Epoxy resin composition, composite material and preparation

Abstract

The invention discloses an epoxy resin composition, a composite material and preparation. The composition comprises the following components in parts by mass: 30-50 parts of epoxy resin, 1-10 parts of modified boron nitride, 0.5-2 parts of a curing agent, 0.1-1 part of an accelerant and 0.2-0.8 part of a dispersing agent, the epoxy resin composite material comprises an epoxy resin composition and an insulating fiber material, the modified boron nitride and the epoxy resin are compounded, and meanwhile, the dosage of the modified boron nitride is small, so that the heat dissipation effect of the epoxy resin is greatly improved; the modified boron nitride is compounded with the insulating fibers with high tensile strength, and the epoxy resin composition is immersed into the insulating fibers, so that the tensile property of the composite material is enhanced, and meanwhile, the heat transfer rate of the modified boron nitride is improved by a heat conduction path constructed by the insulating fibers, and the heat conductivity of the epoxy resin composite material is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of epoxy resin materials, and in particular to an epoxy resin composition and a composite material and their preparation. Background Art

[0002] In recent years, with the development of miniaturization, lightweight, high integration, high power and high density of microelectronic technology, more heat will be generated during use. In addition, it is impossible to make an ideal flat surface by mechanical processing. Therefore, there are many grooves or gaps between the CPU, chip and other heat-generating parts and the radiator. Air is a poor conductor of heat. The grooves and gaps will seriously reduce the heat dissipation efficiency. The small working space makes the working temperature of electronic components very high, which greatly reduces the service life and reliability of electronic components. Insulating thermal conductive composites are used as filling materials between heating parts and radiators. They increase the contact area between heating parts and heat sinks, reduce air thermal resistance, and are important factors in improving heat dissipation efficiency.

[0003] Commonly used insulating thermal conductive materials include epoxy resin materials, but epoxy resin has low thermal conductivity and poor mechanical properties, resulting in poor durability and poor heat dissipation effect of epoxy resin. The existing technology usually adds metal materials to enhance its thermal conductivity and tensile strength, but this will significantly reduce the insulation performance of epoxy resin.

[0004] Therefore, how to simultaneously improve the thermal conductivity and tensile strength of epoxy resin as an insulating material has become an urgent problem to be solved. Summary of the invention

[0005] In view of the defects in the prior art, the present invention proposes an epoxy resin composition and a composite material and preparation thereof, so as to solve the problem of how to improve the thermal conductivity and tensile strength of epoxy resin as an insulating material.

[0006] In order to solve the above technical problems, this application provides the following technical solutions:

[0007] In a first aspect, the present application provides an epoxy resin composition, comprising the following components in parts by weight: 30-50 parts of epoxy resin, 1-10 parts of modified boron nitride, 0.5-2 parts of curing agent, 0.1-1 parts of accelerator, and 0.2-0.8 parts of dispersant.

[0008] Preferably, the preparation method of the modified boron nitride is: mixing boron nitride nanosheets and dopamine, adding tris(hydroxymethyl)aminomethane to adjust the pH value to 8-9, and reacting to obtain the modified boron nitride.

[0009] Preferably, the curing agent includes one or more of methyltetrahydrophthalic anhydride and methylhexahydrophthalic anhydride, the accelerator includes one or more of 2-ethyl-4-methylimidazole and N,N-dimethylbenzylamine; the dispersant includes one or more of diethylene glycol, ethylene glycol ethyl ether and PE wax powder.

[0010] In a second aspect, the present application provides an epoxy resin composite material, which comprises an epoxy resin composition and an insulating fiber material.

[0011] In a third aspect, the present application provides a method for preparing an epoxy resin composite material, comprising the following steps:

[0012] S1. The epoxy resin, modified boron nitride, curing agent, accelerator, and dispersant are uniformly mixed in parts by mass to obtain a resin matrix;

[0013] S2. coating an adhesive on the insulating fiber material, and then impregnating it in the resin matrix to obtain a composite material precursor;

[0014] S3. Curing the composite material precursor by gradient heating to obtain the epoxy resin composite material.

[0015] Preferably, the insulating fiber includes one or more of glass fiber and aramid fiber.

[0016] Preferably, the adhesive comprises one or more of cellulose, polyvinyl butyral, and sodium silicate.

[0017] Preferably, the impregnation is vacuum impregnation, and the temperature of the vacuum impregnation is 20-50°C.

[0018] Preferably, the step of gradient temperature curing is pre-curing at a temperature of 60°C-80°C for 1-3 hours, and then curing at a temperature of 100°C-120°C for 4-10 hours.

[0019] In a fourth aspect, the present application provides an application of an epoxy resin composite material in the electronic and electrical fields.

