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Method for preparing bisphenol S allyl ether

A technology of bisallyl ether and allyl ether, which is applied in the field of preparation of aromatic sulfone organic compounds, can solve the problems that are not conducive to the improvement of single-line production capacity and economic benefits, slow reaction speed, waste alkali pollution, etc., and achieve Easy to control, high product yield, environment-friendly effect

Inactive Publication Date: 2011-11-23
JILIN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The amount of alkali used in this technology is large, and it 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
[0009] In the above methods, only DAE is generated, but no ABE is generated

Method used

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  • Method for preparing bisphenol S allyl ether
  • Method for preparing bisphenol S allyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In a 50L reactor, add 20kg of bisphenol S, add 20% sodium hydroxide solution until the pH value is 10.7, stir, heat to dissolve, add 0.2kg of tetrabutylammonium bromide, slowly drop 2.5kg of allyl chloride, Heat to reflux (60°C) for 5 hours. Filter after cooling to recover tetrabutylammonium bromide. After the filtrate is statically stratified, liquid separation is carried out, the upper layer is the organic phase, and the lower layer is the aqueous phase. The pH of the aqueous phase was adjusted to 9.1 with 60% sulfuric acid solution, and solids were precipitated. The crude product of ABE was obtained by filtration, and purified by recrystallization with 5 kg of 25% ethanol. The solid product obtained after drying was ABE (4.8 kg). The organic phase was washed with water until neutral, heated to reflux, filtered after cooling to obtain a solid, and DAE (15.7kg) was obtained after drying. Filtrate recovery.

Embodiment 2

[0035] The tetrabutylammonium bromide reclaimed in embodiment 1 is tested again by the scheme of embodiment 1, obtains 15.2kg DAE and 5.1kg ABE.

Embodiment 3

[0037] Cetyltrimethylammonium chloride was used to replace tetrabutylammonium bromide in Example 1, and the test was carried out according to the scheme of Example 1 to obtain 15.7kg DAE and 4.9kg ABE.

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Abstract

The invention belongs to the field of preparation of aromatic sulfones organic compounds, and in particular relates to a method for preparing bisphenol S allyl ether (including bisphenol S diallyl ether and bisphenol S monoallyl ether). The method provided by the invention comprises the following steps of: (1) carrying out an etherification reaction: heating and reflowing bisphenol S and allyl halides in an alkaline solution to react for 1-8 hours under the effect of a phase transferring catalyst; (2) recycling the catalyst; (3) separating diallyl ether (DAE) and allyl bisphenol ether (ABE); (4) refining the DAE; and (5) refining the ABE. The method disclosed by the invention has the advantages of simpleness in operation, convenience for recycling the catalyst and the solvent, environment friendliness, high product yield and purity and low manufacturing cost; and the method is suitable for the industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic sulfone organic compounds, in particular to a preparation method of bisphenol S allyl ether (including bisphenol S diallyl ether and bisphenol S monoallyl ether). Background technique [0002] In the following instructions, bisphenol S (4,4'-dihydroxydiphenyl sulfone, CAS: 80-09-1) is represented by BPS, bisphenol S diallyl ether is represented by DAE, bisphenol S monoallyl Base ethers are represented by ABE. [0003] DAE and ABE molecules have heat resistance due to the aromatic sulfone structure, which can improve the heat resistance of other materials, and are mainly used as sensitizers for thermosensitive recording materials. Both DAE and ABE molecules contain double bond groups, which are important monomers for the synthesis of allyl polymers, and are widely used in the fields of new optical materials, resin materials and high-strength materials. DAE is also a raw material for the pre...

Claims

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Application Information

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IPC IPC(8): C07C317/22C07C315/04
CPCY02P20/584
Inventor 贾树勇徐占林任玉荣杨爽赖晓红吕爽
Owner JILIN NORMAL UNIV
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