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Preparation method of 2,4-butanesultone

A technology of butanesulfonic acid and hydroxybutanesulfonic acid, which is applied in the direction of organic chemistry, can solve the problems of inconvenient industrial continuous production, harsh reaction conditions, and complicated reaction steps, and achieve low cost, mild and stable reaction conditions, and high reaction speed. fast effect

Pending Publication Date: 2022-02-22
武汉松石科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is to provide a preparation method of 2,4-butane sultone, aiming at overcoming the complicated reaction steps, There are many problems such as harsh reaction conditions, inconvenient industrial continuous production, and low yield due to impurities generated during sulfonation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The preparation method of 2,4-butane sultone comprises the steps:

[0029] A, 2-butenol and sodium bisulfite aqueous solution (15wt%) are dropped into the reaction vessel and fully mixed, and the mol ratio of 2-butenol and sodium bisulfite is 1:1.2, and the catalyst sodium nitrate aqueous solution ( The concentration of sodium nitrate is 40wt%, and the amount of sodium nitrate is 0.5% of the mass of 2-butenol), and the temperature rises and refluxes under stirring conditions, and free radical addition reaction occurs, and the reaction temperature is controlled to be 70° C., and the pH value is between 6-7. The reaction time was 3 hours, and after the reaction was completed, it was cooled to room temperature to obtain the intermediate 3-hydroxybutanesulfonic acid sodium salt solution;

[0030] B. Using ion exchange process, the 3-hydroxybutanesulfonate solution in A is acidified with styrene-based cation exchange resin to obtain 3-hydroxybutanesulfonic acid, and the dehy...

Embodiment 2

[0033] The preparation method of 2,4-butane sultone comprises the steps:

[0034] A, 2-butenol and sodium bisulfite aqueous solution (25wt%) are dropped into the reaction vessel and fully mixed, and the mol ratio of 2-butenol and sodium bisulfite is 1:1.5, and the catalyst sodium nitrate aqueous solution ( The concentration of sodium nitrate is 25wt%, and the amount of sodium nitrate is 1.0% of the mass of 2-butenol), and the temperature rises and refluxes under stirring conditions, and free radical addition reaction occurs, and the reaction temperature is controlled to be 80° C., and the pH value is between 6-7. The reaction time was 4 hours, and after the reaction was completed, it was cooled to room temperature to obtain the intermediate 3-hydroxybutanesulfonic acid sodium salt solution;

[0035] B. Using ion exchange process, the 3-hydroxybutanesulfonate solution in A is acidified with styrene-based cation exchange resin to obtain 3-hydroxybutanesulfonic acid, and the dehy...

Embodiment 3

[0038] The preparation method of 2,4-butane sultone comprises the steps:

[0039]A, 2-butenol and sodium bisulfite aqueous solution (30wt%) are dropped into the reaction vessel and fully mixed, and the mol ratio of 2-butenol and sodium bisulfite is 1:2.0, and the catalyst sodium nitrate aqueous solution ( The concentration of sodium nitrate is 30wt%, and the amount of sodium nitrate is 2.0% of the mass of 2-butenol), and the temperature rises and refluxes under stirring conditions, and free radical addition reaction occurs, and the reaction temperature is controlled to be 90° C., and the pH value is between 6-7. The reaction time was 5 hours, and after the reaction was completed, it was cooled to room temperature to obtain the intermediate 3-hydroxybutanesulfonic acid sodium salt solution;

[0040] B. Using ion exchange technology, the 3-hydroxybutanesulfonate solution in A is acidified with styrene-based cation exchange resin to obtain 3-hydroxybutanesulfonic acid, and the de...

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Abstract

The invention relates to a preparation method of 2,4-butanesultone. The preparation method comprises the following steps: A, with 2-butenol and an aqueous sodium hydrogen sulfite solution as raw materials and an aqueous sodium nitrate solution as a catalyst, carrying out heating reflux reaction under a stirring condition to obtain a solution containing sodium 3-butanediol sulfonate; B, acidifying the solution with ion exchange resin, adding a dehydrating agent, carrying out distilling under normal pressure to remove water and a dehydrating agent, then performing reduced-pressure distillation, and collecting a 3-butanediol sulfonic acid fraction; and C, carrying out continuous flash evaporation dehydration cyclization on a 3-butanediol sulfonic acid concentrated solution under a high-temperature vacuum condition to obtain 2,4-butanesultone. The method has the advantages of simple process route, mild conditions, cheap and easily available reaction substrates and catalysts, adoption of resin acidification, guarantee of continuous production, reduction in loss and production cost of intermediate reaction links, simple post-treatment, and realization of target product yield of 80% or more.

Description

technical field [0001] The invention belongs to the field of synthesis of fine chemical intermediates, and in particular relates to a preparation method of 2,4-butane sultone. Background technique [0002] 2,4-Butane sultone is a colorless or light yellow-red transparent liquid at room temperature, with a flash point of 93°C, a boiling point of 150°C (1.6kPa), and a relative density of 1.31. It is insoluble in water and can be mixed with various organic solvents. Miscible. 2,4-Butane sultone is an organic sulfoalkylation reagent and fine chemical intermediate with important application prospects, which can be used in the synthesis of (gemini) surfactants, photosensitive materials, pharmaceutical intermediates, color dyes Sensitive agents and daily chemicals, etc. In recent years, 2,4-butane sultone has become increasingly active in the fields of electroplating intermediate synthesis and lithium-ion battery additives, especially as a secondary lithium-ion battery additive, ...

Claims

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Application Information

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IPC IPC(8): C07D327/04
CPCC07D327/04
Inventor 宋朝阳杨磊张章潘菲石国林谭鹏
Owner 武汉松石科技股份有限公司
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