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Phenolic hydroxy epoxidation preparation technology

A phenolic hydroxyl ring and preparation process technology, applied in the field of phenolic hydroxyl epoxidation preparation process, can solve the problems of large environmental pollution, reduced hydrolyzable chlorine content, low epoxy products and the like, achieve process stability and reduce hydrolyzable chlorine content and inorganic chlorine content, the effect of reducing environmental pressure

Inactive Publication Date: 2019-03-12
江苏和和新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The obtained product needs to be washed with water to remove salt, refined with alkali, and post-treatment steps such as water washing, neutralization, filtration, and solvent removal to reduce the hydrolyzable chlorine content. The lowest hydrolyzable chlorine content can reach 68.9ppm, but the above post-treatment The process produces a large amount of waste water and VOC, which pollutes the environment a lot
[0007] Therefore, the currently disclosed phenolic hydroxyl epoxidation process still cannot directly obtain the epoxy product with low hydrolyzable chlorine content

Method used

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  • Phenolic hydroxy epoxidation preparation technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Soak 5g of SBA-15 mesoporous molecular sieve in 100mL aminopropyltriethoxysilane coupling agent hydrolyzate (concentration is 1wt%, adjust pH to 5 with glacial acetic acid and let stand for 2 hours); take out after soaking for 2 hours Dry;

[0049]Mix benzyltriethylammonium chloride aqueous solution (concentration: 20g / L, 100mL) with treated SBA-15 mesoporous molecular sieve (5g), remove the water by evaporation, and place the remaining material in an ultrasonic microwave device for 120 ℃ and heated for 20 minutes to obtain the SBA-15 mesoporous molecular sieve catalyst solidly loaded with benzyltriethylammonium chloride.

[0050] Add bisphenol A and epichlorohydrin (molar ratio 1:2.1) under normal pressure, add the mesoporous molecular sieve catalyst (addition molar amount is bisphenol 0.005 of A), carry out etherification ring-opening reaction at 100°C, the reaction time is 2 hours, and obtain chlorohydrin ether; when the system cools down to about 60°C, the catalyst...

Embodiment 2

[0052] The raw materials and process parameters of the phenolic hydroxyl epoxidation preparation process are exactly the same as in Example 1, the only difference being that the catalyst used is the SBA solid-loaded with benzyltriethylammonium chloride that has been used 5 times and recovered in Example 1. -15 mesoporous molecular sieve catalyst. The performance test results of the final product are listed in Table 1 below.

Embodiment 3

[0054] Soak 10g of SBA-15 mesoporous molecular sieve in 500mL aminopropyltrimethoxysilane coupling agent hydrolyzate (3% concentration, adjust pH to 5 with glacial acetic acid and let it stand for 1 hour); take it out and dry it after soaking for 2 hours;

[0055] Mix benzyltriethylammonium chloride aqueous solution (concentration: 1000g / L, 50mL) with treated SBA-15 mesoporous molecular sieve (10g), remove the water by evaporation, and place the remaining material in an ultrasonic microwave device for 140 ℃ and heated for 40 minutes to obtain the SBA-15 mesoporous molecular sieve catalyst solidly loaded with benzyltriethylammonium chloride.

[0056] Add bisphenol F and epichlorohydrin (molar ratio 1:2) under normal pressure, add the mesoporous molecular sieve catalyst (addition molar amount is bisphenol 0.005 of A), etherification ring-opening reaction was carried out at 110°C, and the reaction time was 1 hour to obtain chlorohydrin ether; when the system was cooled to about 4...

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Abstract

The invention discloses a phenolic hydroxy epoxidation preparation technology. A compound containing phenolic hydroxyl and epoxy chloropropane are taken as raw materials; under the effect of a catalyst, chlorohydrin ether is prepared by etherification ring-opening reaction; and a phenolic hydroxy epoxidation product is prepared by ring-closure reaction, wherein the catalyst is mesoporous molecularsieves with immobilized benzyl triethyl ammonium chloride. The phenolic hydroxy epoxidation preparation technology includes modifying the mesoporous molecular sieves; mixing the modified mesoporous molecular sieves with a benzyl triethyl ammonium chloride water solution; and preparing the phenolic hydroxy epoxidation product by an ultrasonic microwave heating immobilization method. By adopting the phenolic hydroxy epoxidation preparation technology, the epoxidation product with a low hydrolysable chlorine content can be directly prepared, complicated post-treatment technologies are omitted, the technology is stable, material consumption and energy consumption are low, byproducts are fewer, and the catalyst can be recycled, so that the preparation technology can be used for large-scale industrial production.

Description

technical field [0001] The invention relates to an epoxy resin preparation process, in particular to a phenolic hydroxyl epoxidation preparation process. Background technique [0002] Due to its excellent mechanical and electrical properties, epoxy resin has developed into a large class of thermosetting resins and is widely used in adhesives, structural composite materials, electronic semiconductor packaging and other fields. [0003] At present, the preparation process of epoxy resin is prepared by reacting phenolic hydroxyl compound with epichlorohydrin. The preparation process has a great influence on the effective utilization rate of epichlorohydrin, product yield, closed loop rate and waste water generation. With the increasingly stringent national environmental protection policies, the development of high-efficiency and green environmental protection processes has become extremely urgent. [0004] The traditional preparation process only uses alkali, such as sodium hy...

Claims

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Application Information

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IPC IPC(8): C07D301/26C07D301/28C07D303/24C07D303/27C07D303/23B01J31/02C08G59/06
CPCC07D301/26C07D301/28C07D303/23C07D303/24C07D303/27C08G59/022C08G59/063B01J31/0254B01J2231/4288Y02P20/584
Inventor 叶书怀张涛马丹李诚吉和信钟程苟明明袁凯王亮邵博文胡雪敬
Owner 江苏和和新材料股份有限公司
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