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Phosphorous-containing epoxy resin amine curing agent and preparation method thereof

The technology of an amine curing agent and epoxy resin, which is applied in the field of chemical synthesis and its preparation, can solve the problems of application limitation, easy fire, low oxygen index of epoxy resin, etc., and achieve simple preparation method, easy control, mechanical good performance effect

Inactive Publication Date: 2015-07-22
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the oxygen index of epoxy resin is low (about 19.8), and it is a flammable substance. Continuous spontaneous combustion after leaving the fire is easy to cause fire, which greatly restricts its application. Therefore, to improve and improve the flame retardancy of epoxy resin, Has far-reaching implications for reducing fire hazards

Method used

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  • Phosphorous-containing epoxy resin amine curing agent and preparation method thereof
  • Phosphorous-containing epoxy resin amine curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The first step: to the equipped with reflux condenser, thermometer N 2 Add 13.62g of pentaerythritol and 23.8ml of phosphorus oxychloride into the 250ml three-necked bottle of the introduction tube and magnet, then add 80ml of chlorobenzene as solvent, 0.3g of AlCl 3 as a catalyst. Pass N 2 Protection, the temperature was raised to 60°C to start the reaction, after 1 hour, the temperature was raised to 80°C for 3 hours, and then the temperature was raised to 100°C for 8 hours. Pass N after the reaction 2 Protected and cooled to room temperature, a white liquid was obtained. After the liquid was filtered, washed and dried, a white powdery solid was obtained.

[0031] Step 2: In a 100ml three-neck flask equipped with magnetic stirring, dropping funnel and thermometer, add SPDPC5.94g and 40ml of acetonitrile, add 2.1ml of ethylenediamine to the dropping funnel and dilute with 10ml of acetonitrile until the temperature rises to 50 After 1.5 hours of dropping, keep t...

Embodiment 2

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

[0034] Step two:

[0035] Step 2: In a 100ml three-neck flask equipped with magnetic stirring, dropping funnel and thermometer, add SPDPC5.94g and 40ml of acetonitrile, add 2.7ml of ethylenediamine to the dropping funnel and dilute with 10ml of acetonitrile until the temperature rises to 50 After 1.5 hours of dropping, keep the temperature at 70°C until no HCl gas is released, then slowly cool down to room temperature, filter, wash with dichloromethane for several times, and dry at 50°C to obtain a slightly Pale yellow powdery solid.

Embodiment 3

[0037] The first step: the synthetic method of phosphorus-containing intermediate is the same as embodiment 1.

[0038] Step 2: Add SPDPC 29.7g and 100ml of acetonitrile to a 250ml three-neck flask equipped with magnetic stirring, dropping funnel and thermometer, add 10.5ml of ethylenediamine to the dropping funnel and dilute with 40ml of acetonitrile until the temperature rises to 50 After 1.5 hours of dropping, keep the temperature at 70°C until no HCl gas is released, then slowly cool down to room temperature, filter, wash with dichloromethane for several times, and dry at 50°C to obtain a slightly Pale yellow powdery solid.

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Abstract

The invention discloses a phosphorous-containing epoxy resin amine curing agent and a preparation method thereof, and relates to a chemical synthetic agent and a preparation method thereof. Preparation raw materials include pentaerythritol ester rosin (PER), phosphorus oxychloride (POCl3) and ethidene diamine. The preparation method for the curing agent comprises the following two steps: firstly, producing a reaction of PER and POCl3 under a certain condition to generate a phosphorous-containing intermediate, namely spirobisphosphate diphosphonic chloride (SPDPC); secondly, producing a stirring reaction of SPDPC and ethidene diamine for a certain time by introducing inert gas, performing treatment of filtering, washing, drying and the like on a product, and obtaining faint yellow powdery solid. A compound has relatively high thermal stability and expandability as well as high char yield, and can be used as an epoxy resin curing agent for improving flame-retardant performance of a cured product. A process is simple in production condition, relatively high in product purity and yield and simple and convenient in post-treatment process.

Description

technical field [0001] The invention relates to a chemical synthesis agent and a preparation method thereof, in particular to a phosphorus-containing epoxy resin amine curing agent and a preparation method thereof. Background technique [0002] Epoxy resin has been widely used in many fields due to its excellent performance, and has become an extremely important type of thermosetting resin. In recent years, with the rapid development of the electrical and electronic industry, epoxy resin has also been widely used in the fields of electronic component bonding, packaging, and printed circuit board (PCBs) production, and has become one of the most important electronic chemical materials. . However, the oxygen index of epoxy resin is low (about 19.8), and it is a flammable substance. Continuous spontaneous combustion after leaving the fire is easy to cause fire, which greatly restricts its application. Therefore, to improve and improve the flame retardancy of epoxy resin, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/50C08G79/04C07F9/6574
Inventor 梁兵王刚宁志高王长松
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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