Synthesis process of 1,4-butane sultone

A technology of butane sultone and synthesis process, which is applied in the direction of organic chemistry, can solve the problems of using a large amount of organic solvents and cumbersome acidification process, and achieve the goal of reducing the process of recycling organic solvents, shortening the reaction time, and reducing by-products The effect produced

Active Publication Date: 2021-02-09
湖北吉和昌化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In view of this, it is necessary to provide a kind of synthetic technique of 1,4-butane sultone, in order to solve 1,4-butane in the prior art I

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 3-buten-1-ol (72.11g, 1mol), hydrogen peroxide (29.92g, 0.22mol) and 90g water with a mass fraction of 25% were prepared into liquid A, and sodium bisulfite (114.4g, 1.1mol) Prepare liquid B with 550g of water; at 40°C, simultaneously drop liquid A and liquid B into a 1L four-necked flask containing sodium sulfite (27.72g, 0.22mol) and 120g of water for sulfonation, and control the temperature of sulfonation 40°C; control the pH of sulfonation to 6.5-7.5, when the pH is too low, adjust the pH with sodium sulfite aqueous solution; control the addition of liquid A and liquid B at the same time in 40 minutes, and keep it warm for 2 hours to obtain the reaction liquid (intermediate product).

[0018] Concentrate the above reaction solution by rotary evaporation to viscous, then add concentrated sulfuric acid (100g, 1mol) to carry out microwave-assisted esterification reaction, after the reaction, cool down to precipitate salt, filter the filtrate to obtain crude 1,4-butanesu...

Embodiment 2

[0021] In the present embodiment, the preparation process of the intermediate product is completely consistent with that of Example 1, the difference is that:

[0022] Concentrate the above reaction solution by rotary evaporation to viscous, then add concentrated sulfuric acid (75g, 0.75mol) to carry out microwave-assisted esterification reaction, after the reaction, cool down to precipitate salt, filter the filtrate to obtain crude 1,4-butanesulfonate acid lactone. In this process, the power of the microwave is 110W, the frequency of the microwave is 2450Hz, the temperature of the microwave is 110° C., and the time of the microwave is 10 minutes.

[0023] Add 10% calcium oxide of crude 1,4-butane sultone mass to the above crude 1,4-butane sultone for acid removal, then add crude 1,4-butane sultone mass 2 times the water layer, after removing the water layer, add 10% of the mass of crude 1,4-butane sultone to the organic layer for decolorization, then filter and remove the ac...

Embodiment 3

[0025] In the present embodiment, the preparation process of the intermediate product is completely consistent with that of Example 1, the difference is that:

[0026] Concentrate the above reaction solution by rotary evaporation until viscous, then add concentrated sulfuric acid (125g, 1.25mol) to carry out microwave-assisted esterification reaction, after the reaction, cool down to precipitate salt, filter the filtrate to obtain crude 1,4-butanesulfonate acid lactone. In this process, the power of the microwave is 130W, the frequency of the microwave is 2450Hz, the temperature of the microwave is 90°C, and the time of the microwave is 30min.

[0027] Add 5% sodium hydroxide of crude 1,4-butane sultone to the above crude 1,4-butane sultone to remove acid, then add crude 1,4-butane sultone 5 times the mass of the water layer, after removing the water layer, add 2% of the mass of crude 1,4-butane sultone to the organic layer for decolorization, then filter and remove the activ...

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PUM

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Abstract

The invention discloses a synthesis process of 1,4-butane sultone. The synthesis process comprises the following steps: sulfonating 3-buten-1-ol and a sulfonating agent under the action of an initiator to obtain an intermediate product; carrying out rotary evaporation and concentration on the intermediate product until the intermediate product is viscous, adding strong acid, carrying out a microwave-assisted esterification reaction, conducting cooling to separate out salt after the reaction is finished, performing filtering, and taking a filtrate to obtain crude 1,4-butane sultone; and refining the crude 1,4-butane sultone to obtain a finished 1,4-butane sultone product. According to the invention, microwave-assisted esterification is adopted, and the strong acid is used as an acidifying reagent and a catalyst, so reaction selectivity can be improved, by-product generation can be reduced, reaction time can be shortened, and yield can be improved; and no organic solvent needs to be added in the process, so the organic solvent recovery process is avoided, and steps are simple.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a synthesis process of 1,4-butane sultone. Background technique [0002] 1,4-Butane sultone is a colorless liquid at room temperature, with a melting point of 12.5-14.5°C, a boiling point of 134-136°C (0.53kPa), and a relative density of 1.331. It is miscible with various organic solvents and insoluble in water. 1,4-butane sultone can be widely used in the production and manufacture of electroplating intermediates, pharmaceutical intermediates, photosensitive materials, lithium batteries, and daily chemicals. As 1,4-butane sultone has been developed into a wider range of applications, especially in new energy lithium battery electrolytes, its market demand is increasing. [0003] Chinese patent CN 106397392 A discloses a synthesis process of 1,4-butane sultone, which prepares 1,4-butane sultone product through sulfonation, acidification and dehydration ring closure. After refi...

Claims

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Application Information

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IPC IPC(8): C07D327/06
CPCC07D327/06Y02E60/10
Inventor 冯庆诚付远波杨威黄开伟肖忠新付启龙
Owner 湖北吉和昌化工科技有限公司
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