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Preparation method of non-isocyanate polyurea epoxy curing agent

An epoxy curing agent, non-isocyanate technology, used in the preparation of non-isocyanate urea-based epoxy curing agents, can solve the problems of fast curing speed, poor heat resistance, brittle performance, etc. The effect of improving heat resistance, strength and heat resistance

Inactive Publication Date: 2019-03-29
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to solve the problems of traditional epoxy curing agents such as too fast or too slow curing speed, poor heat resistance after curing, brittle performance, and high toxicity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Weigh 20 parts of 1,6-hexamethylenediamine, 62 parts of dimethyl carbonate, 0.05 parts of sodium methoxide, 5 parts of methanol and 138 parts of amino-terminated polyether D400 according to the mass fraction, react at normal pressure 70 °C for 3 hours, and then increase When the temperature reaches 88°C, the methanol produced by the reaction is rectified. The temperature at the top of the rectification column is 63°C. After 5 hours, the rectified product reaches the theoretical amount. At this time, the remaining dimethyl carbonate is removed under a vacuum of -0.07MPa, and then Add amino-terminated polyether D400 to condense, and remove methanol at a reaction temperature of 120°C and a vacuum of -0.097MPa. After 2 hours, the methanol reaches the theoretical value and stops the reaction to obtain a light yellow viscous liquid non-isocyanate urea-based epoxy curing agent. By detection, the yield of the product was 90%, and the number average molecular weight was measured ...

Embodiment 2

[0045]Weigh 13 parts of 1,4-butylene diamine, 80 parts of dimethyl carbonate, 0.2 parts of sodium methoxide, 10 parts of methanol and 68 parts of amino-terminated polyether D230 according to the mass fraction, react at normal pressure 70 ° C for 3 hours, and then increase When the temperature reaches 88°C, the methanol produced by the reaction is rectified. The temperature at the top of the rectification column is 63°C. After 5 hours, the rectified product reaches the theoretical amount. At this time, the remaining dimethyl carbonate is removed under a vacuum of -0.07MPa, and then Add amino-terminated polyether D400 to condense, and remove methanol at a reaction temperature of 120°C and a vacuum of -0.097MPa. After 2 hours, the methanol reaches the theoretical value and stops the reaction to obtain a light yellow viscous liquid non-isocyanate urea-based epoxy curing agent. By detection, the yield of the product was 95%, and the number average molecular weight was 850.

Embodiment 3

[0047] Weigh 32 parts of 1,6 hexamethylenediamine, 148 parts of dimethyl carbonate, 0.5 parts of sodium methoxide, 20 parts of methanol and 128 parts of amino-terminated polyether D230 according to the mass fraction, react at normal pressure 70 ° C for 3 hours, and then increase When the temperature reaches 88°C, the methanol produced by the reaction is rectified. The temperature at the top of the rectification column is 63°C. After 5 hours, the rectified product reaches the theoretical amount. At this time, the remaining dimethyl carbonate is removed under a vacuum of -0.07MPa, and then Add amino-terminated polyether D400 to condense, and remove methanol at a reaction temperature of 120°C and a vacuum of -0.097MPa. After 2 hours, the methanol reaches the theoretical value and stops the reaction to obtain a light yellow viscous liquid non-isocyanate urea-based epoxy curing agent. By detection, the yield of the product was 96%, and the number average molecular weight was 930.

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Abstract

The invention provides a preparation method of a non-isocyanate polyurea epoxy curing agent. The method includes: 1) according to mass percentages, weighing a diamine compound, dialkyl carbonate and acatalyst A, performing a reaction under normal pressure, and removing residual dialkyl carbonate; 2) under effect of a catalyst B, condensing the alkyl methyl dicarbamate and amino-terminated polyether, and after alkyl alcohol reaches theoretical value, stopping the reaction to prepare the non-isocyanate polyurea epoxy curing agent, which is a slightly yellow thick liquid. By adding the polyetherflexible chain segments and urea bonds, the epoxy curing agent is improved in toughness, strength and heat resistance. Compared with conventional epoxy curing agents, the epoxy curing agent is prepared from low-toxic or toxic-free raw materials and is a toxic-free product, is harmless to human body and is green and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of a non-isocyanate urea-based epoxy curing agent. Background technique [0002] Epoxy resin contains a variety of polar groups and highly active epoxy groups, so it has strong adhesion to metals, glass, cement, wood, plastics and other polar materials, especially materials with high surface activity At the same time, the cohesive strength of the epoxy cured product is also very large, so its bonding strength is very high. Basically no low molecular volatiles are produced when the epoxy resin is cured. Good corrosion resistance and dielectric properties. After curing, epoxy resin can resist the corrosion of acid, alkali, salt, solvent and other media. [0003] Although epoxy resin has the above-mentioned characteristics, pure epoxy resin itself does not have these performance characteristics, and its performance advantages can only be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48C08G65/333C08G59/50
CPCC08G59/5006C08G65/33344C08G65/48C08G2650/50
Inventor 赵本波程原刘文俊李治韬邓平
Owner ZHONGBEI UNIV