Dichlorophenylphosphine oxide and m-xylylenediamine epoxy resin curing agent and preparation method thereof

A technology of m-xylylenediamine epoxy resin and phenylphosphonyl dichloride, which is applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc., can solve the influence of matrix mechanical properties, Limited wide application, poor compatibility and other problems, to achieve the effects of good mechanical properties, easy control, and convenient post-processing

Inactive Publication Date: 2017-06-16
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the poor compatibility with the matrix, the traditional additive flame retardants are easy to migrate and have a serious impact on the mechanical properties of the matrix. Although some stu

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 19.498g (0.1mol) of DCPPO, 100ml of 1,2-dichloroethane and 10ml of DMF into a 250ml three-necked flask equipped with a condenser tube, nitrogen conduit, thermometer and magnetic stirring, and accurately measure 40.850g (0.3mol) of MXDA , 10ml of 1,2 dichloroethane was added to the constant pressure dropping funnel, the dropping rate was controlled, the dropping was completed within 2 hours, and the reaction was completed under nitrogen protection at 20°C for 6 hours. The product was filtered, washed, and then dried in a vacuum oven at 60°C for 12 hours to obtain a white solid powder.

Embodiment 2

[0026] Add 19.498g (0.1mol) of DCPPO and 110ml of methylene chloride as a solvent in a 250ml three-necked flask equipped with a condenser, a nitrogen conduit, a thermometer and a magnetic stirrer, and accurately measure 40.850g (0.3mol) of MXDA to control the rate of addition. The dropwise addition was completed within 2 hours, and the reaction was completed under nitrogen protection at 20°C for 6 hours. The product was filtered, washed, and then dried in a vacuum oven at 60°C for 12 hours to obtain a white solid powder.

Embodiment 3

[0028] Add 19.498g (0.1mol) of DCPPO and 110ml of methylene chloride as a solvent in a 250ml three-neck flask equipped with a condenser, a nitrogen conduit, a thermometer and a magnetic stirrer, and accurately measure 47.659g (0.35mol) of MXDA to control the rate of addition. The dropwise addition was completed within 2 hours, and the reaction was completed under nitrogen protection at 20°C for 6 hours. The product was filtered, washed, and then dried in a vacuum oven at 60°C for 12 hours to obtain a white solid powder.

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PUM

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Abstract

The invention relates to a curing agent and a preparation method thereof, and concretely relates to a dichlorophenylphosphine oxide and m-xylylenediamine epoxy resin curing agent and a preparation method thereof. Raw materials for preparing the dichlorophenylphosphine oxide and m-xylylenediamine epoxy resin curing agent comprise dichlorophenylphosphine oxide and m-xylylenediamine. The method for preparing the curing agent comprises the following steps; stirring and reacting dichlorophenylphosphine oxide (DCPPO) and m-xylylenediamine (MXDA) under the introduction of an inert gas for a certain period of time, and carrying out filtering, washing and drying treatment on the above obtained product to obtain a white solid. The above compound has good compatibility with epoxy resin, can be cured together with the epoxy resin, has small influences on the mechanical performances of a cured product, can be used as an epoxy resin curing agent, and also effectively improves the flame retardation performance of the epoxy resin. The method has the advantages of simple production conditions, high purity and high yield of the target product, and simple post-treatment process.

Description

technical field [0001] The invention relates to a curing agent and a preparation method thereof, in particular to a phenylphosphonic dichloride and m-xylylenediamine epoxy resin curing agent and a preparation method thereof. Background technique [0002] Epoxy resin is a widely used high polymer, which is widely used in casting, coating, adhesive and composite materials, showing excellent mechanical and electrical properties. Nevertheless, their flammability limits their applications in electronics (printed circuit boards, electronic packaging, etc.) and transportation (cars, trains, and airplanes). Therefore, the development of flame-retardant epoxy resin plays a very important role in broadening its application fields. [0003] At present, many technologies have been widely used in the flame retardant technology of epoxy resin. Among them, halogenated flame retardants are widely used in the flame retardant of epoxy resin because of their excellent flame retardant effect. ...

Claims

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Application Information

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IPC IPC(8): C07F9/44C08G59/50
CPCC07F9/448C08G59/504
Inventor 梁兵刘晓丽
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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