis-o-cresol fluorene epoxy resin (DGEMBF for short), 4 parts of phenol novolac epoxy resin, 9 parts of alicyclic epoxy resin, 28 parts of silicon micropowder, 5 parts of 4, 4-diaminodiphenylmethane, 17 parts of diamine fluorene, 42 parts of propylene glycol monomethyl ether and 0.11 part of aluminum acetylacetonate.
Examples 8 to 14:
a high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, the insulating layer, mould pressing structural part are one layer or more than one layer of high temperature resistant epoxy aramid fiber-fabric prepreg that overlap and make composite material after the hot briquetting;
the high-temperature-resistant epoxy aramid fiber-fabric prepreg is an aramid fiber-fabric impregnating material which is formed by impregnating aramid fiber-fabric with a high-temperature-resistant epoxy adhesive and then baking the impregnated aramid fiber-fabric, wherein the impregnating material comprises the following components in parts by weight: the weight percentage of the semi-cured substance is 15-55%, and the weight percentage of the aramid fiber-fabric is 45-85%;
the high-temperature-resistant epoxy adhesive comprises the following components in parts by weight: 12-45 parts of epoxy resin, 5-35 parts of modified epoxy resin, 1-61 parts of filler, 6-34 parts of curing agent, 9.5-201 parts of solvent and 0.01-0.18 part of accelerator.
The specific weight parts of the raw materials of each component in each example are shown in the following table 4:
table 4: the specific weight parts of the raw materials of each component in examples 8-14 are as follows:
Figure BDA0003076952800000201
in the above embodiments 4 to 14: the aramid fiber-fabric is one or a mixture of more than two of aramid fiber checkered cloth, aramid fiber twill cloth, aramid fiber plain cloth, aramid fiber satin cloth, aramid fiber stitch-bonded felt, aramid fiber continuous felt, aramid fiber composite cloth and aramid fiber composite felt;
in the above embodiments 8 to 14: the epoxy resin is one or a mixture of more than two of bisphenol fluorene epoxy resin (DGEBF for short), bis-o-cresol fluorene epoxy resin (DGEMBF for short) and bis-di-o-cresol fluorene epoxy resin (DGEDMFF for short);
in the above embodiments 8 to 14: the modified epoxy resin is one or a mixture of more than two of alicyclic glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, biphenyl type epoxy resin, phenol type novolac epoxy resin, o-cresol type novolac epoxy resin, bisphenol A novolac epoxy resin, resorcinol type epoxy resin, epoxy resin of dicyclopentadiene or dicyclic diene and novolac polycondensation resin, isocyanate modified epoxy resin and hydantoin epoxy resin;
in the above embodiments 8 to 14: the curing agent is a mixture of two or more than two of 4, 4-diaminodiphenylmethane, 4-diaminodiphenyl sulfone and diamine fluorene;
in the above embodiments 8 to 14: the filler is one or a mixture of more than two of aluminum hydroxide, alumina, boehmite, silica micropowder, hydrotalcite and talcum powder;
in the above embodiments 8 to 14: the accelerant is one or a mixture of more than two of 2-methylimidazole, 2-ethyl-4-methylimidazole, N-dimethylbenzylamine, boron trifluoride ethylamine, triethylamine, hexamethyltetramine and aluminum acetylacetonate;
in the above embodiments 8 to 14: the solvent is one or a mixture of more than two of toluene, xylene, ethylene glycol dimethyl ether, ethylene glycol ethyl ether acetate, propylene glycol methyl ether, methyl ethyl ketone, cyclohexanone, methyl acetate, butanone, acetone, DMF and ethanol.