[0020] In summary, compared with the prior art, the present invention achieves the following technical effects: the present application compounds modified boron nitride with epoxy resin, and the amount of modified boron nitride used is small, which greatly improves the heat dissipation effect of epoxy resin; by compounding with high tensile strength insulating fibers, the epoxy resin composition is impregnated into the insulating fibers, thereby enhancing the tensile properties of the composite material, and at the same time, the thermal conductive path constructed by the insulating fibers improves the heat transfer rate of the modified boron nitride, thereby improving the thermal conductivity of the epoxy resin composite material. DETAILED DESCRIPTION

[0021] In order to enable those skilled in the art to better understand the solutions of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below in combination with the solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work should fall within the scope of protection of the present invention.

[0022] The present application provides an epoxy resin composition, comprising the following components in parts by mass: 30-50 parts of epoxy resin, 1-10 parts of modified boron nitride, 0.5-2 parts of curing agent, 0.1-1 parts of accelerator, and 0.2-0.8 parts of dispersant.

[0023] In the present application, modified boron nitride is used as a thermal conductive filler and compounded with epoxy resin, and is evenly dispersed by a dispersant to improve the thermal conductivity of the epoxy resin.

[0024] In some embodiments, the modified boron nitride is prepared by mixing boron nitride nanosheets and dopamine, adding tris(hydroxymethyl)aminomethane to adjust the pH value to 8-9, and reacting to obtain the modified boron nitride.

[0025] In the present application, the modified boron nitride is a boron nitride nanosheet coated with polydopamine, which is beneficial to improving the compatibility of boron nitride with epoxy resin, making boron nitride less likely to agglomerate and improving thermal conductivity.

[0026] In some embodiments, the curing agent includes one or more of methyltetrahydrophthalic anhydride and methylhexahydrophthalic anhydride, the accelerator includes one or more of 2-ethyl-4-methylimidazole and N,N-dimethylbenzylamine; the dispersant includes one or more of diethylene glycol, ethylene glycol ethyl ether, and PE wax powder.

[0027] In the present application, the epoxy resin includes one or more of bisphenol A epoxy resin, hydrogenated bisphenol A epoxy resin, bisphenol S epoxy resin, bisphenol F epoxy resin, and novolac epoxy resin.

[0028] The present application provides an epoxy resin composite material, which comprises an epoxy resin composition and an insulating fiber material.

[0029] The present application provides a method for preparing an epoxy resin composite material, comprising the following steps:

[0030] S1. The epoxy resin, modified boron nitride, curing agent, accelerator, and dispersant are uniformly mixed in parts by mass to obtain a resin matrix;

[0031] S2. coating an adhesive on the insulating fiber material, and then impregnating it in the resin matrix to obtain a composite material precursor;

[0032] S3. Curing the composite material precursor by gradient heating to obtain the epoxy resin composite material.

[0033] The present application enhances the tensile properties of the composite material by compounding with insulating fibers with high tensile strength and impregnating the epoxy resin composition into the insulating fibers. At the same time, the thermal conductive path constructed by the insulating fibers increases the heat transfer rate of the modified boron nitride and improves the thermal conductivity of the epoxy resin composite material.

[0034] In some embodiments, the insulating fiber includes one or more of glass fiber and aramid fiber.

[0035] In some embodiments, the adhesive includes one or more of cellulose, polyvinyl butyral, and sodium silicate.

[0036] In some embodiments, the impregnation is vacuum impregnation, and the temperature of the vacuum impregnation is 20-50°C.

[0037] In some embodiments, the step of gradient temperature curing is pre-curing at a temperature of 60° C.-80° C. for 1-3 hours, and then curing at a temperature of 100° C.-120° C. for 4-10 hours.

[0038] The present application provides an application of an epoxy resin composite material in the field of electronics and electrical engineering.

[0039] The present solution is further described below through specific embodiments.

[0040] Example 1

[0041] An epoxy resin composition comprises the following components in parts by mass: 30 parts of bisphenol A epoxy resin, 1 part of modified boron nitride, 0.5 parts of methyltetrahydrophthalic anhydride, 0.1 parts of 2-ethyl-4-methylimidazole, and 0.2 parts of ethylene glycol ethyl ether.

[0042] Among them, the preparation method of modified boron nitride is: mix boron nitride nanosheets and dopamine, then add tris(hydroxymethyl)aminomethane to adjust the pH value to 8, and react at 30°C for 5 hours to obtain modified boron nitride. The mass ratio of boron nitride nanosheets, dopamine, and tris(hydroxymethyl)aminomethane is 100:50:10.

[0043] Example 2

[0044] An epoxy resin composition comprises the following components in parts by mass: 50 parts of bisphenol A epoxy resin, 10 parts of modified boron nitride, 2 parts of methyl hexahydrophthalic anhydride, 1 part of N,N-dimethylbenzylamine, and 0.8 parts of PE wax powder.

[0045] Among them, the preparation method of modified boron nitride is: mix boron nitride nanosheets and dopamine, then add tris(hydroxymethyl)aminomethane to adjust the pH value to 8, and react at 30°C for 5 hours to obtain modified boron nitride. The mass ratio of boron nitride nanosheets, dopamine, and tris(hydroxymethyl)aminomethane is 100:40:15.

