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The preparation method of diallyl bisphenol S ether

A diallyl bisphenol and solvent technology, which is applied in the field of preparation of diallyl bisphenol S ether, can solve the problems of unavoidable, expensive catalysts in the subsequent process of wastewater treatment, etc., and achieves increased usage and improved disposable Conversion rate, the effect of reducing product cost

Active Publication Date: 2022-05-17
ZHANGJIAKOU SIRUIKAI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method does not use solvent recovery, but there are disadvantages of subsequent processing of a large amount of waste water and expensive catalysts
[0008] From the preparation process of the above-mentioned prior art, it is unavoidable to produce a large amount of sodium chloride and potassium in the process of producing diallyl bisphenol S ether after reacting with alkali to form a salt with bisphenol S as raw material. Inorganic salt wastewater, and water or liquid caustic soda is added to the reaction, so that the impurity of bisphenol S triallyl ether will inevitably appear in the target product

Method used

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  • The preparation method of diallyl bisphenol S ether
  • The preparation method of diallyl bisphenol S ether
  • The preparation method of diallyl bisphenol S ether

Examples

Experimental program
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Effect test

Embodiment 1

[0025] In a three-neck flask with stirring, add 192 grams of diethylene glycol monomethyl ether, 24 grams of sodium hydroxide, stir for about 10 minutes, add 64 grams of bisphenol S under stirring conditions, then add 3.2 grams of catalyst, and stir for 10 minutes Finally, add 50 grams of allyl chloride, replace the environment in the kettle with nitrogen, seal the reactor, adjust the reaction temperature to 60°C, then gradually adjust the reaction temperature to 100°C, maintain the reaction temperature for 5 hours, cool to room temperature and filter, and leave the reaction mother liquor apply.

[0026] After filtering, add 250 grams of toluene to the obtained filter cake, heat and dissolve the product and then heat filter, wash the filter cake with toluene to obtain sodium chloride salt with a purity of 99%, then concentrate the mother liquor, crystallize, filter, and dry Finally, 69 grams of diallyl bisphenol S ether was obtained, with a content of 99.6% and a yield of 82%....

Embodiment 2

[0028] In the three-neck flask with stirring, add the reaction mother liquor obtained by filtering in Example 1, add 10 grams of solvent, 24 grams of sodium hydroxide, stir for about 10 minutes, add 64 grams of bisphenol S under stirring conditions, and then add the catalyst 0.2 grams, after stirring for 10 minutes, add 50 grams of allyl chloride, replace the environment in the kettle with nitrogen, seal the reactor, adjust the reaction temperature to 60°C, then gradually adjust the reaction temperature to 100°C, maintain the reaction temperature for 5 hours, and then cool down to Filter at room temperature, and keep the mother liquor for future use.

[0029] Sodium chloride and bisphenol S diallyl ether were separated from the filter cake according to the method used in Example 1. Test result: diallyl bisphenol S ether 77.7 grams, content 99.7%, yield 92%.

Embodiment 3

[0031] In the there-necked flask with stirring, add the reaction mother liquor obtained by filtering in Example 2, add 10 grams of solvent, 24 grams of sodium hydroxide, stir for about 10 minutes, add 64 grams of bisphenol S under stirring conditions, and then add the catalyst 0.1 g, after stirring for 10 minutes, add 50 g of allyl chloride, replace the environment in the kettle with nitrogen, seal the reactor, adjust the reaction temperature to 60°C, and then gradually adjust the reaction temperature to 100°C, maintain the temperature for 5 hours, cool down to room temperature and filter .

[0032] Sodium chloride and bisphenol S diallyl ether were separated from the filter cake according to the method used in Example 1. Test result: Diallyl bisphenol S ether 78.6 grams, content 99.6%, yield 93%.

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Abstract

The invention discloses a preparation method of diallyl bisphenol S ether. In an anhydrous aprotic strong polar solvent, solid base, bisphenol S and allyl chloride are added to react in the presence of a catalyst. The reaction temperature is 55°C-100°C, reaction time 7-12 hours; solid-liquid separation, and then separate diallyl bisphenol S ether and inorganic salt from the obtained filter cake; directly recycle the filtrate containing the solvent and catalyst In the next preparation of diallyl bisphenol S ether; wherein, the catalyst is a non-ionic surfactant, and the dosage is at least 5% of the weight of bisphenol S. The invention belongs to anhydrous reaction, which not only improves the one-time conversion rate of raw materials, but also does not need to recover and purify the solvent and catalyst used, and can be directly applied mechanically, so it fundamentally solves the problem of industrial wastewater, and realizes the target product and by-products high quality and high yield.

Description

technical field [0001] The invention relates to a preparation method of diallyl bisphenol S ether. Background technique [0002] Diallyl bisphenol S ether (bisphenol S diallyl ether) has a wide range of uses, and is often used as a raw material for polymer heat-resistant materials, a color developer for thermal recording materials, and a raw material for polymer flame retardants. With bisphenol S (4,4'-dihydroxydiphenyl sulfone, the molecular formula is C 12 h 10 o 4 S,) gradually replace the product bisphenol A, as the follow-up product of bisphenol S, the market demand for diallyl bisphenol S ether is increasing day by day. The synthesis method of this product is to use alcohols as solvents, under caustic alkali conditions, raise the temperature to 70-90°C, and the reaction time is more than 24 hours. Bisphenol S and 3-chlorinated propene undergo a substitution reaction to form diallyl bis Phenol S ether, the yield is about 92%, the product purity is relatively low, an...

Claims

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Application Information

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IPC IPC(8): C07C315/04C07C317/22
CPCC07C315/04C07C317/22Y02P20/584
Inventor 郭明堂刘建高占德郭志新
Owner ZHANGJIAKOU SIRUIKAI TECH
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