Example 15:
a preparation method of a high temperature-resistant epoxy aramid fiber insulating layer and a molded part comprises the following steps:
a. preparing a high-temperature-resistant epoxy adhesive:
(a) preparing materials: taking raw materials of the components according to the weight ratio of 12-45 parts of epoxy resin, 5-35 parts of modified epoxy resin, 1-61 parts of filler, 6-34 parts of curing agent, 9.5-201 parts of solvent and 0.01-0.18 part of accelerator; the specific raw materials and the weight parts are the same as those in any one of the embodiments 4 to 14;
(b) adding the epoxy resin, the modified epoxy resin and the filler in the formula amount in the step (a) into a glue preparation tank at room temperature, stirring for 1.25 hours at 105 ℃, adding a curing agent, stirring for 3.25 hours at 125 ℃, adding an accelerant to adjust the forming time of the glue solution after the glue solution is fully dispersed uniformly, sampling, testing the forming time of the glue solution by using a knife method, and completing preparation of the high-temperature-resistant epoxy adhesive when the forming time is 440-530 seconds under the condition of a hot plate at 210 ℃ to obtain the high-temperature-resistant epoxy adhesive;
b. preparing high-temperature-resistant epoxy aramid fiber-fabric prepreg:
coating the high-temperature-resistant epoxy adhesive in the step a on aramid fiber-fabric by a horizontal or vertical gluing machine, and baking the aramid fiber-fabric by a baking channel of the gluing machine, wherein the baking channel of the gluing machine is 24m long and is divided into 4 sections and 6m sections, the baking temperature is 90-175 ℃, the speed of the gluing machine is 21m/min, and the high-temperature-resistant epoxy aramid fiber-fabric prepreg is prepared after baking;
the aramid fiber-fabric is one or a mixture of more than two of aramid fiber checkered cloth, aramid fiber twill cloth, aramid fiber plain cloth, aramid fiber satin cloth, aramid fiber stitch-bonded felt, aramid fiber continuous felt, aramid fiber composite cloth and aramid fiber composite felt;
c. and (3) pressing the high-temperature-resistant epoxy aramid fiber insulating layer and a molded part:
cutting the prepared high temperature resistant epoxy aramid fiber-fabric prepreg into a required shape and size according to the drawing (process) requirements of a high temperature resistant epoxy aramid fiber insulating layer and a molded part, putting the 2 layers of the cut high temperature resistant epoxy alkali-free aramid fiber-fabric prepreg on a stainless steel mold (the two surfaces of which are coated with a release agent), feeding the high temperature resistant epoxy aramid fiber-fabric prepreg into a common hot press or a vacuum hot press with a hot plate, controlling the temperature to be 240 ℃ and the pressure to be 23MPa, and carrying out hot press molding for 0.5h to obtain the high temperature resistant epoxy aramid fiber insulating layer and the molded part.
Example 16:
a preparation method of a high temperature-resistant epoxy aramid fiber insulating layer and a molded part comprises the following steps:
a. preparing a high-temperature-resistant epoxy adhesive:
(a) preparing materials: taking raw materials of the components according to the weight ratio of 12-45 parts of epoxy resin, 5-35 parts of modified epoxy resin, 1-61 parts of filler, 6-34 parts of curing agent, 9.5-201 parts of solvent and 0.01-0.18 part of accelerator; the specific raw materials and the weight parts are the same as those in any one of the embodiments 4 to 14;
(b) adding the epoxy resin, the modified epoxy resin and the filler in the formula amount in the step (a) into a glue preparation tank at room temperature, stirring for 0.85 hour at the temperature of 95 ℃, adding a curing agent, stirring for 3 hours at the temperature of 120 ℃, adding an accelerant to adjust the forming time of the glue solution after the glue solution is fully and uniformly dispersed, sampling, testing the forming time of the glue solution by using a knife method, and preparing the high-temperature-resistant epoxy adhesive after the preparation is finished under the condition of a hot plate at 210 ℃ and when the forming time is 440-530 seconds;
b. preparing high-temperature-resistant epoxy aramid fiber-fabric prepreg:
coating the high-temperature-resistant epoxy adhesive in the step a on aramid fiber-fabric by a horizontal or vertical gluing machine, and baking the aramid fiber-fabric by a baking channel of the gluing machine, wherein the baking channel of the gluing machine is 24m long and is divided into 4 sections and 6m in each section, the baking temperature is 85-175 ℃, the speed of the gluing machine is 20m/min, and the high-temperature-resistant epoxy aramid fiber-fabric prepreg is prepared after baking;
the aramid fiber-fabric was the same as in example 15;
c. and (3) pressing the high-temperature-resistant epoxy aramid fiber insulating layer and a molded part:
cutting the prepared high temperature resistant epoxy aramid fiber-fabric prepreg into a required shape and size according to the requirements of a high temperature resistant epoxy aramid fiber insulating layer and a drawing (process) of a molded part, putting 300 layers of the cut high temperature resistant epoxy aramid fiber-fabric prepreg on a stainless steel mold (the two sides of which are coated with a release agent), sending the high temperature resistant epoxy aramid fiber-fabric prepreg into a common hot press or a vacuum hot press with a hot plate, controlling the temperature to be 240 ℃ and the pressure to be 26MPa, and carrying out hot press molding for 30 hours to obtain the high temperature resistant epoxy aramid fiber insulating layer and the molded part.
