A kind of phosphorus, nitrogen-containing epoxy resin flame retardant curing agent and preparation method thereof

A nitrogen epoxy resin and curing agent technology, applied in the field of chemical curing agent and its preparation, can solve problems such as fire hazards, and achieve the effects of convenient post-processing, high purity and easy control

Inactive Publication Date: 2018-06-22
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the manufacturer's practice of reducing production costs and "responsive to environmental protection regulations" has led to serious fire hazards
This allows an extremely small source of ignition to sustain burning of unflammable televisions, which has resulted in the loss of many lives

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The first step: to the equipment equipped with reflux condenser, thermometer, N 2 Add 300ml of acetonitrile as a solvent into the 500ml three-neck flask of the introduction tube and magnet, and then add 26.9g of PEPA and 23.0g of POCl 3 . Access to N 2 Protected, the temperature was raised to 80°C for 20h. After the reaction, a light yellow liquid slurry is obtained, and the liquid is filtered, rotary evaporated, and dried to obtain a light yellow viscous liquid, which is the intermediate.

[0028] The second step: in the tank equipped with magnetic stirring, dropping funnel, N 2 Add 50ml of acetonitrile as a solvent into the 100ml four-necked bottle of the introduction tube and thermometer, and then add 13.60g of m-xylylenediamine; dissolve 14.85g of the intermediate in 20ml of acetonitrile, and transfer the solution to a constant pressure dropping funnel, ice Start dropwise addition under the bath, after 2.0 hours of dropwise addition, raise the temperature to 50°...

Embodiment 2

[0030] The first step: the synthetic method of phosphorus, nitrogen intermediate is the same as embodiment 1.

[0031] The second step: equipped with magnetic stirring, dropping funnel, N 2 Add 60ml of acetonitrile as a solvent into the 100ml four-necked flask of the introduction tube and thermometer, and then add 20.40g of m-xylylenediamine; dissolve 22.25g of the intermediate in 30ml of acetonitrile, and transfer it to a constant pressure dropping funnel, ice Start dropwise addition under the bath, after 2.0 hours of dropwise addition, raise the temperature to 50°C, keep the temperature for 16 hours, and end the reaction. After treatment, a white solid can be obtained.

Embodiment 3

[0033] The first step: the synthetic method of phosphorus, nitrogen intermediate is the same as embodiment 1.

[0034] The second step: equipped with magnetic stirring, dropping funnel, N 2 Add 100ml of acetonitrile as a solvent to the 250ml four-necked bottle of the introduction tube and thermometer, and then add 40.80g of m-xylylenediamine; dissolve 44.50g of the intermediate in 60ml of acetonitrile, and transfer it to a constant pressure dripping funnel, and put it in an ice bath After 3.0 hours of dropping, the temperature was raised to 50°C, and the temperature was kept for 24 hours to complete the reaction. After treatment, a white solid was obtained.

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Abstract

A phosphorus and nitrogen-containing epoxy resin flame retardant curing agent and its preparation method, relating to a chemical curing agent and its preparation method, the preparation raw materials include: phosphorus oxychloride, 1-oxyphospha-4-hydroxymethyl ‑2,6,7‑trioxabicyclo[2.2.2]octane and m-xylylenediamine, the method for preparing the flame retardant is divided into two steps, the first step, phosphorus oxychloride (POCl3 ) and 1-oxygen phospha-4-hydroxymethyl-2,6,7-trioxabicyclo [2.2.2] octane (PEPA) react under certain conditions to generate a phosphorus-containing intermediate; the second step, The intermediate obtained in the first step is stirred and reacted with m-xylylenediamine under the introduction of an inert gas for a certain period of time, and the product is filtered, washed, dried, etc. to obtain a white solid. The compound has good compatibility with epoxy resin, can be cured together with epoxy resin, and has little influence on the mechanical properties of the cured product. It can be used as a curing agent for epoxy resin, and can effectively improve the flame retardant properties.

Description

technical field [0001] The invention relates to a chemical curing agent and a preparation method thereof, in particular to a phosphorus and nitrogen-containing epoxy resin flame retardant curing agent and a preparation method thereof. Background technique [0002] Epoxy resin is a kind of thermosetting polymer synthetic material with excellent bonding, anti-corrosion, insulation, formability, high strength and other properties. It has excellent performance in mechanics, electrical appliances, heat and chemical resistance. Due to the above-mentioned excellent properties, epoxy resin is widely used in the manufacture of adhesives, coatings, insulating materials, etc. And it plays an important role in electronics, electricity, optical machinery, aerospace, shipping and many other industrial fields, and its application covers almost all industrial fields. However, the biggest disadvantage of epoxy resin in application is that it is flammable, and flammability is also a common p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/50C07F9/6574
CPCC07F9/65742C08G59/504
Inventor 梁兵王志国
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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