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Preparation method of Lewis acid ionic liquid catalyzed synthesis of phosphoric acid triester

A phosphate triester and ionic liquid technology, which is applied in the production of phosphorus organic compounds and bulk chemicals, can solve the problems of unstable catalysts, unrecyclable, and environmental pollution, and achieve the effect of cheap raw materials, good quality, and good color

Active Publication Date: 2015-11-18
张家港市飞航科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst types can be roughly divided into three categories: 1. Lewis acid, such as anhydrous AlCl 3 , MgCl 2 etc. (Shen Qi, Zhou Lequn, Qiu Guocai, etc. The preparation method of TCPP flame retardant [P].CN101007952A), these catalysts themselves are unstable, and are easily hydrolyzed in the air; post-reaction treatment is difficult, cannot be recycled and pollutes the environment

Method used

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  • Preparation method of Lewis acid ionic liquid catalyzed synthesis of phosphoric acid triester

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Experimental program
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Effect test

Embodiment 1

[0037] BTEAC22.78g (0.1mol) was added to a three-necked flask (100mL) equipped with a condenser tube (connected to the exhaust gas absorption device at the top) and a thermometer, CH 2 Cl 2 30mL, then add AlCl 3 13.34g (0.1mol), react at room temperature for 5h, stop the reaction, cool down, remove the solvent to obtain the final product, the yield is 92%.

Embodiment 2

[0039] In a three-necked flask (100mL) equipped with a condenser tube (connected to the exhaust gas absorption device) and a thermometer, add BTEAC45.56g (0.2mol), CH 2 Cl 2 40mL, then add AlCl 3 13.34g (0.1mol) was reacted at room temperature for 5h, the reaction was stopped, the temperature was lowered, and the solvent was removed to obtain the final product with a yield of 90%.

Embodiment 3

[0041] In a three-necked flask (250mL) equipped with a condenser tube (connected to the exhaust gas absorption device) and a thermometer, add BTEAC68.34g (0.3mol), CH 2 Cl 2 50mL, then add AlCl 3 13.34g (0.1mol), reacted at room temperature for 5h, stopped the reaction, cooled the temperature, removed the solvent to obtain the final product, and the yield was 89%.

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Abstract

The invention discloses a preparation method for synthesizing phosphotriester under the catalysis of Lewis acid ionic liquid. According to the method, the phosphotriester is generated by performing ring-opening reaction of phosphorus oxychloride and an epoxide under the catalysis of a catalyst, wherein ionic liquid [A]-x[Lewis acid] formed by the catalyst is Lewis acid and A; and A is amine and a derivative thereof, imidazole or a derivative thereof or pyridine and a derivative thereof. According to the preparation method, the catalyst is low in cost of raw materials, high in catalytic efficiency, little in using amount and environment-friendly, and a process is simple; and the prepared phosphate flame retardant product is high in quality, small in acid value, good in color and high in purity.

Description

technical field [0001] The invention relates to a preparation process of a flame retardant phosphoric acid ester, in particular to a preparation method of a flame retardant phosphoric acid triester synthesized by the Lewis acid ionic liquid catalyzing the ring-opening reaction of phosphorus oxychloride and an epoxide. Background technique [0002] Phosphate ester is an excellent flame retardant widely used in synthetic materials, architectural decoration, cables, batteries, soft (hard) polyurethane foam, etc., and has good thermal conductivity, hydrolysis stability and low temperature in rigid polyurethane foam. low viscosity. The flame retardant effect is remarkable, and it has the functions of plasticizing, moisture-proof and anti-static, so it has a good development prospect. [0003] A preparation method of the phosphoric acid ester is that phosphorous oxychloride and an epoxide undergo a ring-opening reaction under the action of a catalyst to obtain a phosphoric acid t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/09
CPCY02P20/542Y02P20/54
Inventor 职慧珍杨锦飞黄小冬
Owner 张家港市飞航科技有限公司