Example 17:
a preparation method of a high temperature-resistant epoxy aramid fiber insulating layer and a molded part comprises the following steps:
a. preparing a modified epoxy adhesive:
(a) preparing materials: taking raw materials of the components according to the weight ratio of 12-45 parts of epoxy resin, 5-35 parts of modified epoxy resin, 1-61 parts of filler, 6-34 parts of curing agent, 9.5-201 parts of solvent and 0.01-0.18 part of accelerator; (ii) a The specific raw materials and the weight parts are the same as those in any one of the embodiments 4 to 14;
(b) adding the epoxy resin, the modified epoxy resin and the filler in the formula amount in the step (a) into a glue preparation tank at room temperature, stirring for 2 hours at the temperature of 110 ℃, adding a curing agent, stirring for 2.75 hours at the temperature of 140 ℃, adding an accelerant to adjust the forming time of the glue solution after the glue solution is fully and uniformly dispersed, sampling, testing the forming time of the glue solution by using a knife method, and preparing the high-temperature-resistant epoxy adhesive after the preparation is finished under the condition of a hot plate at the temperature of 210 ℃ and when the forming time is 440-530 seconds;
b. preparing high-temperature-resistant epoxy aramid fiber-fabric prepreg:
coating the high-temperature-resistant epoxy adhesive in the step a on aramid fiber-fabric by a horizontal or vertical gluing machine, and baking the aramid fiber-fabric by a baking channel of the gluing machine, wherein the baking channel of the gluing machine is 24m long and is divided into 4 sections and 6m sections, the baking temperature is 85-165 ℃, the speed of the gluing machine is 13m/min, and the high-temperature-resistant epoxy aramid fiber-fabric prepreg is prepared after baking;
the aramid fiber-fabric was the same as in example 15;
c. and (3) pressing the high-temperature-resistant epoxy aramid fiber insulating layer and a molded part:
cutting the prepared high temperature resistant epoxy aramid fiber-fabric prepreg into required shape and size according to drawing (process) requirements of insulating layers and mould pressing structural members for extra-high voltage direct current power transmission and transformation, placing 150 layers of the cut high temperature resistant epoxy aramid fiber-fabric prepreg on a stainless steel mould (with two surfaces coated with a release agent), sending the high temperature resistant epoxy aramid fiber-fabric prepreg into a common hot press or a vacuum hot press with a hot plate, controlling the temperature to be 140-250 ℃ and the pressure to be 5-30 MPa for hot press molding, and obtaining the high temperature resistant epoxy aramid fiber insulating layers and mould pressing finished pieces, wherein the hot press molding time is 15.5 h.
Example 18:
a high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, this high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece are one deck and more than one deck high temperature resistant epoxy aramid fiber-fabric prepreg that overlap and make the composite material after the hot briquetting (namely high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece);
the high-temperature-resistant epoxy aramid fiber-fabric prepreg is formed by impregnating aramid fiber-fabric with an epoxy adhesive and baking (removing part of solvent in the aramid fiber-fabric) the aramid fiber-fabric prepreg with a semi-cured material;
the high-temperature-resistant epoxy adhesive comprises the following components in parts by weight: 12 parts of epoxy resin, 5 parts of modified epoxy resin, 1 part of filler, 6 parts of curing agent, 9.5 parts of solvent and 0.01 part of accelerator.
Example 19:
a high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, this high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece are one deck and more than one deck high temperature resistant epoxy aramid fiber-fabric prepreg that overlap and make the composite material after the hot briquetting (namely high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece);
the high-temperature-resistant epoxy aramid fiber-fabric prepreg is formed by impregnating aramid fiber-fabric with an epoxy adhesive and baking (removing part of solvent in the aramid fiber-fabric) the aramid fiber-fabric prepreg with a semi-cured material;
the high-temperature-resistant epoxy adhesive comprises the following components in parts by weight: 45 parts of epoxy resin, 35 parts of modified epoxy resin, 61 parts of filler, 34 parts of curing agent, 201 parts of solvent and 0.18 part of accelerator.
Example 20:
a high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, this high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece are one deck and more than one deck high temperature resistant epoxy aramid fiber-fabric prepreg that overlap and make the composite material after the hot briquetting (namely high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece);
the high-temperature-resistant epoxy aramid fiber-fabric prepreg is formed by impregnating aramid fiber-fabric with an epoxy adhesive and baking (removing part of solvent in the aramid fiber-fabric) the aramid fiber-fabric prepreg with a semi-cured material;
the high-temperature-resistant epoxy adhesive comprises the following components in parts by weight: 28 parts of epoxy resin, 20 parts of modified epoxy resin, 31 parts of filler, 20 parts of curing agent, 105 parts of solvent and 0.1 part of accelerator.
Example 21:
a high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, in the high temperature resistant epoxy aramid fiber-fabric preimpregnation material: the weight percentage of the semi-cured substance is 15 percent, and the weight percentage of the aramid fiber-fabric is 85 percent; the same as in any of examples 18 to 20, except that the above-mentioned process is omitted.
Example 22:
a high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, in the high temperature resistant epoxy aramid fiber-fabric preimpregnation material: the weight percentage of the semi-cured product is 55 percent, and the weight percentage of the aramid fiber-fabric is 45 percent; the same as in any of examples 18 to 20, except that the above-mentioned process is omitted.
