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A method for preparing 1,3-propane sultone from 3-hydroxypropanesulfonic acid

A technology of hydroxypropanesulfonic acid and propane sultone, which is applied in the field of propane sultone preparation, can solve the problems of prolonged reaction time and low yield, and achieves the advantages of reducing carbonization loss, improving product purity, and reducing distillation operations. Effect

Active Publication Date: 2022-04-08
常熟聚和化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is also reported that adding water-carrying agent during the reaction is carried out, although adding water-carrying agent can reduce the reaction temperature, but the reaction time is also extended accordingly
And above-mentioned two kinds of cyclization liquids only obtain propane sultone crude product through distillation operation, and yield is lower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for preparing 1,3-propane sultone by 3-hydroxypropanesulfonic acid, comprising the steps of:

[0026] Mix 100 parts of 3-hydroxypropanesulfonic acid, 0.01 part of hydroxyanisole, 0.01 part of phenothiazine, 0.01 part of inhibitor 701 and 0.01 part of inhibitor 501, then heat to 120°C for cyclization reaction, and the reaction time is 2 hours , -0.09Mpa to monitor the cyclization rate of more than 96%, stop the reaction, cool the reaction system to 25 ° C, add 30 parts of pure water, stir at 40 ° C for 1 h, let stand for 1 h and separate the layers, take the lower layer at 60-90 ° C Concentrate and remove water to obtain propane sultone.

[0027] The purity of the obtained propane sultone detected by GC was 99.909%, and the yield was 84.7%.

Embodiment 2

[0029] A method for preparing 1,3-propane sultone by 3-hydroxypropanesulfonic acid, comprising the steps of:

[0030] Mix 100 parts of 3-hydroxypropanesulfonic acid, 0.01 part of hydroxyanisole, 0.01 part of phenothiazine, 0.01 part of polymerization inhibitor 701 and 2 parts of polymerization inhibitor 501, then heat to 120°C for cyclization reaction, and the reaction time is 2h , -0.09Mpa to monitor the cyclization rate of more than 96%, stop the reaction, cool the reaction system to 25 ° C, add 30 parts of pure water, stir at 40 ° C for 1 h, let stand for 1 h and separate the layers, take the lower layer at 60-90 ° C Concentrate and remove water to obtain propane sultone.

[0031] The purity of the obtained propane sultone detected by GC was 99.915%, and the yield was 86.6%.

Embodiment 3

[0033] A method for preparing 1,3-propane sultone by 3-hydroxypropanesulfonic acid, comprising the steps of:

[0034] Mix 100 parts of 3-hydroxypropanesulfonic acid, 0.01 part of hydroxyanisole, 0.01 part of phenothiazine and 0.01 part of polymerization inhibitor 701, then heat to 120°C for cyclization reaction, the reaction time is 2h, and the cyclization is monitored at -0.09Mpa When the reaction rate exceeds 96%, stop the reaction, cool the reaction system to 25°C, add 30 parts of pure water, stir at 40°C for 1 hour, let it stand for 1 hour, then separate and separate layers, take the lower layer and concentrate at 60-90°C to remove water. propane sultone.

[0035] The purity of the obtained propane sultone detected by GC was 99.902%, and the yield was 80.3%.

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PUM

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Abstract

The invention belongs to the technical field of preparation of hydroxypropane sultone, and in particular relates to a method for preparing 1,3-propane sultone from 3-hydroxypropanesulfonic acid. The method comprises the steps of: mixing 3-hydroxypropanesulfonic acid, hydroxyanisole, phenothiazine and a polymerization inhibitor, heating to undergo a cyclization reaction, and stopping the reaction when the monitored cyclization rate exceeds 96%, wherein the polymerization inhibitor The addition amount of agent is equivalent to 0.02-2% by weight of 3-hydroxypropanesulfonic acid. In this patent, one or more mixed polymerization inhibitors are added to the cyclization section to reduce the cyclization between 1,3-propane sultone molecules, which is beneficial to improve product purity and yield.

Description

technical field [0001] The invention belongs to the technical field of propane sultone preparation, and in particular relates to a method for preparing 1,3-propane sultone from 3-hydroxypropanesulfonic acid. Background technique [0002] 1,3-Propane sultone is an important intermediate in organic synthesis. Due to its chemical structure, it has strong reactivity with organic substances such as alcohols, phenols, mercaptans, and amines, and alcoholysis or aminolysis occurs. , is an important raw material for the synthesis of cationic or zwitterionic surfactants, and has been widely used in dye finishing agents, copper plating polishing agents and finishing additives, photosensitive materials, tanning, ink, medicine and other fields. It can also be used in the synthesis of polycarbonate fire retardant, lubricating grease thickener, polypropylene antistatic agent, polyethyleneimine crosslinking agent, sulfonating agent, etc. [0003] At present, the dehydration route of 3-hydr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 徐晓峰陈娓曹广宇
Owner 常熟聚和化学有限公司