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Epoxy resin modified amine flame-retarding curing agent and preparation method thereof

A technology of epoxy resin and curing agent, which is applied in the field of chemical synthesis and its preparation, can solve problems such as fire hazards, and achieve the effects of convenient post-processing, simple preparation method, and mild conditions

Inactive Publication Date: 2016-11-16
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

[0026] 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 magneton, and then add 20.4gPER and 23.0g POCl respectively 3 and 0.61gAlCl 3 . Access to N 2 Protected, heated to 80°C for 6 hours, 100°C for 4 hours, filtered, washed, and dried after the reaction to obtain a white solid powder, which is the intermediate SPDPC.

[0027] The second step: in the tank equipped with magnetic stirring, dropping funnel, N 2 Add 100ml of acetonitrile as a solvent into the 250ml four-neck bottle of the introduction tube and thermometer, then add 5.94g of intermediate SPDPC and 4.15g of triethylamine; mix 5.90g of 1,3-BAC with 20ml of acetonitrile, and transfer the solution to a constant pressure drop In the liquid funnel, start dropwise addition at room temperature. After 2.0 hours of dropwise addition, the temperature is raised to 50°C, and the reaction is ke...

Embodiment 2

[0029] The first step: the synthetic method of the intermediate is the same as in Example 1.

[0030] The second step: equipped with magnetic stirring, dropping funnel, N 2 Add 300ml of acetonitrile as a solvent to the 500ml four-necked bottle of the introduction tube and thermometer, then add 18.0g of intermediate SPDPC and 12.5g of triethylamine; mix 18.0g of 1,3-BAC with 50ml of acetonitrile, and transfer it to a constant pressure drop In the liquid funnel, start dropwise addition at room temperature, after 2.0 hours of dropwise addition, raise the temperature to 70°C, keep the temperature for 6 hours, and end the reaction. After treatment, a white solid powder can be obtained.

Embodiment 3

[0032] The first step: the synthetic method of the intermediate is the same as in Example 1.

[0033] The second step: in the tank equipped with magnetic stirring, dropping funnel, N 2 Add 100ml of acetonitrile as a solvent into the 250ml four-neck bottle of the introduction tube and thermometer, then add 5.94g of intermediate SPDPC and 4.15g of triethylamine; mix 5.90g of 1,3-BAC with 20ml of acetonitrile, and transfer the solution to a constant pressure drop In the liquid funnel, start dropwise addition at room temperature, after 2.0 hours of dropwise addition, raise the temperature to 60°C, keep the temperature for 10 hours, and end the reaction. After treatment, a white solid powder can be obtained.

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PUM

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Abstract

The invention provides an epoxy resin modified amine flame-retarding curing agent and a preparation method thereof and relates to a chemical synthetic agent and a preparation method thereof. The epoxy resin modified amine flame-retarding curing agent is prepared from the following raw materials: phosphorus oxychloride (POCl3), pentaerythritol (PER) and 1,3-bis(aminomethyl)-cyclohexan (1,3-BAC); a method for preparing a fire retardant comprises the following two steps: step 1, taking the POCl3 and the PER to react under a certain condition to generate a phosphorus-containing intermediate SPDPC (Spirobisphosphate Diacyl Chloride); step 2, stirring the intermediate obtained in the step 1 and the 1,3-BAC to react for certain time under the condition that inert gas is introduced; filtering, washing and drying a product and so on to obtain white solid powder. The compound has good dispersiveness in epoxy resin and can be cured with the epoxy resin together; the compound can be used as a curing agent of the epoxy resin and can also effectively improve the flame-retarding property of the epoxy resin. The epoxy resin modified amine flame-retarding curing agent and the preparation method thereof have the advantages of simple process production conditions, relatively high purity and yield of the product and simple and convenient post-treatment process.

Description

technical field [0001] The invention relates to a chemical synthesis agent and a preparation method thereof, in particular to an epoxy resin modified amine 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 problem with most...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/50C07F9/6574
CPCC08G59/5046C07F9/65744
Inventor 梁兵王志国
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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