Example 23:
a high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, in the high temperature resistant epoxy aramid fiber-fabric preimpregnation material: the weight percentage of the semi-cured product is 35 percent, and the weight percentage of the aramid fiber-fabric is 65 percent; the same as in any of examples 18 to 20, except that the above-mentioned process is omitted.
Example 24:
a preparation method of a high temperature-resistant epoxy aramid fiber insulating layer and a molded part comprises the following steps:
a. preparing a high-temperature-resistant epoxy adhesive:
(a) preparing materials: taking raw materials of each component according to the composition and weight ratio of 12 parts of epoxy resin, 5 parts of modified epoxy resin, 2 parts of filler, 6 parts of curing agent, 10 parts of solvent and 0.01 part of accelerator;
(b) adding the epoxy resin, the modified epoxy resin and the filler in the formula amount in the step (a) into a glue preparation tank at room temperature, stirring for 2 hours at 55 ℃, adding a curing agent, stirring for 4 hours at 100 ℃, cooling, adding a solvent, fully and uniformly dispersing, adding an accelerant to adjust the forming time of the glue solution, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the epoxy adhesive under the condition of a hot plate at 210 ℃ and when the forming time is 440-530 seconds, thus obtaining the high-temperature-resistant epoxy adhesive;
b. preparing high-temperature-resistant epoxy aramid fiber-fabric prepreg:
dipping the aramid fiber-fabric into the high-temperature-resistant epoxy adhesive in the step a through a gluing machine (which can be a horizontal or vertical gluing machine), baking the aramid fiber-fabric through a baking channel of the gluing machine, wherein the baking channel of the gluing machine is 24m long and is divided into 4 sections and 6m in each section, the baking temperature range is 70-175 ℃, the speed of the gluing machine is 7m/min, and the high-temperature-resistant epoxy aramid fiber-fabric prepreg is prepared after baking;
c. and (3) pressing the high-temperature-resistant epoxy aramid fiber insulating layer and a molded part:
and (c) cutting the high-temperature-resistant epoxy aramid fiber-fabric prepreg prepared in the step (b) into a required shape and size according to the drawing (process) requirements of the high-temperature-resistant epoxy aramid fiber insulating layer and a molded part, placing the cut layer of high-temperature-resistant epoxy aramid fiber-fabric prepreg on a stainless steel mold (the two surfaces of which are coated with a release agent), feeding the cut layer of high-temperature-resistant epoxy aramid fiber-fabric prepreg into a hot press (which can be a common hot press or a vacuum hot press) with a hot plate, controlling the temperature to be 140 ℃ and the pressure to be 5MPa, and carrying out hot press molding for 0.5h to obtain the high-temperature-resistant epoxy aramid fiber insulating layer and the molded part.
Example 25:
a preparation method of a high temperature-resistant epoxy aramid fiber insulating layer and a molded part comprises the following steps:
a. preparing a high-temperature-resistant epoxy adhesive:
(a) preparing materials: taking raw materials of the components according to the weight ratio of 45 parts of epoxy resin, 35 parts of modified epoxy resin, 60 parts of filler, 34 parts of curing agent, 200 parts of solvent and 0.18 part of accelerator;
(b) adding the epoxy resin, the modified epoxy resin and the filler in the formula amount in the step (a) into a glue preparation tank at room temperature, stirring for 0.5 hour at the temperature of 115 ℃, adding a curing agent, stirring for 1 hour at the temperature of 145 ℃, cooling, adding a solvent, fully and uniformly dispersing, adding an accelerator to adjust the forming time of the glue solution, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the epoxy adhesive when the forming time is 440-530 seconds under the condition of a hot plate at 210 ℃ to obtain the high-temperature-resistant epoxy adhesive;
b. preparing high-temperature-resistant epoxy aramid fiber-fabric prepreg:
dipping the aramid fiber-fabric into the high-temperature-resistant epoxy adhesive in the step a through a gluing machine (which can be a horizontal or vertical gluing machine), baking the aramid fiber-fabric through a baking channel of the gluing machine, wherein the length of the baking channel of the gluing machine is 24m, the baking channel is divided into 4 sections and 6m in each section, the baking temperature range is 70-175 ℃, the speed of the gluing machine is 21m/min, and the high-temperature-resistant epoxy aramid fiber-fabric prepreg is prepared after baking;
c. and (3) pressing the high-temperature-resistant epoxy aramid fiber insulating layer and a molded part:
and (b) cutting the high-temperature-resistant epoxy aramid fiber-fabric prepreg prepared in the step (b) into a required shape and size according to the drawing (process) requirements of the high-temperature-resistant epoxy aramid fiber insulating layer and a molded part, placing 35 layers of the cut high-temperature-resistant epoxy aramid fiber-fabric prepreg on a stainless steel mold (the two surfaces of which are coated with a release agent), feeding the high-temperature-resistant epoxy aramid fiber-fabric prepreg into a hot press (which can be a common hot press or a vacuum hot press) with a hot plate, controlling the temperature to be 250 ℃ and the pressure to be 30MPa, and carrying out hot press molding for 15.5 hours to obtain the high-temperature-resistant epoxy aramid fiber insulating layer and the molded part.
