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A kind of liquid crystal epoxy resin and its preparation method and application

An epoxy resin and liquid crystal technology, applied in the direction of organic chemistry, can solve the problems of high curing process cost and high melting point, and achieve the effect of low curing cost, high curing temperature and high activity

Active Publication Date: 2017-01-25
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the rigid rod-shaped epoxy resin monomers have a high melting point, and the curing process must be completed under high-temperature melting, and the curing process cost is relatively high

Method used

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  • A kind of liquid crystal epoxy resin and its preparation method and application
  • A kind of liquid crystal epoxy resin and its preparation method and application
  • A kind of liquid crystal epoxy resin and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A preparation method of 3,5'-di-tert-butyl-5,3'-dimethyl biphenyl diglycidyl ether liquid crystal epoxy resin, comprising the following steps:

[0031] (1) Dissolve 32g of 3,5'-di-tert-butyl-5,3'-dimethylbiquinone shown in general formula (1) in 130g of epichlorohydrin and 80mL of In isopropanol, heat up to 70°C, add 0.96g tetrabutylammonium bromide, after the system is clear and transparent, slowly add (10min) 40g aqueous sodium hydroxide solution with a mass fraction of 30%, react for 3h, vacuumize and distill to remove Excess epichlorohydrin and isopropanol, the product was extracted with the organic solvent ethyl acetate, washed several times with water, dried with anhydrous sodium sulfate to remove water, filtered to obtain the filtrate, and the organic solvent ethyl acetate was removed by rotary evaporation, vacuum at 50°C Dry to obtain 3,5'-di-tert-butyl-5,3'-dimethylbiphenyl diglycidyl ether represented by formula (2), with a yield of 94%;

[0032] (2) Mix 5.27...

Embodiment 2

[0034] A preparation method of 3,5'-di-tert-butyl-5,3'-dimethyl biphenyl diglycidyl ether liquid crystal epoxy resin, comprising the following steps:

[0035] (1) Dissolve 32g of 3,5'-di-tert-butyl-5,3'-dimethylbiquinone shown in general formula (1) in 130g of epichlorohydrin and 80mL of In isopropanol, heat up to 80°C, add 1g of benzyltriethylammonium chloride, after the system is clear and transparent, slowly add (9min) 40g of 40% aqueous sodium hydroxide solution dropwise, react for 2h, vacuum distillation Remove excess epichlorohydrin and isopropanol, extract the product with organic solvent dichloromethane, wash with water several times, dry with desiccant anhydrous magnesium sulfate to remove water, filter to obtain filtrate, rotary evaporate to remove organic solvent dichloromethane, 50°C Vacuum drying to obtain 3,5'-di-tert-butyl-5,3'-dimethylbiphenyl diglycidyl ether represented by formula (2), with a yield of 92%;

[0036] (2) Mix 5.27g of 3,5'-di-tert-butyl-5,3'-di...

Embodiment 3

[0038] A preparation method of 3,5'-di-tert-butyl-5,3'-dimethyl biphenyl diglycidyl ether liquid crystal epoxy resin, comprising the following steps:

[0039] (1) Dissolve 32g of 3,5'-di-tert-butyl-5,3'-dimethylbiquinone shown in general formula (1) in 130g of epichlorohydrin and 80mL of In isopropanol, heat up to 70°C, add 0.96g tetrabutylammonium bromide, after the system is clear and transparent, slowly add (8min) 40g aqueous sodium hydroxide solution with a mass fraction of 30%, react for 3h, vacuumize and distill off Excess epichlorohydrin and isopropanol, the product was extracted with the organic solvent ethyl acetate, washed several times with water, dried with anhydrous sodium sulfate to remove water, filtered to obtain the filtrate, and the organic solvent ethyl acetate was removed by rotary evaporation, vacuum at 50°C Dry to obtain 3,5'-di-tert-butyl-5,3'-dimethylbiphenyl diglycidyl ether shown in formula (2);

[0040] (2) 5.27g of 3,5'-di-tert-butyl-5,3'-dimethylb...

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Abstract

The invention discloses liquid crystal epoxy resin as well as a preparation method and an application thereof. The preparation method comprises the following steps: reacting 3,5'-di-tert-butyl-5,3'-dimethyl biphenol with excessive epichlorohydrin in the presence of a phase transfer catalyst, thereby obtaining 3,5'-di-tert-butyl-5,3'-dimethyl diphenyl diglycidyl ether, wherein the softening point of 3,5'-di-tert-butyl-5,3'-dimethyl diphenyl diglycidyl ether is measured to be 10 DEG C through DSC, and the 3,5'-di-tert-butyl-5,3'-dimethyl diphenyl diglycidyl ether is a thick non-solid product at the room temperature; then, selecting a proper curing agent to pre-cure at a low temperature, enabling a biphenyl rid-rod-shaped structure to orientate and arrange with enough time, curing and cross-linking at a high temperature, thereby obtaining a liquid crystal structure. Compared with the conventional preparation method for the rigid-rod-shaped epoxy resin, the preparation method disclosed by the invention is low in curing cost.

Description

technical field [0001] The invention belongs to the technical field of chemical product preparation, and in particular relates to a liquid crystal epoxy resin and a preparation method and application thereof. Background technique [0002] Electronic materials are the basis for the development of the microelectronics industry. As the main structural material for the production of integrated circuits—epoxy molding compound is developing rapidly with the development of chip technology, and the development of packaging material technology will greatly promote the development of the microelectronics industry. At present, integrated circuits are developing towards high integration, miniaturization of wiring, large-scale chips and surface mount technology. The corresponding research and development trend of plastic packaging materials is to make materials with high purity, high reliability, high thermal conductivity, high solder resistance, High glass transition temperature, low ex...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/24C08G59/50C07D303/30C07D301/26
Inventor 吕满庚郭会龙
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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