Heat-resistant flame-retardant epoxy resin latent curing agent

A latent curing agent, epoxy resin technology, applied in latent curing agent and its preparation, triazine heterocyclic modified imidazole type epoxy resin latent curing agent and its preparation field, can solve short storage period, durability Low heat resistance, lengthy steps, etc., to achieve both heat resistance and flame retardancy, improve heat resistance and flame retardancy, and increase crosslinking density

Active Publication Date: 2019-07-16
广东固研电子材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw materials of this method are expensive, the steps are lengthy, the imidazole as the curing agent is easy to be released, and the storage property of the epoxy resin compound is poor, the heat resistance is low, and the phosphorus-containing substances are easy to form phosphorus-rich wastewater
CN107099022A reports another kind of latent flame retardant curing agent, which adopts phosphorus-containing organic acid and organophosphorus chloride and imidazole to react to generate phosphorus-containing imidazole curing agent, which has short storage period, low heat resistance, and is easy to generate phosphorus-rich wastewater

Method used

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  • Heat-resistant flame-retardant epoxy resin latent curing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Dissolve 184.5g of cyanuric chloride in 500ml of tetrahydrofuran, cool to below 10°C, add 41.7g of 1-(3-aminopropyl)imidazole, and stir for 1 hour. Then 100g of 40% aqueous sodium hydroxide solution was added dropwise to neutralize the generated hydrogen chloride. The reactants were moved into a small autoclave, filled with saturated liquid ammonia, and all valves were closed. The temperature was then slowly raised to 100° C., and the reaction was continued for 2 hours. Then the pressure was released, and the product was suction filtered and washed with water to obtain a white solid. This solid was blended with 129g of cyanuric acid and 258g of water, heated to 80°C for 1 hour. After filtering and drying, a white solid was obtained, which was finally crushed into an ultrafine powder.

Embodiment 2

[0023] Dissolve 184.5 g of cyanuric chloride in 600 g of 1,4-dioxane, cool to 0-10°C, add 46.3 g of 1-(3-aminopropyl)-2-methylimidazole, and stir for 1 hour. Add 100g of 40% sodium hydroxide aqueous solution to neutralize the generated hydrogen chloride. The reactants were transferred into a small autoclave, filled with saturated liquid ammonia, and closed the valve. Slowly raise the temperature to 100°C, and continue the reaction for 2 hours. Then release the pressure, filter with suction and wash with water to obtain a white solid. This solid was blended with 129g of cyanuric acid and 258g of water, heated to 90°C for 1 hour. After filtering and drying, a white solid was obtained, which was finally crushed into an ultrafine powder.

Embodiment 3

[0025] Dissolve 184.5 g of cyanuric chloride in 650 g of n-butyl ether, cool to 10°C, add 41.7 g of 1-(2-aminoethyl)-2-methylimidazole, and react for 1 hour. The reactant was transferred into a small autoclave, and the temperature was raised while feeding liquid ammonia under high pressure to react, and finally the temperature was raised to 100°C and the high-pressure ammonia flow was maintained, and the reaction was continued for 1 hour. The n-butyl ether was distilled off under reduced pressure, and the residue was washed with water to obtain a white solid. This solid was blended with 129 g of cyanuric acid and 258 g of water and heated to reflux for 1 hour. After filtering and drying, a white solid was obtained, which was finally crushed into an ultrafine powder.

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Abstract

The invention discloses a heat-resistant flame-retardant epoxy resin latent curing agent and a preparation method thereof, and belongs to the technical field of organic synthesis. According to the preparation method, a reaction of cyanuric chloride and a primary amino-containing imidazole compound is carried out at a molar ratio of 1:1 at 0-10 DEG C in a suitable solvent, then a melamine intermediate containing an imidazole group is produced by pressurized ammonolysis at 100 DEG C, finally a complex is produced by reacting with cyanuric acid according to a molar ratio of 1:1 in a hot water, and the latent curing agent is obtained by filtering, drying and crushing. The compounded substance of the latent curing agent prepared by the method and epoxy resin can be stored for a long period of time and can be cured at a medium temperature, and the cured product has high heat resistance and excellent flame retardancy.

Description

technical field [0001] The invention relates to a latent curing agent and a preparation method thereof, in particular to a triazine heterocyclic modified imidazole type epoxy resin latent curing agent and a preparation method thereof, belonging to the technical field of organic synthesis. Background technique [0002] Epoxy resins and corresponding curing agents are mainly used in adhesives, coatings and composite materials. Because the cured product has excellent electrical insulation, it is widely used in the field of electronic and electrical industries. Epoxy resin curing agent is divided into two-component and one-component type, among which the one-component epoxy curing agent is accurate in measurement, easy to use, excellent in electrical insulation performance and mechanical strength of the cured product, and is widely used in electronic components, circuits Plates, sealing materials and composite materials. However, there are heating and flammability problems dur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/50
CPCC08G59/5086C08G59/5093
Inventor 康富春唐增花刘海明
Owner 广东固研电子材料有限公司
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