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Method for preparing phenyl glycidyl ether

A technology of phenyl glycidyl ether and synthesis method, which is applied in the direction of organic chemistry, can solve the problems of low utilization rate of synthesis method, use of volatile solvents, large environmental pollution, etc., achieve small color number, reduce color number, and product yield high rate effect

Active Publication Date: 2015-05-06
HUBEI GREENHOME MATERIALS TECH INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a synthetic method of phenyl glycidyl ether, which solves the problems of low utilization rate, high production cost, slow reaction speed, long reaction time, high energy consumption, low production efficiency and volatile use of existing synthetic methods. Solvent, environmental pollution and other technical problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Under nitrogen protection, the stirrer was turned on, and 120 parts of phenol, 2.4 parts of N,N-dimethylethanolamine, 14.4 parts of tetrabutylammonium hydrogen sulfate, and 2.4 parts of polyquaternium-7 were added to the reaction kettle. Heat up, when the temperature reaches 75°C, add 360 parts of epichlorohydrin dropwise, control the temperature at 80-85°C, after 3 hours of dripping, continue to keep warm for 1h; cool down to 50°C, under the protection of nitrogen, at 55-60°C Add 150 parts of 48% liquid caustic soda dropwise at a temperature of 1 hour, and continue to keep warm at a temperature of 55-60 °C for 3 hours; let it stand, drain the salt water, and then wash with 50 parts of soft water, and the lower oil phase is recovered by vacuum distillation. After epichlorohydrin was added, 190 parts of phenyl glycidyl ether were obtained, with a main content of 98.30%, an epoxy value of 0.655 mol / 100 parts, and an APHA color number of No. 10.

Embodiment 2

[0021] Under nitrogen protection, the stirrer was turned on, and 120 parts of phenol, 14.4 parts of N,N-dimethylethanolamine, 4.8 parts of tetrabutylammonium hydrogen sulfate, and 4.3 parts of polyquaternium-7 were added to the reaction kettle. Heat up, when the temperature reaches 75°C, add 360 parts of epichlorohydrin dropwise, control the temperature at 80-85°C, after 3 hours of dripping, continue to keep warm for 1h; cool down to 50°C, under the protection of nitrogen, at 55-60°C Add 150 parts of 48% liquid caustic soda dropwise at a temperature of 1 hour, and continue to keep warm at a temperature of 55-60 °C for 3 hours; let it stand, drain the salt water, and then wash with 50 parts of soft water, and the lower oil phase is recovered by vacuum distillation. After epichlorohydrin was added, 190 parts of phenyl glycidyl ether were obtained, with a main content of 97.61%, an epoxy value of 0.650 mol / 100 parts, and an APHA color number of No. 10.

Embodiment 3

[0023] Under nitrogen protection, the stirrer was turned on, and 120 parts of phenol, 7.2 parts of N,N-dimethylethanolamine, 7.2 parts of tetrabutylammonium hydrogen sulfate, and 2.5 parts of polyquaternium-7 were added to the reaction kettle. Heat up, when the temperature reaches 75°C, add 240 parts of epichlorohydrin dropwise, control the temperature at 80-85°C, after 3 hours of dripping, continue to keep warm for 1h; cool down to 50°C, under the protection of nitrogen, at 55-60°C Add 150 parts of 48% liquid caustic soda dropwise at a temperature of 1 hour, and continue to keep warm at a temperature of 55-60 °C for 3 hours; let it stand, drain the salt water, and then wash with 50 parts of soft water, and the lower oil phase is recovered by vacuum distillation. After epichlorohydrin was added, 190 parts of phenyl glycidyl ether were obtained, the main content was 98.4%, the epoxy value was 0.656mol / 100 parts, and the color number was No. 10.

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Abstract

The invention relates to a synthetic method of phenyl glycidyl ether. The method comprises the following steps: carrying out ring-opening reaction; carrying out ring-closure reaction; washing; refining; and recovering excessive epoxy chloropropane in vacuum from a phenyl glycidyl ether coarse to obtain a phenyl glycidyl ether finished product, wherein the recovered epoxy chloropropane is directly reused in next batch. The method comprises the following steps: by taking phenol and epoxy chloropropane as raw materials, firstly, carrying out ring-opening reaction under the action of a ternary compound catalyst comprising N,N-dimethylethanolamine, tetrabutylammonium hydrogen sulfate and quaternary ammonium salt-7 to prepare an intermediate phenyl chlorhydrin; and then carrying out ring-closure reaction with a sodium hydroxide solution to prepare the phenyl glycidyl ether, wherein the recovered epoxy chloropropane can be directly reused. The method provided by the invention has the advantages of simple process, short production cycle, high final product yield, high epoxide number, small color number and the like and is easily industrialized.

Description

technical field [0001] The invention relates to a phenyl glycidyl ether, in particular to a synthesis method of the phenyl glycidyl ether. Background technique [0002] The molecule of phenyl glycidyl ether contains benzene ring, ether bond and epoxy group, and it contains a rigid segment in the structure. It has better heat resistance and anti-corrosion performance. Compared with butyl glycidyl ether, the cured product has a lower heat distortion temperature There is a significant improvement. Widely used in electronics, electrical appliances, electromechanical, and machinery industries to reduce the viscosity of epoxy, suitable for potting, casting, impregnation and other application processes, and can also be used in adhesives. Epoxy resin curing agent can be prepared by reacting with polyamine. [0003] The traditional synthesis method of phenyl glycidyl ether is a one-step method, that is, it is obtained by reacting phenol, epichlorohydrin and sodium hydroxide in the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/23C07D301/26
CPCC07D301/26C07D303/23
Inventor 杨华胡登华肖华青黄圣
Owner HUBEI GREENHOME MATERIALS TECH INC
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