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Preparation method of modified anhydride curing agent for extending applicability of epoxy resin system

A technology of epoxy resin system and acid anhydride curing agent, applied in the chemical industry, can solve the problems of short applicability of epoxy resin, and achieve the effect of solving short applicability and prolonging applicability

Inactive Publication Date: 2018-09-28
ZHEJIANG ALPHARM CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the deficiencies in the prior art, one of the purposes of the present invention is to provide a preparation method of a modified anhydride curing agent that extends the applicability of the epoxy resin system, which can solve the problem of short applicability of the epoxy resin

Method used

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  • Preparation method of modified anhydride curing agent for extending applicability of epoxy resin system
  • Preparation method of modified anhydride curing agent for extending applicability of epoxy resin system

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preparation example Construction

[0030] See figure 1 , A method for preparing a modified acid anhydride curing agent for extending the applicability of an epoxy resin system, comprising the following steps:

[0031] S101: Put 2-ethyl-4-methylimidazole and deionized water into the bottle, stir and raise the temperature to 20-50°C. Slowly add quantitative formaldehyde, rinse with deionized water after the addition;

[0032] S102: Raise the temperature to 60-90°C and keep it for 16-20 hours;

[0033] S103: Remove a small amount of supernatant liquid, and neutralize with dilute hydrochloric acid to a pH of 7-8;

[0034] S104: Extract with a small amount of ethyl acetate, and then put it in the refrigerator to cool to 3-8°C;

[0035] S105: Filter with Buchner funnel and wash with water, put the filter cake into a beaker, add water and stir for 20-50 minutes, filter with suction and wash with water;

[0036] S106: The filter cake is dried in a vacuum oven at 50-80°C to obtain a latent accelerator;

[0037] S107: Mix the acce...

Embodiment 1

[0041] Example 1: Put 2-ethyl-4-methylimidazole and deionized water into the bottle, stir and raise the temperature to 20-50°C. Slowly add quantitative formaldehyde, rinse with deionized water after dripping; the ratio of 2-ethyl-4-methylimidazole to deionized water is 590:33, the ratio of 2-ethyl-4-methylimidazole to formaldehyde Between 2 / 3 and 1 / 3.

[0042] Warm up to 70℃ for 16-20 hours; remove a small amount of supernatant, neutralize with dilute hydrochloric acid to a pH of 7-8; extract with a small amount of ethyl acetate, then put it in the refrigerator to cool to 5℃; use a Buchner funnel Filter with suction and wash with water, put the filter cake in a beaker, add water and stir for 30 minutes, filter and wash with water; the filter cake is dried in a vacuum oven at 60°C to obtain a latent accelerator; the accelerator and acid anhydride curing agent are evenly mixed.

Embodiment 2

[0043] Example 2: Put 2-ethyl-4-methylimidazole and deionized water into the bottle, stir and raise the temperature to 20-50°C. Slowly add quantitative formaldehyde, rinse with deionized water after dripping; the ratio of 2-ethyl-4-methylimidazole to deionized water is 590:33, the ratio of 2-ethyl-4-methylimidazole to formaldehyde 33:19.2.

[0044] Warm up to 70℃ for 16-20 hours; remove a small amount of supernatant, neutralize with dilute hydrochloric acid to a pH of 7-8; extract with a small amount of ethyl acetate, then put it in the refrigerator to cool to 5℃; use a Buchner funnel Filter with suction and wash with water, put the filter cake in a beaker, add water and stir for 30 minutes, filter and wash with water; the filter cake is dried in a vacuum oven at 60°C to obtain a latent accelerator; the accelerator and acid anhydride curing agent are evenly mixed.

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Abstract

The invention discloses a preparation method of a modified anhydride curing agent for extending applicability of an epoxy resin system. The preparation method comprises the following steps: adding 2-ethyl-4-methylimidazole and deionized water into a bottle, heating to 20-50 DEG C while stirring, dropwise adding a fixed amount of formaldehyde slowly, and rinsing by using deionized water after dropwise adding; heating to 60-90 DEG C, and preserving heat for 16-20 hours; removing a small amount of a supernatant, and neutralizing by using dilute hydrochloric acid till the pH is 7-8; extracting byusing a small amount of ethyl acetate, and then putting in a cold storage room to cool to 3-8 DEG C; performing suction filtration by using a Buchner funnel, washing by using water, putting a filter cake into a beaker, adding water, stirring for 20-50 minutes, performing suction filtration and washing by using water; drying the filter cake by using a 50-80 DEG C vacuum drying oven to obtain a latent accelerator; uniformly mixing the accelerator and an anhydride curing agent. The latent accelerator is used for modifying the anhydride curing agent in a form of a composite formula, so that the applicability of the epoxy resin system can be greatly extended and the problem of short applicability of epoxy resin is solved.

Description

Technical field [0001] The invention relates to the field of chemical engineering, and in particular to a method for preparing a modified acid anhydride curing agent that extends the applicability of an epoxy resin system. Background technique [0002] Epoxy resins and acid anhydride curing agents are used more and more widely in various industries, and their development potential is very large. Epoxy resin refers to a general term for a class of polymers containing more than two epoxy groups in the molecule. It is a polycondensation product of epichlorohydrin and bisphenol A or polyol. Due to the chemical activity of epoxy group, a variety of compounds containing active hydrogen can be used to open the ring, cure and crosslink to form a network structure, so it is a thermosetting resin. Bisphenol A epoxy resin is not only the largest in output and the most complete variety, but also new modified varieties are still increasing, and the quality is constantly improving. [0003] Ac...

Claims

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Application Information

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IPC IPC(8): C08G59/42C07D233/58
CPCC07D233/58C08G59/4238
Inventor 翁高翔张骏吴云鑫
Owner ZHEJIANG ALPHARM CHEM TECH
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