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Reactive type flame-retardant epoxy resin curing agent and preparation method thereof

An epoxy resin curing and reactive flame retardant technology is applied in the field of flame retardants to achieve the effects of reduced impact, good application prospect and simple preparation method

Inactive Publication Date: 2017-11-28
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, they all react with equimolar functional groups, rather than equimolar functional groups, which have not been reported in epoxy resins.

Method used

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  • Reactive type flame-retardant epoxy resin curing agent and preparation method thereof
  • Reactive type flame-retardant epoxy resin curing agent and preparation method thereof
  • Reactive type flame-retardant epoxy resin curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) To a place equipped with a thermometer, condensing reflux, magnetic stirring, dropping funnel and N 2 Add 20mL deionized water and 0.01mol p-phenylenediamine into the 250ml four-necked flask, stir and heat to 95°C to make it completely dissolved, then add 0.05mol terephthalaldehyde dropwise to the flask, under N 2 The reaction was carried out under protective atmosphere for 4h.

[0025] (2) After the reaction is finished, the reaction mixture is placed in a refrigerator for low temperature cooling, and the crude product is obtained by suction filtration. It was dissolved in deionized water and heated, then cooled and recrystallized by the same method, repeated three times, and finally dried in a vacuum oven at 80° C. for 24 hours to obtain an intermediate product.

[0026] (3) to a thermometer, condensing reflux, magnetic stirring and N 2 Add 0.02mol DOPO, 0.01mol intermediate product and 10mL DMF into the 250ml three-necked flask that was passed through, and grad...

Embodiment 2

[0030] (1) To a place equipped with a thermometer, condensing reflux, magnetic stirring, dropping funnel and N 2 Add 20mL deionized water and 0.01mol p-phenylenediamine into the 250ml four-neck flask that was passed through, stir and heat to 95°C and make it completely dissolve, then add 0.07mol terephthalaldehyde dropwise to the flask, and in N 2 The reaction was carried out for 4 h under a protective atmosphere, and the intermediate product was obtained by separation and purification.

[0031] (2) to a thermometer, condensing reflux, magnetic stirring and N 2 Add 0.024mol DOPO, 0.01mol intermediate product and 10mL DMF into the 250ml three-neck flask that was passed through, and gradually raise the temperature to dissolve completely. 2 React for 6 hours under protective atmosphere, and obtain a new type of reactive flame-retardant epoxy resin curing agent after separation and purification.

Embodiment 3

[0033] (1) To a place equipped with a thermometer, condensing reflux, magnetic stirring, dropping funnel and N 2 Add 20mL deionized water and 0.01mol p-phenylenediamine into the 250ml four-neck flask that was passed through, stir and heat to 95°C and make it completely dissolve, then add 0.07mol terephthalaldehyde dropwise to the flask, and in N 2 The reaction was carried out for 6 hours under a protective atmosphere, and the intermediate product was obtained by separation and purification.

[0034] (2) to a thermometer, condensing reflux, magnetic stirring and N 2 Add 0.024mol DOPO, 0.01mol intermediate product and 10mL DMF into the 250ml three-necked flask, gradually raise the temperature to make it completely dissolved, at 140℃, N 2 React for 6 hours under protective atmosphere, and obtain a new type of reactive flame-retardant epoxy resin curing agent after separation and purification.

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Abstract

The invention discloses a reactive type flame-retardant epoxy resin curing agent and a preparation method thereof. The curing agent is prepared by enabling p-phenylenediamine and terephthalaldehyde to react to generate an intermediate product and by further enabling the intermediate product to react with DOPO. The curing agent has two active amino groups and two imino groups, can be used for curing epoxy resins, has flame-retardant elements P and N, and has a function of synergic flame retardancy. The curing agent has the advantages that raw materials are easy to obtain, a preparation process is simple, separation and purification are easily implemented and the like, and is convenient in large-scale popularization and application.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a reactive flame retardant epoxy resin curing agent and a preparation method thereof. Background technique [0002] In recent years, with the continuous improvement of people's environmental protection and safety awareness, the flame retardant of epoxy resin materials has also been developing in a green direction. Nitrogen, phosphorus and silicon compounds are environmentally friendly flame retardant materials, almost no toxic substances are produced during their combustion, and their flame retardant performance is no less than that of halogen-containing flame retardants, and when the compound contains two or more retardants When combustible elements are used, the flame retardant effect will be greatly improved. [0003] Although the synthesis of aldimines and polymethylimines has been reported for a long time, the flame retardancy of epoxy resins has only recently prog...

Claims

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Application Information

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IPC IPC(8): C08G59/50C07F9/6574C07F9/6571
CPCC08G59/5046C07F9/657172C08G59/504
Inventor 彭永利张满倪思瑶熊丽君万春杰
Owner WUHAN INSTITUTE OF TECHNOLOGY
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