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Chemical synthesis method for improving reaction rate and yield of bisphenol S monoallyl ether

A monoallyl ether, reaction rate technology, applied in the field of chemical synthesis, can solve the problems of slow reaction speed, large amount, waste alkali pollution, etc., to reduce the difficulty of refining, improve the specificity and rate of the reaction, and increase the yield Effect

Inactive Publication Date: 2021-03-12
XIAN WONDER SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current preparation technology uses a large amount of alkali, which is easy to cause waste alkali pollution
In addition, the reaction speed is slow, which is not conducive to the improvement of single-line production capacity and economic benefits

Method used

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  • Chemical synthesis method for improving reaction rate and yield of bisphenol S monoallyl ether
  • Chemical synthesis method for improving reaction rate and yield of bisphenol S monoallyl ether
  • Chemical synthesis method for improving reaction rate and yield of bisphenol S monoallyl ether

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Effect test

preparation example Construction

[0019] Such as Figure 1~4 Shown, a kind of chemical synthesis method that improves bisphenol S monoallyl ether reaction rate and yield may further comprise the steps:

[0020] Step (1). Add 500 grams of water, 1500 grams of organic solvent, 350-400 grams of BPS, 225-260 grams of liquid caustic soda and 5-10 grams of catalyst into the reaction flask in turn, and stir evenly;

[0021] Step (2). Add 145-165 grams of chloropropene, heat to 75-80 ° C, react for 2 hours, take a sample for detection, and the reaction ends;

[0022] Step (3). Slowly adjust the pH to 7 with hydrochloric acid;

[0023] Step (4). Lower the temperature to 25°C, stir and crystallize for 2 hours; obtain the crude product by suction filtration;

[0024] Step (5). The crude product is dissolved in 200-350ml of organic solvent and 200-350ml of water, heated to reflux to dissolve, cooled to 25°C, stirred and crystallized for 3 hours, suction filtered to obtain the finished product, and dried to obtain the pr...

Embodiment 1

[0028] Implementation 1: Add 500 grams of water, 1,500 grams of organic solvent, 350 grams of BPS, 225 grams of liquid caustic soda and 5 grams of catalyst into the reaction flask in sequence, and stir evenly; add 145 grams of allyl chloride, heat to 80°C, react for 2 hours, and take samples for detection , the reaction is over; the pH is slowly adjusted to 7 with hydrochloric acid; the temperature is lowered to 25°C, stirred and crystallized for 2 hours; the crude product is obtained by suction filtration; the crude product is dissolved in 200ml of ethanol and 200ml of water, heated to reflux to dissolve, cooled to 25°C, stirred and crystallized for 2 hours Hour, suction filtration obtains finished product, obtains product 390 grams after oven dry; Calculate with BPS, molar yield 96.0%; Wherein catalyzer is tetrabutylammonium iodide and sodium iodide mass ratio (5~1): (1~5 ) mixture, see attached figure 1 .

Embodiment 2

[0029] Implementation 2: Add 500 grams of water, 1500 grams of organic solvent, 350 grams of BPS, 225 grams of liquid caustic soda and 10 grams of catalyst into the reaction flask in sequence, and stir evenly; add 145 grams of chloropropene, heat to 79 ° C, react for 2 hours, and take samples for detection , the reaction is over; slowly adjust the pH to 7 with hydrochloric acid; cool down to 25°C, stir and crystallize for 2 hours; suction filter to obtain the crude product; dissolve the crude product in 200ml of isopropanol and 200ml of water, heat to reflux to dissolve, cool to 25°C, stir and crystallize After 2 hours, the finished product was obtained by suction filtration, and 388 grams of the product were obtained after drying; calculated by BPS, the molar yield was 95.6%. Wherein the catalyst is a mixture of tetrabutylammonium iodide and sodium iodide mass ratio (5-1): (1-5), the purity is detailed in the attached figure 2 .

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Abstract

The invention provides a chemical synthesis method for improving the reaction rate and yield of bisphenol S monoallyl ether, and the method comprises the following steps: (1) sequentially adding 500gof water, 1,500g of organic solvent, 350-400g of BPS, 225-260g of caustic soda liquid and 5-10g of catalyst into a reaction bottle, and performing uniform stirring; (2) adding 145-165 g of chloropropene, performing heating to 75-80 DEG C, performing reacting for 2 hours, performing sampling and detecting, and finishing the reaction; (3) slowly adjusting the pH value to 7 by using hydrochloric acid; (4) performing cooling to 25 DEG C, performing stirring and crystallizing for 2 hours, and performing suction filtration to obtain a crude product; (5) dissolving the crude product in 200-350ml of an organic solvent and 200-350ml of water, carrying out heating reflux dissolution, performing cooling to 25 DEG C, carrying out stirring crystallization for 3h, carrying out suction filtration to obtain a finished product, and performing drying to obtain the product. According to the method, a reasonable catalyst is used, so that the reaction specificity and speed of bisphenol S and chloropropeneare greatly improved, the yield of the product is greatly increased, the refining difficulty of the product is reduced, and meanwhile, a high-purity product can be obtained.

Description

technical field [0001] The invention relates to the field of chemical synthesis methods, in particular to a chemical synthesis method for improving the reaction rate and yield of bisphenol S monoallyl ether. Background technique [0002] Bisphenol S (4,4'-dihydroxydiphenyl sulfone, CAS: 80-09-1) is represented by BPS. The aromatic sulfone monomer has hydrolysis resistance, high stability of electrical properties, small shrinkage during molding processing, and excellent Heat resistance, chemical stability, and nuclear radiation resistance have been widely used in the fields of electronic microelectronics and aerospace. The current preparation technology uses a large amount of alkali, which is easy to cause waste alkali pollution. In addition, the reaction speed is slow, which is not conducive to the improvement of single-line production capacity and economic benefits. Contents of the invention [0003] The technical problem to be solved by the present invention is to prov...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/22C07C315/04
CPCC07C315/04C07C317/22
Inventor 王传宝刘立强
Owner XIAN WONDER SCI & TECH
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