Example 26:
a preparation method of a high temperature-resistant epoxy aramid fiber insulating layer and a molded part comprises the following steps:
a. preparing a high-temperature-resistant epoxy adhesive:
(a) preparing materials: taking raw materials of the components according to the weight proportion of 29 parts of epoxy resin, 20 parts of modified epoxy resin, 30 parts of filler, 20 parts of curing agent, 100 parts of solvent and 0.09 part of accelerant;
(b) adding the epoxy resin, the modified epoxy resin and the filler in the formula amount in the step (a) into a glue preparation tank at room temperature, stirring for 1.5 hours at the temperature of 85 ℃, adding a curing agent, stirring for 2.5 hours at the temperature of 125 ℃, cooling, adding a solvent, fully and uniformly dispersing, adding an accelerator to adjust the forming time of the glue solution, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the epoxy adhesive when the forming time is 440-530 seconds under the condition of a hot plate at 210 ℃ to obtain the high-temperature-resistant epoxy adhesive;
b. preparing high-temperature-resistant epoxy aramid fiber-fabric prepreg:
dipping the aramid fiber-fabric into the high-temperature-resistant epoxy adhesive in the step a through a gluing machine (which can be a horizontal or vertical gluing machine), baking the aramid fiber-fabric through a baking channel of the gluing machine, wherein the baking channel of the gluing machine is 24m long and is divided into 4 sections and 6m in each section, the baking temperature range is 70-175 ℃, the speed of the gluing machine is 14m/min, and the high-temperature-resistant epoxy aramid fiber-fabric prepreg is prepared after baking;
c. and (3) pressing the high-temperature-resistant epoxy aramid fiber insulating layer and a molded part:
and (b) cutting the high-temperature-resistant epoxy aramid fiber-fabric prepreg prepared in the step (b) into a required shape and size according to the drawing (process) requirements of the high-temperature-resistant epoxy aramid fiber insulating layer and a molded part, placing the cut 12 layers of overlapped high-temperature-resistant epoxy aramid fiber-fabric prepreg on a stainless steel mold (the two surfaces of which are coated with a release agent), feeding the high-temperature-resistant epoxy aramid fiber-fabric prepreg into a hot press (which can be a common hot press or a vacuum hot press) with a hot plate, controlling the temperature to be 190 ℃ and the pressure to be 18MPa for hot press molding, and performing hot press molding for 6 hours to obtain the high-temperature-resistant epoxy aramid fiber insulating layer and the molded part.
In the above embodiments 18 to 26:
the epoxy resin is one or a mixture of more than two of bisphenol fluorene epoxy resin (DGEBF for short), bis-o-cresol fluorene epoxy resin (DGEMBF for short) and bis-di-o-cresol fluorene epoxy resin (DGEDMFF for short);
the modified epoxy resin is bisphenol A type epoxy resin (product production providing company and brand may be DER-383 of Dow, DER-331 of Dow, E-51 of Baling, CYD-128 of Baling, etc.), bisphenol F type epoxy resin (product production providing company and brand may be EPON-862 of Hansen Miji, NPEF-170 of Nanya epoxy resin (Kunshan), etc.), alicyclic epoxy resin (product production providing company and brand may be TDE-85 of Hubei Xinrunder chemical Co., Ltd., CEL2021P of DAICEL, UVR-6110 of DOW, CY-179 of Hunan, etc.), glycidyl amine type epoxy resin (product production providing company and brand may be AG: Shanghai synthetic resin research institute, etc.), (product production providing company and brand may be DE-383 of Shanghai, etc.), Biphenyl type epoxy resin (product manufacturing and providing enterprises and brands may be BPNE3501LL/9781 of Jiangshan materials science and technology Limited in Hunan), phenol type novolac epoxy resin (product manufacturing and providing enterprises and brands may be NPPN-638S of Nanasia epoxy resin (Kunshan) Limited, EPON 154 of Hansen Mitsukuji materials group in USA, DPNH9501 of Jiangshan materials science and technology Limited in Hunan, etc.), o-cresol type novolac epoxy resin (product manufacturing and providing enterprises and brands may be N-XP of Japan ink corporation, CNE202 of Taiwan Changchun resin factory, NPCN-704/703 of Nanasia epoxy resin (Kunshan) Limited, etc.), bisphenol A novolac type epoxy resin (product manufacturing and providing enterprises and brands may be BNE200 of Taiwan Changchun resin factory, F-51 of Shanghai Satsu chemical technology Limited in China, etc.), bisphenol A novolac type epoxy resin (product manufacturing and brands may be BNE200 of Taiwan China, F-51 of Shanghai Katsu technology Limited in China, etc.), One or a mixture of two or more