Process for preparing glycidic amine type polyfunctional epoxy resin

A technology of glycidyl amine type and epoxy resin, which is applied in chemical recycling, organic chemistry, etc., can solve the problems of unseen preparation methods, and achieve the effects of low cost, low production cost, and less three wastes

Inactive Publication Date: 2007-01-24
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] N, N, N', N'-tetraglycidyl-4,4'-methylenedi-o-toluidine (TGMDT) has not yet seen a disclosed preparation method

Method used

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  • Process for preparing glycidic amine type polyfunctional epoxy resin
  • Process for preparing glycidic amine type polyfunctional epoxy resin
  • Process for preparing glycidic amine type polyfunctional epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 21.6 grams (0.1 moles) of 4,4'-methylene di-o-toluidine (MDT), 37 grams (0.4 moles) of epichlorohydrin (ECH), 10.8 grams of water and 22 milliliters of ethanol were added in a three-necked flask, and the After stirring and reacting for 7 hours at ℃, raise the reaction temperature, react at 80℃ for 2 hours, then raise the reaction temperature, and react at 90℃ for 1 hour, cool the reaction solution to 60℃, add dropwise 80 grams (0.4 moles) of 20% Concentrated sodium hydroxide aqueous solution, after dripping within 2 hours, continue to react at 80°C for 6 hours. Add 800 milliliters of toluene, stir to dissolve, filter to remove sodium chloride, wash the mother liquor with water, let stand, separate liquids, remove the water phase, and leave the organic phase mother liquor. The mother liquor is devolatilized in vacuum, and the volatile matter is collected for reuse in the next cycle; the residue after devolatilization is an amber viscous substance, which is N, N, N', N'-t...

Embodiment 2

[0028] 21.6 grams (0.1 moles) of 4,4'-methylene di-o-toluidine (MDT), 185 grams (2.0 moles) of epichlorohydrin (ECH), 2.16 grams of water and 38 milliliters of ethanol were added in a three-necked flask, at 40 After 4 hours of stirring reaction at ℃, raise the reaction temperature, react at 80℃ for 3 hours, then raise the reaction temperature, and react at 90℃ for 10 minutes, cool the reaction solution to 60℃, add dropwise 320 grams (1.6 moles) of 20% Concentrated sodium hydroxide aqueous solution, after dripping within 2 hours, continue to react at 80°C for 3 hours. Cool, stand still, separate liquid, remove sodium chloride solid and water, and obtain epichlorohydrin layer and resin layer. Recover epichlorohydrin for next recycling; put the resin layer into a three-necked flask, add 800 milliliters of toluene to the resin, stir to dissolve, wash the mother liquor with water, let stand, separate liquids, remove the water phase, and keep the organic phase mother liquor. The mo...

Embodiment 3

[0030] Except adding 92.5 grams (1.0 mole) of epichlorohydrin (ECH), 100 grams of 20% aqueous sodium hydroxide solution, other process steps, material quantities and reaction parameters are all the same as in Example 2. As a result, N, N, N', N'-tetraglycidyl-4,4'-methylenedi-o-toluidine (TGMDT) was obtained, which was measured by the amount of 4,4'-methylenedi-o-toluidine The yield is 98%, the epoxy value is 0.701, and the volatile matter is 0.94%.

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Abstract

The process of preparing glycidic amine type polyfunctional epoxy resin includes the following steps: 1. reaction between 4, 4'-methylene di-o-methylaniline and chloroepoxy propane in the molar ratio of 1 to 4-20 in water-alcohol solvent at 40-90 deg.c for 3-10 hr; and 2. dropping water solution of alkali metal hydroxide in the concentration of 20 % at 60 deg.c to produce desalting ring-closing reaction at 60-80 deg.c, extracting with extractant, water washing, separating, and vacuum volatizing to obtain N, N, N', N'-tetraglycidyl-4, 4'-methylene di-o-methylaniline. The present invention is one industrial process with simple operation, low cost, high product quality, high yield and less three wastes.

Description

technical field [0001] The present invention relates to a kind of preparation method of glycidyl amine type polyfunctional epoxy resin, especially relate to a kind of N,N,N',N'-tetraglycidyl-4,4'-methylenedi-o-toluidine Preparation. Background technique [0002] Glycidylamine type multifunctional epoxy resin is an important raw material for preparing high temperature resistant adhesives, fiber reinforced prepregs, packaging materials for electronic components, high temperature resistant electrical insulating varnishes and coatings. [0003] The molecular structure of glycidylamine type multifunctional epoxy resin contains multiple epoxy groups, which can chemically react with various active groups such as amino groups, hydroxyl groups, and carboxyl groups. Therefore, it can react with compounds containing the above active groups or The polymer undergoes a copolymerization reaction to cure and crosslink. [0004] Multi-functional epoxy resin, such as CIBA-GEIGY's MY720, has...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/32C07D305/10
CPCY02P20/582
Inventor 虞鑫海刘万章胡彬徐永芬赵炯心
Owner DONGHUA UNIV
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