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Preparation method of heat-conducting liquid crystal epoxy resin

An epoxy resin and liquid crystal technology, applied in liquid crystal materials, chemical instruments and methods, etc., can solve the problems of low thermal conductivity, low thermal conductivity, and difficult curing process.

Pending Publication Date: 2022-07-29
ZHEJIANG YASHA DECORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The epoxy resin has low thermal conductivity
[0008] For the research on intrinsic thermal conductivity liquid crystal epoxy resin, there has not been an ideal epoxy resin with high intrinsic thermal conductivity in recent years, and most of the rigid rod-shaped epoxy monomers have high melting points, and the curing process must be melted at high temperature. Difficulty, high cost, low thermal conductivity, poor impact strength

Method used

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  • Preparation method of heat-conducting liquid crystal epoxy resin
  • Preparation method of heat-conducting liquid crystal epoxy resin
  • Preparation method of heat-conducting liquid crystal epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method of a thermally conductive liquid crystal epoxy resin, comprising the following steps;

[0027] (1) Dissolve 4-hydroxybiphenyl-4-carboxylic acid in ethanol, add potassium hydroxide to dissolve in distilled water, slowly add dropwise to the solution, heat to reflux and then add allyl bromide dropwise, keep at 80°C and reflux The reaction is carried out for 7h, electrophilic substitution reaction is carried out, and the phenolic hydroxyl group of 4-hydroxybiphenyl-4-carboxylic acid is alkylated. As the reaction proceeds, potassium bromide is gradually precipitated, and the molar concentration of the potassium hydroxide solution is 1.3 mol / L, the molar ratio of the 4-hydroxybiphenyl-4-carboxylic acid, allyl bromide, and potassium hydroxide solution is 1:1.1:2.6, after filtration, the ethanol is evaporated to obtain a reaction mixture, and distilled water is added. After that, the organic impurities are extracted with the extraction agent 1 (n-hexane) to...

Embodiment 2

[0037] A preparation method of a thermally conductive liquid crystal epoxy resin, comprising the following steps;

[0038] (1) Dissolve 4-hydroxybiphenyl-4-carboxylic acid in ethanol, add potassium hydroxide to dissolve in distilled water, slowly add dropwise to the solution, heat to reflux and then add allyl bromide dropwise, keep refluxing at 100°C Reaction 10h, potassium bromide is separated out, the mol ratio of described 4-hydroxybiphenyl-4-carboxylic acid, allyl bromide, potassium hydroxide solution is 1: 1.3: 3, after filtration, ethanol is evaporated to obtain reaction mixture , after adding distilled water, the organic impurities were extracted by extraction agent 1 (n-hexane) to obtain a premix, the aqueous phase was heated to 40 ° C, and a hydrochloric acid solution with a mass fraction of 20% was added dropwise to the premix, neutralization was carried out, and the crude product P1 was precipitated , utilize recrystallization method to purify to obtain P1, the stru...

Embodiment 3

[0046] A preparation method of a thermally conductive liquid crystal epoxy resin, comprising the following steps;

[0047] (1) Dissolve 4-hydroxybiphenyl-4-carboxylic acid in ethanol, add potassium hydroxide to dissolve in distilled water, slowly add dropwise to the solution, heat to reflux and then add allyl bromide dropwise, keep refluxing at 90°C The reaction is carried out for 8h, electrophilic substitution reaction is carried out, and the phenolic hydroxyl group of 4-hydroxybiphenyl-4-carboxylic acid is alkylated. As the reaction proceeds, potassium bromide is gradually precipitated, and the molar concentration of the potassium hydroxide solution is 1.4mol / L, the molar ratio of the 4-hydroxybiphenyl-4-carboxylic acid, allyl bromide, and potassium hydroxide solution is 1:1.2:2.8, after filtration, the ethanol is evaporated to obtain the reaction mixture, and the organic impurity to obtain a premix, the water phase is heated to 40 ℃, and the hydrochloric acid solution with ...

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Abstract

The invention provides a preparation method of heat-conducting liquid crystal epoxy resin, and belongs to the technical field of organic synthesis. The preparation method comprises the following steps: (1) mixing 4-hydroxybiphenyl-4-carboxylic acid, a potassium hydroxide solution and allyl bromide, and carrying out electrophilic substitution reaction to separate out P1; (2) mixing the P1 and thionyl chloride to obtain an intermediate product P2; (3) mixing 1, 4-butanediol and dichloromethane, dropwise adding the mixture into the P2, and performing suction filtration, water washing and drying to obtain an intermediate product P3; (4) mixing the intermediate product P3 with dichloromethane, cleaning with a mixed cleaning solution after the reaction is finished, and cleaning and recrystallizing a crude product with absolute ethyl alcohol to obtain a heat-conducting liquid crystal epoxy resin monomer; and (5) mixing the heat-conducting liquid crystal epoxy resin monomer and a curing agent, melting, carrying out vacuum defoaming, and curing to obtain the heat-conducting liquid crystal epoxy resin. The epoxy resin is high in heat conductivity, good in impact strength and low in curing and melting temperature in the preparation process.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of a thermally conductive liquid crystal epoxy resin. Background technique [0002] With the advent of the 5G era, electronic products are developing in the direction of miniaturization, densification and high power. The serious heat dissipation problem has become a bottleneck affecting the stability and reliability of electronic equipment, and the demand for efficient thermal management materials is gradually increasing. increase. [0003] Epoxy resin is a kind of high molecular polymer, the molecular formula is (C11H12O3)n, which refers to the general name of a class of polymers containing more than two epoxy groups in the molecule. It is the polycondensation product of epichlorohydrin and bisphenol A or polyol. Due to the chemical activity of the epoxy group, a variety of compounds containing active hydrogen can be used to open the r...

Claims

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Application Information

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IPC IPC(8): C08G59/24C09K19/38
CPCC08G59/245C09K19/3804
Inventor 丁欣欣王文广周东珊马俊丽彭伟
Owner ZHEJIANG YASHA DECORATION