of resorcinol type epoxy resin (product production providing company and brand may be ERISYS RDGE-H of Jia Dida chemical Co., Ltd., YF-554 of Guangzhou Yifu chemical materials Co., Ltd.), epoxy resin of dicyclopentadiene or dicycladiene and phenol-formaldehyde polycondensation resin (product production providing company and brand may be NPNE1501 of Hunan Jiasheng Material science and technology Co., Ltd., DNE260 of Jinninghuaka resin Co., Ltd., DNE280A75 of Tiangao New technology Co., Ltd.), isocyanate modified epoxy resin (product production providing company and brand may be A-IME AER4152 of Jiangsai chemical Co., Ltd., SEB-350 of SHIN-A T & C, etc.), and hydantoin type epoxy resin (product production providing company and brand may be Whitman electronic material Co., Whitman, HY-070, etc.) An agent;
the curing agent is a mixture of two or more than two of 4, 4-diaminodiphenylmethane, 4-diaminodiphenyl sulfone and diamine fluorene;
the filler is one or a mixture of more than two of aluminum hydroxide, aluminum oxide, boehmite, magnesium hydroxide, silicon micropowder, montmorillonite, kaolin, fumed silica, silicon dioxide micropowder, graphene, hydrotalcite and talcum powder;
the accelerant is one or a mixture of more than two of 2-methylimidazole, 2-ethyl-4-methylimidazole, N-dimethylbenzylamine, boron trifluoride ethylamine, triethylamine, hexamethyltetramine and aluminum acetylacetonate;
the solvent is one or a mixture of more than two of toluene, xylene, ethylene glycol dimethyl ether, ethylene glycol ethyl ether acetate, propylene glycol methyl ether, methyl ethyl ketone, cyclohexanone, methyl acetate, butanone, acetone, N-dimethylformamide and ethanol;
the aramid fiber-fabric is aramid fiber plaid (product production providing enterprises can be DuPont, Japanese emperor, Chengdou morning new material science and technology Co., Ltd.), aramid fiber twill (product production providing enterprises can be David Co., Minda textile Co., Shantou City, Minda textile Co., Ltd., Jiangsu Kangdun new material, etc.), aramid fiber plaid (product production providing enterprises can be David Kong Special weaving science and technology Co., Shantou Kong, Minda textile Co., Ltd., Jiangsu Kangdun new material, etc.), aramid fiber satin cloth (product production providing enterprises can be Jiangyin Hua textile Co., Ltd., Yixing Hua Jie carbon fiber product Co., Ltd., Yixing Hua high performance fiber weaving Co., etc.), aramid fiber stitch-woven felt (product production providing enterprises can be Zhejiang Wei De Wei Yongda, etc.), The aramid fiber continuous felt (the product production providing enterprise can be Wednd environmental protection science and technology Co., Ltd. from Zhejiang), the aramid fiber composite cloth (the product production providing enterprise can be Wednd environmental protection science and technology Co., Ltd. from Zhejiang) and the aramid fiber composite felt (the product production providing enterprise can be Wednd environmental protection science and technology Co., Ltd. from Zhejiang).
Examples 24 to 26 above: the high-temperature-resistant epoxy aramid fiber-fabric prepreg prepared in the step b is a high-temperature-resistant epoxy aramid fiber-fabric prepreg with a semi-cured product on an aramid fiber-fabric, wherein the high-temperature-resistant epoxy aramid fiber-fabric prepreg comprises the following components in percentage by weight: the weight percentage of the semi-cured substance is in the range of 15-55%, the weight percentage of the aramid fiber-fabric is in the range of 45-85%, and the sum of the weight percentages of the semi-cured substance and the aramid fiber-fabric is 100%.
In the above embodiments 15 to 17, 24 to 26: the shape of the stainless steel mold in step c can be flat plate type, U-shaped, L-shaped or similar shape, and other special shapes.
In the above embodiment: and c, bending strength of the prepared high-temperature-resistant epoxy aramid fiber insulating layer and the molded part is larger than 330MPa at the temperature of 230 ℃, the bending strength retention rate of 96h (h) at the temperature of 121 ℃ and the humidity of 100% reaches more than 50% at normal temperature, namely more than 275MPa, and the shear strength is larger than or equal to 25 MPa.
In the above embodiment: the process parameters (temperature, pressure, time, concentration, vehicle speed, etc.) and the amounts of the components in each step are within the range, and any point can be applicable.
In the above embodiment: the percentages used, not specifically noted, are weight (mass) percentages or percentages known to those skilled in the art; the proportions used, not specifically noted, are weight (mass) proportions; the parts by weight may each be grams or kilograms.
