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Phosphorus-nitrogen flame-retardant imidazole latent curing agent and preparation method thereof

A latent curing agent, phosphorus nitrogen flame retardant technology, applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc., can solve the problems of high curing activity, short storage period, etc. The effect of long storage period, easy availability of raw materials and high yield

Active Publication Date: 2018-03-20
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, ordinary imidazole curing agents have high curing activity at room temperature, and the one-component system composed of them and epoxy resin has a short shelf life.

Method used

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  • Phosphorus-nitrogen flame-retardant imidazole latent curing agent and preparation method thereof
  • Phosphorus-nitrogen flame-retardant imidazole latent curing agent and preparation method thereof
  • Phosphorus-nitrogen flame-retardant imidazole latent curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The preparation method of the adduct DOPO-TGIC of DOPO and TGIC, the specific steps are as follows:

[0042] 29.7g of triglycidyl isocyanurate (TGIC) was added to the reaction flask, and 21.6g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide ( DOPO) powder was added to the reaction bottle batch by batch; after the addition of DOPO, the reaction was continued at 140°C for 6h, and then cooled to obtain DOPO-TGIC powder, an adduct of intermediate product DOPO and TGIC.

Embodiment 2

[0044] Phosphorus nitrogen flame retardant imidazole latent curing agent, its molecular structure is as follows:

[0045] Among them, R 1 and R 2 Both are hydrogen.

[0046] The preparation method of the above-mentioned phosphorus-nitrogen flame-retardant imidazole latent curing agent: mix 13.6g of imidazole and N,N-dimethylformamide uniformly in a reaction bottle, and then mix 51.3g of Example 1 Add the prepared TGIC-DOPO powder into the reaction bottle batch by batch; after the addition, continue the reaction at 130°C for 5h; Class latent curing agent (code: A).

Embodiment 3

[0048] Phosphorus nitrogen flame retardant imidazole latent curing agent, its molecular structure is as follows:

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

[0050] The preparation method of the above-mentioned phosphorus-nitrogen flame-retardant imidazole latent curing agent: mix 16.4g of 2-methylimidazole and N,N-dimethylformamide in a reaction bottle, and then mix 51.3g of gTGIC-DOPO powder was added to the reaction flask batch by batch; after the addition, the reaction was continued at 145°C for 6 hours; after the reaction, N,N-dimethylformamide was removed by rotary evaporation to obtain the latent Curing agent (code: B).

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Abstract

The invention discloses a phosphorus-nitrogen flame-retardant imidazole latent curing agent, and the molecular structural formula of the curing agent is described shown in the description. A preparation method of the phosphorus-nitrogen flame-retardant imidazole latent curing agent comprises the step of enabling an active N-H bond in an imidazole compound, a P-H bond in 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and triglycidyl isocyanurate (TGIC), which are taken as raw materials, to be subjected to an addition reaction so as to obtain the phosphorus-nitrogen flame-retardant imidazole latent curing agent containing phosphaphenanthrene and a triazinetrione ring. The phosphorus-nitrogen flame-retardant imidazole latent curing agent has the characteristics of being good in flame-retardant effect, excellent in latent property and high in curing activity for epoxy resin.

Description

technical field [0001] The invention relates to a flame-retardant latent curing agent for epoxy resin and a preparation method thereof, which are used in an intrinsically flame-retardant one-component epoxy resin system. Background technique: [0002] Epoxy resin has the advantages of good mechanical properties, adhesive properties, chemical corrosion resistance, electrical properties, and dimensional stability, and is widely used in coatings, adhesives, laminates, and electronics industries. However, ordinary epoxy resin is a flammable material, and to expand its application range, it must be modified by flame retardancy. [0003] On the other hand, latent curing agent is a research hotspot in the field 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 mixing latent curing agent and epoxy resin has the advantages of simplifying the production operatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/50C07F9/6574
CPCC07F9/657172C08G59/5073C08G59/5086
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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