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DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) modified anhydride epoxy resin flame-retardant curing agent and preparation method thereof

A technology of acid anhydride epoxy resin and curing agent, which is applied in the field of curing agent and its preparation, can solve problems such as the limitation of the application range of flammable epoxy resin, and achieve the effects of easy control, simple preparation method and mild conditions

Inactive Publication Date: 2017-05-31
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Flammability greatly limits the application range of epoxy resin

Method used

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  • DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) modified anhydride epoxy resin flame-retardant curing agent and preparation method thereof
  • DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) modified anhydride epoxy resin flame-retardant curing agent and preparation method thereof
  • DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) modified anhydride epoxy resin flame-retardant curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Equipped with reflux condenser, thermometer, N 2 Add 160ml of dioxane as a solvent into the 250ml three-necked bottle of the introduction tube and magneton, add 86.4g of DOPO, and pass through N 2 Protect. Heat and stir until it is completely dissolved, then add 66.47g of 2-methyltetrahydrophthalic anhydride, react at reflux temperature for 12 hours, cool down to room temperature, rotary evaporate, and stand to cool to obtain a light yellow liquid.

Embodiment 2

[0023] Equipped with reflux condenser, thermometer, N 2 Add 86.4g DOPO into the 250ml three-necked bottle of the introduction tube and magnet, and inject N 2 Protect. Heat to raise the temperature, add 66.47g of 2-methyltetrahydrophthalic anhydride after it is completely melted, start stirring, react at 140°C for 6h, cool down to room temperature, and stand overnight to obtain a light yellow liquid.

Embodiment 3

[0025] Equipped with reflux condenser, thermometer, N 2 Add 160ml of toluene as a solvent to the 250ml three-necked flask that introduces the tube and magnet, add 36g of DOPO, and pass through N 2 Protect. Heat and stir until it is completely dissolved, then add 66.47g of 2-methyltetrahydrophthalic anhydride, react at reflux temperature for 8 hours, cool down to room temperature, rotary evaporate, and stand still to obtain a colorless transparent liquid.

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Abstract

The invention provides a DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) modified anhydride epoxy resin flame-retardant curing agent and a preparation method thereof and relates to a chemical synthesis agent and a preparation method thereof. The curing agent comprises the following raw materials: DOPO and 2-methyl tetrahydrophthalic phthalic anhydride. The flame-retardant curing agent is simple in a preparation process and can be prepared only by a one-step reaction, that is, DOPO and 2-methyl tetrahydrophthalic phthalic anhydride are mixed with a solvent under an inert gas atmosphere for a reaction for hours at a certain temperature, and rotary evaporateion and solvent removal are performed, so as to obtain a product; or DOPO reacts with 2-methyl tetrahydrophthalic phthalic anhydride react with each other for hours under the condition of no solvent and then are cooled to the room temperature, so as to obtain an acquired product; and the products obtained under different proportion conditions are colorless liquid to light yellow liquid. In a processing process, the raw materials can be well mixed with epoxy resin and can be cured into one together with the epoxy resin; and the flame-retardant curing agent can be taken as a curing agent of the epoxy resin, and the flame retardant property of the epoxy resin can be effectively improved. The preparation method is simple and convenient, and modified anhydride curing agents with different phosphorus contents can be prepared as required.

Description

technical field [0001] The invention relates to a curing agent and a preparation method thereof, in particular to a DOPO modified acid anhydride epoxy resin flame retardant curing agent and a preparation method thereof. Background technique [0002] Epoxy resin is a kind of thermosetting polymer material with excellent bonding, anti-corrosion, insulation, molding processing, high strength and other properties. It has superior performance in mechanics, heat and chemical resistance. Widely used in coatings, adhesives, insulating materials, electrical and electronic, optical machinery, aerospace and many other industrial fields. During application it was found that the epoxy resin was extremely flammable. The flammability greatly limits the scope of application of epoxy resins. Therefore, it is of great significance to study the flame retardancy of epoxy resin for expanding its application in the fields of electronics, aerospace and aerospace. [0003] The research on the fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/42C07F9/6574
CPCC08G59/4238C07F9/657172
Inventor 梁兵王志国
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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