The present invention and the technical contents not specifically described in the above examples are the same as those of the prior art, and the raw materials are all commercially available products.
The present invention is not limited to the above-described embodiments, and the present invention can be implemented with the above-described advantageous effects.

Claims (7)

1. A high temperature resistant epoxy aramid fiber insulating layer, mould pressing finished piece, characterized by: the high-temperature-resistant epoxy aramid fiber insulating layer and the molded part are composite materials prepared by hot-press molding one or more layers of overlapped high-temperature-resistant epoxy aramid fiber-fabric prepreg;
the high-temperature-resistant epoxy aramid fiber-fabric prepreg is formed by impregnating aramid fiber-fabric with an epoxy adhesive and then baking the impregnated aramid fiber-fabric with a semi-cured product;
the aramid fiber-fabric is one or a mixture of more than two of aramid fiber checkered cloth, aramid fiber twill cloth, aramid fiber plain cloth, aramid fiber satin cloth, aramid fiber stitch-bonded felt, aramid fiber continuous felt, aramid fiber composite cloth and aramid fiber composite felt;
the high-temperature-resistant epoxy adhesive comprises the following components in parts by weight: 12-45 parts of epoxy resin, 5-35 parts of modified epoxy resin, 1-61 parts of filler, 6-34 parts of curing agent, 9.5-201 parts of solvent and 0.01-0.18 part of accelerator;
the epoxy resin is one or a mixture of more than two of bisphenol fluorene epoxy resin, bis-o-cresol fluorene epoxy resin and bis-di-o-cresol fluorene epoxy resin;
the modified epoxy resin is one or a mixture of more than two of bisphenol A epoxy resin, bisphenol F epoxy resin, alicyclic epoxy resin, glycidyl amine epoxy resin, biphenyl epoxy resin, phenol novolac epoxy resin, o-cresol novolac epoxy resin, bisphenol A novolac epoxy resin, resorcinol epoxy resin, epoxy resin of dicyclopentadiene or dicyclopentadiene and phenolic polycondensation resin, isocyanate modified epoxy resin and hydantoin epoxy resin;
the curing agent is a mixture of two or more than two of 4, 4-diaminodiphenylmethane, 4-diaminodiphenyl sulfone and diamine fluorene;
the filler is one or a mixture of more than two of aluminum hydroxide, aluminum oxide, boehmite, magnesium hydroxide, silicon micropowder, montmorillonite, kaolin, fumed silica, silicon dioxide micropowder, graphene, hydrotalcite and talcum powder;
the accelerant is one or a mixture of more than two of 2-methylimidazole, 2-ethyl-4-methylimidazole, N-dimethylbenzylamine, boron trifluoride ethylamine, triethylamine, hexamethyltetramine and aluminum acetylacetonate;
the solvent is one or a mixture of more than two of toluene, xylene, ethylene glycol dimethyl ether, ethylene glycol ethyl ether acetate, propylene glycol methyl ether, methyl ethyl ketone, cyclohexanone, methyl acetate, butanone, acetone, N-dimethylformamide and ethanol.
2. The high temperature resistant epoxy aramid fiber insulation layer and molded part as claimed in claim 1, wherein: in the high-temperature-resistant epoxy aramid fiber-fabric prepreg: the weight percentage of the semi-cured substance is 15-55%, and the weight percentage of the aramid fiber-fabric is 45-85%.
3. The high temperature resistant epoxy aramid fiber insulating layer and the molded part according to claim 1 or 2, which is characterized in that: the bending strength of the high-temperature-resistant epoxy aramid fiber insulating layer and the molded part is more than 330MPa at the temperature of 230 ℃, the bending strength retention rate of 96 hours at the temperature of 121 ℃ and the humidity of 100% reaches more than 50% at normal temperature, namely more than 275MPa, and the shear strength is more than or equal to 25 MPa.