[0046] Example 3

[0047] An epoxy resin composite material, the preparation steps of which include:

[0048] S1. 30 parts of bisphenol A epoxy resin, 1 part of modified boron nitride, 0.5 parts of methyltetrahydrophthalic anhydride, 0.1 parts of 2-ethyl-4-methylimidazole, and 0.2 parts of ethylene glycol ethyl ether were mixed uniformly by mass to obtain a resin matrix;

[0049] S2. Take 50 parts of glass fiber material, spray cellulose adhesive on its surface, and then impregnate it in a resin matrix under vacuum at 20°C to obtain a composite material precursor;

[0050] S3. Curing the composite material precursor by gradient temperature increase, wherein the steps of gradient temperature increase curing are: pre-curing at a temperature of 60°C for 1 hour, and then curing at a temperature of 120°C for 5 hours, to obtain the epoxy resin composite material.

[0051] Comparative Example 1

[0052] An epoxy resin composite material, other contents of which are the same as those of Example 3, except that modified boron nitride is not included.

[0053] Comparative Example 2

[0054] An epoxy resin composite material, the other contents are the same as those of Example 3, except that the modified boron nitride is replaced by unmodified boron nitride.

[0055] Comparative Example 3

[0056] An epoxy resin composite material, the other contents are the same as those of Example 3, except that no adhesive is used.

[0057] Comparative Example 4

[0058] An epoxy resin composite material, other contents are the same as those of Example 3, except that the glass fiber is replaced by graphite fiber.

[0059] Test and Evaluation

[0060] The epoxy resin composite materials obtained in the examples and comparative examples were tested, and the results are shown in Table 1. The test contents are as follows:

[0061] Thermal conductivity test: The thermal conductivity was tested using the German NETZSCH LFA467 laser flash thermal conductivity meter. According to the ASTM1461 standard, the sample thickness was 1mm±0.1mm.

[0062] Volume resistivity test: Tested in accordance with the standard of GB8815-2002.

[0063] Tensile strength test: Tested in accordance with GBT 2568-1995 standard.

[0064] Table 1 Test results of various composite materials

[0065]

[0066] The present application compounds modified boron nitride with epoxy resin, and the amount of modified boron nitride used is small, which greatly improves the heat dissipation effect of the epoxy resin; by compounding with insulating fibers with high tensile strength, the epoxy resin composition is impregnated into the insulating fibers, thereby enhancing the tensile properties of the composite material. At the same time, the thermal conductive path constructed by the insulating fibers improves the heat transfer rate of the modified boron nitride, thereby improving the thermal conductivity of the epoxy resin composite material.

[0067] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. An epoxy resin composition, characterized in that The invention comprises the following components in parts by weight: 30-50 parts of epoxy resin, 1-10 parts of modified boron nitride, 0.5-2 parts of curing agent, 0.1-1 parts of accelerator and 0.2-0.8 parts of dispersant.

2. The epoxy resin composition according to claim 1, characterized in that The preparation method of the modified boron nitride is: mixing boron nitride nanosheets and dopamine, adding tris(hydroxymethyl)aminomethane to adjust the pH value to 8-9, and reacting to obtain the modified boron nitride.

3. The epoxy resin composition according to claim 1, characterized in that The curing agent includes one or more of methyltetrahydrophthalic anhydride and methylhexahydrophthalic anhydride; the accelerator includes one or more of 2-ethyl-4-methylimidazole and N,N-dimethylbenzylamine; and the dispersant includes one or more of diethylene glycol, ethylene glycol ethyl ether and PE wax powder.

4. An epoxy resin composite material, characterized in that: The invention comprises the epoxy resin composition according to any one of claims 1 to 3 and an insulating fiber material.

5. A method for preparing the epoxy resin composite material according to claim 4, characterized in that: The following steps are involved: S1. The epoxy resin, modified boron nitride, curing agent, accelerator, and dispersant are uniformly mixed in parts by mass to obtain a resin matrix; S2. coating an adhesive on the insulating fiber material, and then impregnating it in the resin matrix to obtain a composite material precursor; S3. Curing the composite material precursor by gradient heating to obtain the epoxy resin composite material.

6. The method for preparing the epoxy resin composite material according to claim 5, characterized in that: The insulating fiber includes one or more of glass fiber and aramid fiber.

7. The method for preparing the epoxy resin composite material according to claim 5, characterized in that: The adhesive comprises one or more of cellulose, polyvinyl butyral ester and sodium silicate.

8. The method for preparing the epoxy resin composite material according to claim 5, characterized in that: The impregnation is vacuum impregnation, and the temperature of the vacuum impregnation is 20-50°C.

9. The method for preparing the epoxy resin composite material according to claim 5, characterized in that: The steps of gradient temperature curing are: pre-curing at a temperature of 60°C-80°C for 1-3 hours, and then curing at a temperature of 100°C-120°C for 4-10 hours.

10. Use of the epoxy resin composite material according to claim 4 in the field of electronics and electrical appliances.

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