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3,3',5,5'-tetramethyl-4,4'-biphenyldiglycid ether preparation method

A technology of glycidyl ether and tetramethyl, which is applied in 3 fields, can solve the problems of cumbersome processing, achieve good solubility, reduce production cost, and improve reliability

Inactive Publication Date: 2006-02-15
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional method for preparing 3,3',5,5'-tetramethyl-4,4'-biphenyl diglycidyl ether is mainly prepared by one-step NaOH method, but in order to obtain a product with an epoxy equivalent close to the theoretical value, NaOH The addition method is strictly required, and the post-reaction treatment is cumbersome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take 10mL of isopropanol, 110g of epichlorohydrin, 14.52g of 3,3',5,5'-tetramethyl-4,4'-diphenol, 0.15g of tetrabutylammonium bromide, at 90°C Stir and react with nitrogen gas for 10 hours, add dropwise a solution containing 8g of sodium hydroxide with a concentration of 30%, and distill off excess epichlorohydrin at the same time under reduced pressure. Recrystallize twice with a mixed solution of methanol / acetone (2:1 volume ratio), after the activated carbon fades, dry it in vacuum at 70°C to obtain light yellow 3,3',5,5'-tetramethyl-4,4'-linked 24.84g of benzene diglycidyl ether. Yield: 86%, epoxy equivalent: 189 g / mol, melting point: 104-106°C.

Embodiment 2

[0016] Take isopropanol 10mL, epichlorohydrin 80g, 3,3',5,5'-tetramethyl-4,4'-diphenol 14.52g, benzyltriethylammonium chloride 0.65g, 90 Stir and react under nitrogen for 6 hours at ℃, add dropwise a solution containing 8g of sodium hydroxide with a concentration of 40%, and simultaneously remove excess epichlorohydrin under reduced pressure, continue stirring and reacting for 1 hour after the dropwise addition, rinse with cold water twice, and pump After filtering, use methanol / acetone (2:1 volume ratio) mixed solution to recrystallize twice, after the activated carbon fades, vacuum-dry at 70°C to obtain light yellow 3,3',5,5'-tetramethyl-4,4' - Biphenyl diglycidyl ether 23.11 g. Yield: 80%, epoxy equivalent: 198 g / mol, melting point: 102-104°C.

Embodiment 3

[0018] Take 12mL of ethanol, 198g of epichlorohydrin, 29.04g of 3,3',5,5'-tetramethyl-4,4'-biphenyldiol, 0.65g of tetrabutylammonium bromide, and pass nitrogen at 80°C Stir and react for 12 hours, add dropwise a solution containing 16g of sodium hydroxide with a concentration of 50%, and simultaneously remove excess epichlorohydrin under reduced pressure, continue to stir and react for 45 minutes after the dropwise addition, rinse twice with cold water, and use methanol / Acetone (2:1 volume ratio) mixed solution was recrystallized twice, and after the activated carbon faded, it was vacuum-dried at 70°C to obtain light yellow 3,3',5,5'-tetramethyl-4,4'-biphenyl Diglycidyl ether 50.84g. Yield: 88%, epoxy equivalent: 193 g / mol, melting point: 100-102°C.

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Abstract

The invention relates to a process for preparing 3,3',5,5'-tetramethyl-4,4'-biphenyl didycidyl ether, wherein the 3,3',5,5'-tetramethyl-4,4'-biphenol is reacted with excess epichlorohydrin under the action of phase transition catalyst. The prepared has low epoxy equivalent weight, high yield, and simple reaction steps.

Description

technical field [0001] The invention relates to a preparation method of 3,3',5,5'-tetramethyl-4,4-biphenyl diglycidyl ether. 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 molding compound 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 and high solder resistance. , high moisture resistance, high bonding strength, high glass transition temperature, low stress, low expansion, low viscos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/12
Inventor 任少平吕满庚凌有道郑一泉
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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