4. A preparation method of a high-temperature-resistant epoxy aramid fiber insulating layer and a molded part is characterized by comprising the following steps:
a. preparing a high-temperature-resistant epoxy adhesive:
(a) preparing materials: taking raw materials of the components according to the weight ratio of 12-45 parts of epoxy resin, 5-35 parts of modified epoxy resin, 1-61 parts of filler, 6-34 parts of curing agent, 9.5-201 parts of solvent and 0.01-0.18 part of accelerator;
the epoxy resin is one or a mixture of more than two of bisphenol fluorene epoxy resin, bis-o-cresol fluorene epoxy resin and bis-di-o-cresol fluorene epoxy resin;
the modified epoxy resin is one or a mixture of more than two of bisphenol A epoxy resin, bisphenol F epoxy resin, alicyclic epoxy resin, glycidyl amine epoxy resin, biphenyl epoxy resin, phenol novolac epoxy resin, o-cresol novolac epoxy resin, bisphenol A novolac epoxy resin, resorcinol epoxy resin, epoxy resin of dicyclopentadiene or dicyclopentadiene and phenolic polycondensation resin, isocyanate modified epoxy resin and hydantoin epoxy resin;
the curing agent is a mixture of two or more than two of 4, 4-diaminodiphenylmethane, 4-diaminodiphenyl sulfone and diamine fluorene;
the filler is one or a mixture of more than two of aluminum hydroxide, aluminum oxide, boehmite, magnesium hydroxide, silicon micropowder, montmorillonite, kaolin, fumed silica, silicon dioxide micropowder, graphene, hydrotalcite and talcum powder;
the accelerant is one or a mixture of more than two of 2-methylimidazole, 2-ethyl-4-methylimidazole, N-dimethylbenzylamine, boron trifluoride ethylamine, triethylamine, hexamethyltetramine and aluminum acetylacetonate;
the solvent is one or a mixture of more than two of toluene, xylene, ethylene glycol dimethyl ether, ethylene glycol ethyl ether acetate, propylene glycol methyl ether, methyl ethyl ketone, cyclohexanone, methyl acetate, butanone, acetone, N-dimethylformamide and ethanol;
(b) adding the epoxy resin, the modified epoxy resin and the filler in the formula amount in the step (a) into a glue preparation tank at room temperature, stirring for 0.5-2 hours at the temperature of 55-115 ℃, adding a curing agent, stirring for 1-4 hours at the temperature of 100-145 ℃, cooling, adding a solvent, uniformly dispersing, adding an accelerator to adjust the forming time of the glue solution, sampling, testing the forming time of the glue solution by using a knife method, and finishing the preparation of the epoxy adhesive when the forming time is 440-530 seconds under the condition of a 210 ℃ hot plate to obtain the high-temperature-resistant epoxy adhesive;
b. preparing high-temperature-resistant epoxy aramid fiber-fabric prepreg:
dipping the aramid fiber-fabric into the high-temperature-resistant epoxy adhesive in the step a through a gluing machine, and baking the aramid fiber-fabric through a baking channel of the gluing machine, wherein the baking channel of the gluing machine is 24m long and is divided into 4 sections and 6m in each section, the baking temperature range is 70-175 ℃, the speed of the gluing machine is 7-21 m/min, and the high-temperature-resistant epoxy aramid fiber-fabric prepreg is prepared after baking;
the aramid fiber-fabric is one or a mixture of more than two of aramid fiber checkered cloth, aramid fiber twill cloth, aramid fiber plain cloth, aramid fiber satin cloth, aramid fiber stitch-bonded felt, aramid fiber continuous felt, aramid fiber composite cloth and aramid fiber composite felt;
c. and (3) pressing the high-temperature-resistant epoxy aramid fiber insulating layer and a molded part:
cutting the high temperature resistant epoxy aramid fiber-fabric prepreg prepared in the step b into a required shape and size according to the drawing requirements of the high temperature resistant epoxy aramid fiber insulating layer and a molded part, placing one or more layers of the cut high temperature resistant epoxy aramid fiber-fabric prepreg on a stainless steel mold, feeding the high temperature resistant epoxy aramid fiber-fabric prepreg into a hot press with a hot plate, controlling the temperature to be 140-250 ℃ and the pressure to be 5-30 MPa for hot press molding, and determining the hot press molding time to be 0.5-30 h according to the thickness of a molded structural part, thus preparing the high temperature resistant epoxy aramid fiber insulating layer and the molded part.
5. The preparation method of the high temperature resistant epoxy aramid fiber insulating layer and the molded part according to claim 4 is characterized in that: the high-temperature-resistant epoxy aramid fiber-fabric prepreg prepared in the step b is a high-temperature-resistant epoxy aramid fiber-fabric prepreg with a semi-cured product on an aramid fiber-fabric, wherein the high-temperature-resistant epoxy aramid fiber-fabric prepreg comprises the following components in percentage by weight: the weight percentage of the semi-cured substance is 15-55%, and the weight percentage of the aramid fiber-fabric is 45-85%.
6. The preparation method of the high temperature resistant epoxy aramid fiber insulating layer and the molded part according to claim 4 is characterized in that: the shape of the stainless steel die in the step c is a flat plate shape, a U shape, an L shape or the like.
7. The preparation method of the high temperature resistant epoxy aramid fiber insulating layer and the molded part according to the claim 4, 5 or 6 is characterized in that: and c, bending strength of the prepared high-temperature-resistant epoxy aramid fiber insulating layer and the molded part is greater than 330MPa at the temperature of 230 ℃, the bending strength retention rate of 96h at the temperature of 121 ℃ and the humidity of 100% reaches more than 50% at normal temperature, namely, the bending strength retention rate is greater than 275MPa, and the shear strength is greater than or equal to 25 MPa.
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