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

A technology of epoxy resin and biphenyl, which is applied in the direction of liquid crystal materials, chemical instruments and methods, organic chemistry, etc., can solve the problems of high melting point, high cost, and difficult curing process, so as to improve thermal conductivity, reduce scattering, and cure The effect of low difficulty

Active Publication Date: 2020-10-16
中科广化(重庆)新材料研究院有限公司 +3
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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, which makes the curing process difficult and expensive

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048]A preparation method of 4,4'-bis(5,6-epoxyhexyloxy) biphenyl liquid crystal epoxy resin, comprising the following steps:

[0049] (1) Dissolve 18.6g of biphenol shown in formula I in 350-500mL of acetone under the protection of nitrogen, raise the temperature to 60°C, add 34.5g of anhydrous potassium carbonate powder, and stir for half an hour to one hour , Add 40.75g of 6-bromo-1-hexene in batches, and react for 24h. Potassium carbonate was removed by filtration, the filtrate was vacuum-distilled to remove acetone, washed several times with absolute ethanol, filtered to obtain white flaky crystals, and dried in vacuum at 50°C to obtain 4,4'-bis(5-hexenyloxy) as shown in II. Base) biphenyl, productive rate 84%;

[0050] (2) Dissolve 14g of 4,4'-bis(5-hexenyloxy)biphenyl prepared in step (1) in 150-200mL of dichloromethane, raise the temperature to 40°C, and add 17.2g of m-chloro Peroxybenzoic acid, reacted for 1 week, filtered to remove the precipitated m-chlorobenzoic...

Embodiment 2

[0053] A preparation method of 4,4'-bis(5,6-epoxyhexyloxy) biphenyl liquid crystal epoxy resin, comprising the following steps:

[0054] (1) Dissolve 18.6g of biphenol shown in formula I in 350-500mL of acetone under the protection of nitrogen, raise the temperature to 60°C, add 34.5g of anhydrous potassium carbonate powder, and stir for half an hour to one hour , Add 40.75g of 6-bromo-1-hexene in batches, and react for 24h. Potassium carbonate was removed by filtration, the filtrate was vacuum-distilled to remove acetone, washed several times with absolute ethanol, filtered to obtain white flaky crystals, and dried in vacuum at 50°C to obtain 4,4'-bis(5-hexenyloxy) as shown in II. Base) biphenyl, productive rate 84%;

[0055] (2) Dissolve 14g of 4,4'-bis(5-hexenyloxy)biphenyl prepared in step (1) in 150-200mL of dichloromethane, raise the temperature to 40°C, and add 17.2g of m-chloro Peroxybenzoic acid, reacted for 1 week, filtered to remove the precipitated m-chlorobenzoi...

Embodiment 3

[0058] A preparation method of 4,4'-bis(5,6-epoxyhexyloxy) biphenyl liquid crystal epoxy resin, comprising the following steps:

[0059] (1) Dissolve 18.6g of biphenol shown in formula I in 350-500mL of acetone under the protection of nitrogen, raise the temperature to 60°C, add 34.5g of anhydrous potassium carbonate powder, and stir for half an hour to one hour , Added 35.86g of 6-bromo-1-hexene in batches, and reacted for 24h. Potassium carbonate was removed by filtration, the filtrate was vacuum-distilled to remove acetone, washed several times with absolute ethanol, filtered to obtain white flaky crystals, and dried in vacuum at 50°C to obtain 4,4'-bis(5-hexenyloxy) as shown in II. Base) biphenyl, productive rate 80%;

[0060] (2) Dissolve 14g of 4,4'-bis(5-hexenyloxy)biphenyl prepared in step (1) in 150-200mL of dichloromethane, raise the temperature to 40°C, and add 15.14g of m-chloro Peroxybenzoic acid, reacted for 1 week, filtered to remove the precipitated m-chlorob...

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Abstract

The invention discloses diphenyl liquid-crystal epoxy resin as well as a preparation method and application thereof. The preparation method of the diphenyl liquid-crystal epoxy resin comprises the following steps of: (1) dissolving diphenyl diphenol in acetone, rising the temperature to 60-80 DEG C, adding potassium carbonate, stirring with 6-bromo-1-hexene for reaction, and obtaining 4,4'-di(5-hexenyloxo)diphenyl; (2) dissolving the 4,4'-di(5-hexenyloxo)diphenyl in dichloromethane, then rising the temperature to 40-50 DEG C, adding peroxide for reaction, and obtaining 4,4'-di(5,6-epoxyhexyloxy)diphenyl; (3) dissolving the 4,4'-di(5,6-epoxyhexyloxy)diphenyl and a curing agent in an organic solvent to obtain mixed liquid; then vacuumizing the mixed liquid till to be constant weight, and after the solvent is volatilized, carrying out sectional curing to obtain the diphenyl liquid-crystal epoxy resin. The diphenyl liquid-crystal epoxy resin, the preparation method and the application disclosed by the invention have the beneficial effects that the curing difficulty is low, the curing cost is low, and the obtained diphenyl liquid-crystal epoxy resin is good in heat-conducting property.

Description

technical field [0001] The invention belongs to the technical field of chemical product preparation, and in particular relates to a biphenyl 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 temperatur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D301/14C07D303/30C09K19/34C08G59/24C08G59/50
CPCC07D301/14C07D303/30C08G59/245C08G59/5006C08G59/5033C08G59/504C09K19/3411
Inventor 吕满庚张倩陈国康张世恒吴昆
Owner 中科广化(重庆)新材料研究院有限公司
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