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DOPO type curing agent for epoxy resin system and application of DOPO type curing agent

An epoxy resin system, epoxy resin technology, applied in DOPO type compound D-DICY and its application field in epoxy resin system, can solve the problem of lack of flame retardant performance, and achieve the effect of good compatibility

Inactive Publication Date: 2018-11-30
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Epoxy resin is a flammable substance, and the limiting oxygen index (LOI) of untreated epoxy resin is only 19.8%. Therefore, it is necessary to improve its flame retardancy in many applications, but currently the existing curing agents generally do not have flame retardancy. Flammability

Method used

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  • DOPO type curing agent for epoxy resin system and application of DOPO type curing agent
  • DOPO type curing agent for epoxy resin system and application of DOPO type curing agent
  • DOPO type curing agent for epoxy resin system and application of DOPO type curing agent

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Experimental program
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Effect test

preparation example Construction

[0032] The synthetic method of compound D-DICY, concrete steps are as follows:

[0033] Under an inert atmosphere, add an appropriate amount of DOPO into the reaction flask and heat until the DOPO is completely melted, then add an appropriate amount of dicyandiamide into the reaction flask to form a mixture, and the reaction temperature is higher than 110 ° C to ensure that the mixture is in a molten state, and then The temperature was raised to 175°C, and the reaction was carried out for 6-12 hours. The reaction product was washed and filtered with tetrahydrofuran to remove unreacted DOPO, then washed with hot deionized water and dried in a vacuum oven to obtain the final product.

[0034] The H NMR spectrum of the product is attached figure 2 shown. From the analysis in Table 1, it can be confirmed that the obtained product is D-DICY.

[0035] Table 1

[0036]

Embodiment 1

[0038] The application method of novel compound D-DICY in epoxy resin, its specific steps are as follows:

[0039] 1. Select epoxy resin CYD127, mix it with 10wt% compound D-DICY, 1wt% DMP-30 or imidazole (all in terms of epoxy resin mass, the same below) and filler;

[0040] 2. Pour the above mixed solution into a self-made silicone mold, heat it to 100°C for 1 hour to pre-cure, and make it into shape;

[0041] 3. Heat the mixture to 115°C for 4 hours, so that the curing agent can fully cure the epoxy resin, and then continue to heat up to 135°C and cure for 2 hours, so as to eliminate internal stress and improve the bonding strength and the comprehensive performance of the epoxy resin cured product.

[0042] Mechanism of Curing Epoxy Resin Using D-DICY See figure 1 . Under appropriate conditions, the primary amino group on D-DICY first reacts with the epoxy group, the epoxy group ring-opens and reacts to form a hydroxyl group, the primary amine loses an active H to form a ...

Embodiment 2

[0044] 1. Select epoxy resin E51, mix it with 15wt% compound D-DICY, 3wt% DMP-30 or imidazole and filler;

[0045] 2. Pour the above mixture into a self-made silicone mold, heat to 100°C for 2 hours to pre-cure, and make it into shape; heat up to 115°C for 4 hours, and continue to heat up to 135°C for 2 hours.

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Abstract

The present invention discloses an application method of a novel compound D-DICY as a curing agent and a flame retardant in an epoxy resin system. The method is specifically as follows: the D-DICY ismixed with epoxy resin; an accelerator and a filling material are added; the materials are stirred to be mixed evenly; the mixture is heated to 100 DEG C for pre-curing for 1-2 h for shaping; the shaped mixture is continuously heated to 115 DEG C for curing for 4-6 h to enable the curing agent fully cures the epoxy resin; finally the mixture is heated to 135 DEG C to continue the curing for 2 h tocomplete the curing; and finally a cross-linked net-shaped cured product is formed. The novel compound has relatively good compatibility with the epoxy resin, can cure the epoxy resin and can be usedfor flame retarding of the epoxy resin, and is also halogen-free, low-smoke and low-toxic, and in line with the requirement of a novel, green and environmentally-friendly curing agent.

Description

technical field [0001] The invention relates to the technical field of epoxy resin materials, in particular to DOPO compound D-DICY and its application in epoxy resin systems. Background technique [0002] As an important class of thermosetting polymer materials, epoxy resin has the advantages of high specific strength and specific stiffness, good corrosion resistance, stable structure and size, good insulation and strong adhesion, and is widely used in adhesives, coatings, etc. , emerging composite materials in the aviation and electronics industries. [0003] Epoxy resin is a flammable substance, and the limiting oxygen index (LOI) of untreated epoxy resin is only 19.8%. Therefore, it is necessary to improve its flame retardancy in many applications, but currently the existing curing agents generally do not have flame retardancy. flammability. . Therefore, there is an urgent need for the application of a new type of curing agent and flame retardant in epoxy resin system...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/50C08K5/5313
CPCC08G59/504C08G59/5046C08K5/5313
Inventor 彭永利张灿万春杰熊丽君
Owner WUHAN INSTITUTE OF TECHNOLOGY