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Flame-retardant imidazole latent curing agent and preparation method thereof

A latent curing agent, imidazole technology, applied in the field of epoxy resin latent curing agent, can solve the problem of not considering the group with flame retardant effect, can not be used to prepare flame retardant epoxy resin, etc. Curing activity, long shelf life effect

Active Publication Date: 2019-07-23
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the previous modification methods did not consider the introduction of groups with flame-retardant effects into the molecular structure of imidazole compounds, which cannot be used to prepare intrinsically flame-retardant epoxy resins.

Method used

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  • Flame-retardant imidazole latent curing agent and preparation method thereof
  • Flame-retardant imidazole latent curing agent and preparation method thereof
  • Flame-retardant imidazole latent curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A flame-retardant imidazole latent curing agent, its molecular structure is as follows:

[0035] Among them, R 1 and R 2 Both are hydrogen.

[0036] The preparation method of above-mentioned flame-retardant type imidazole latent curing agent comprises the following steps:

[0037] 1) Mix 18.45g of cyanuric chloride, 30.3g of triethylamine and 250ml of tetrahydrofuran in a three-necked flask evenly, and continuously feed nitrogen; dissolve 6.8g of imidazole in 50ml of tetrahydrofuran, at 25°C, nitrogen, stirring conditions , drop the imidazole / tetrahydrofuran solution into the above-mentioned three-necked flask through a constant pressure dropping funnel;

[0038] 2) After the imidazole / tetrahydrofuran solution was added dropwise, the reaction was stirred at 70°C for 1h; then the temperature was lowered to 25°C, and 43.2g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene was mixed under nitrogen and stirring conditions -10-oxide (DOPO) powder is added to the reaction so...

Embodiment 2

[0041] A flame-retardant imidazole latent curing agent, its molecular structure is as follows:

[0042] Among them, R 1 for methyl and R 2 for hydrogen.

[0043] The preparation method of above-mentioned flame-retardant type imidazole latent curing agent comprises the following steps:

[0044] 1) Mix 18.45g of cyanuric chloride, 30.3g of triethylamine and 250ml of tetrahydrofuran in a three-necked flask, and continuously feed nitrogen; dissolve 8.2g of 2-methylimidazole in 50ml of tetrahydrofuran, and heat the Under stirring conditions, add the 2-methylimidazole / tetrahydrofuran solution dropwise into the above-mentioned three-necked flask through a constant pressure dropping funnel;

[0045] 2) After the addition of 2-methylimidazole / tetrahydrofuran solution was completed, the reaction was stirred at 70°C for 1 hour; then the temperature was lowered to 25°C, and 43.2g of 9,10-dihydro-9-oxa-10 - Phosphaphenanthrene-10-oxide (DOPO) powder is added to the reaction solution ...

Embodiment 3

[0048] A kind of flame-retardant imidazole latent curing agent, its molecular structure formula is as follows:

[0049] Among them, R 1 for ethyl and R 2 for hydrogen.

[0050] The preparation method of above-mentioned flame-retardant type imidazole latent curing agent comprises the following steps:

[0051] 1) Mix 18.45g of cyanuric chloride, 30.3g of triethylamine and 250ml of tetrahydrofuran in a three-necked flask evenly, and continuously feed nitrogen; dissolve 9.6g of 2-ethylimidazole in 50ml of tetrahydrofuran, at 40°C, nitrogen, Under the condition of stirring, add the 2-ethylimidazole / tetrahydrofuran solution dropwise into the bottle through the constant pressure dropping funnel;

[0052] 2) After the addition of 2-ethylimidazole / tetrahydrofuran solution was completed, the reaction was stirred at 75°C for 1h; then the temperature was lowered to 35°C, and 43.2g of 9,10-dihydro-9-oxa-10 - Phosphaphenanthrene-10-oxide (DOPO) powder is added to the reaction solution b...

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Abstract

The invention discloses a flame-retardant imidazole latent curing agent. The structure formula of the flame-retardant imidazole latent curing agent is as shown in the specification. According to the flame-retardant imidazole latent curing agent, imidazole group with curing activity and triazine ring and phosphaphenanthrene group which have good flame-retardant effect are constructed in one molecule by substituting reaction, so that the prepared novel curing agent is high in curing activity for epoxy resin, high in latent performance and good in flame-retardant effect.

Description

technical field [0001] The invention belongs to the technical field of latent curing agents for epoxy resins, in particular to flame-retardant imidazole latent curing agents. Background technique [0002] Epoxy resins have excellent comprehensive properties and are widely used in electronics, construction, aerospace and other fields. However, ordinary epoxy resin is a flammable material, which limits its application range. In recent years, epoxy resin latent curing agent is the research focus of epoxy resin curing agent at home and abroad. Compared with the two-component epoxy resin system commonly used at present, the one-component epoxy resin system prepared by latent curing agent and epoxy resin has the advantages of simplifying the production operation process, reducing environmental pollution, improving product quality, and adapting to Large-scale industrial production and other advantages. The imidazole curing agent can initiate anionic chain polymerization of epoxy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/50C07F9/6574
CPCC07F9/657172C08G59/5086
Inventor 杨爽胡业发章桥新周祖德丁国平王钧
Owner WUHAN UNIV OF TECH
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