Phosphorus and nitrogen containing flame-retardant curing agent for epoxy resin and preparation method for agent

A nitrogen epoxy resin and curing agent technology, which is applied in the field of phosphorus-containing, nitrogen epoxy resin flame retardant curing agent and its preparation, can solve the problems of plastic products cannot be recycled or destroyed, waste the environment, pollution, etc. The effect of protection, convenient post-processing and high purity

Inactive Publication Date: 2017-08-18
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the in-depth research, it is found that a small amount of dioxin or dibenzofuran will be released during the combustion process. These substances produced by combustion will cause serious harm to the human body, and at the same time make plastic products unable to be recycled or destroyed. Causes great waste and brings serious environmental pollution problems

Method used

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  • Phosphorus and nitrogen containing flame-retardant curing agent for epoxy resin and preparation method for agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The first step: to the equipment equipped with reflux condenser, thermometer, N 2 Add 50.598g (0.33mol) of phosphorus oxychloride to the 250ml three-necked bottle of the introduction tube and dropping funnel, and 120ml of dichloromethane as a solvent, then add 25.612g (0.35mol) of diethylamine and triethylamine in the dropping funnel 33.393g (0.33mol), feed N 2 Protection, the dropwise addition was completed in 3 hours under ice-bath conditions, the temperature was raised to 20°C, and the reaction was kept for 12 hours. After the reaction, a light yellow liquid slurry is obtained, and the liquid is filtered, rotary evaporated, and vacuum distilled to obtain a colorless transparent liquid, which is an intermediate.

[0021] The second step: equipped with magnetic stirring, dropping funnel, N 2 Add 22.512g (0.2mol) p-phenylenediamine to the 250ml four-necked bottle of the introduction tube and thermometer, add 120ml chloroform as solvent, dissolve 20.418g intermediate i...

Embodiment 2

[0023] The first step: the synthetic method of phosphorus, nitrogen intermediate is the same as embodiment 1.

[0024] The second step: equipped with magnetic stirring, dropping funnel, N 2 Add 22.512g (0.2mol) p-phenylenediamine in the 250ml four-necked bottle of introduction tube and thermometer, add 120ml dichloromethane as solvent, 20.418g (0.1mol) intermediate is dissolved in 20ml dichloromethane, and its Transfer to a constant pressure dropping funnel, raise the temperature to 40°C and start dropwise addition. After 2.0 hours, the dropwise addition is completed, and the reaction is continued for 12 hours. The product can be treated to obtain a light gray solid.

Embodiment 3

[0026] The first step: the synthetic method of phosphorus, nitrogen intermediate is the same as embodiment 1.

[0027] The second step: equipped with magnetic stirring, dropping funnel, N 2 Add 23.798g (0.22mol) of p-phenylenediamine in the 250ml four-neck bottle of the introduction tube and thermometer, add 120ml of dichloromethane as solvent, dissolve 20.418g (0.1mol) of the intermediate in 20ml of dichloromethane, and Transfer to a constant pressure dropping funnel, raise the temperature to 40°C and start dropwise addition. After 2.0 hours, the dropwise addition is completed, and the reaction is continued for 12 hours. The product can be treated to obtain a light gray solid.

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Abstract

The invention discloses a phosphorus and nitrogen containing flame-retardant curing agent for epoxy resin and a preparation method for the agent, and relates to a chemical synthesis agent and a preparation method thereof. Preparation raw materials comprise phosphorus oxychloride, ethylenediamine and p-phenylenediamine. The method for preparing the flame-retardant curing agent comprises the following two steps: step 1, reacting phosphorus oxychloride (POCl3) with ethylenediamine under a certain condition to generate a phosphorus-containing intermediate; and step 2, reacting the obtained intermediate with p-phenylenediamine under a condition of an introduced inert gas with stirring for a period, and performing filtering, washing, drying and other processing on the obtained product, so as to obtain a light grey solid. The prepared compound has good compatibility with epoxy resin, can be cured together with epoxy resin, has little influence on mechanical properties of the cured material, can be used as a curing agent of epoxy resin, and also can effectively improve the flame retardancy of epoxy resin. The production conditions are simple, the product purity and yield are relatively high, and the post-processing process is simple.

Description

technical field [0001] The invention relates to a flame retardant curing agent for phosphorus and nitrogen epoxy resin and a preparation method thereof, in particular to a flame retardant curing agent for phosphorus and nitrogen epoxy resin and a preparation method thereof. Background technique [0002] Epoxy resin is one of the general plastics. It is widely used in pouring, coatings, adhesives and various composite materials. It shows excellent mechanical properties and electrical properties. Its better processing type and low shrinkage rate are more Its wide application is possible. However, its application is seriously hindered by its flammability. Therefore, it is of great significance to take necessary measures to improve its flame retardancy to broaden its application fields. [0003] The traditional flame retardant method is mainly to add additive flame retardants. Among them, halogenated flame retardants perform best in improving flame retardancy. However, due t...

Claims

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Application Information

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IPC IPC(8): C08G59/50C07F9/22
CPCC08G59/504C07F9/224
Inventor 梁兵刘晓丽
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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