Method for synthetizing 2, 4-butane sulfonic acid lactone

A kind of technology of butane sultone and synthesis method, which is applied in the field of preparation method of sultone derivatives, and can solve the problems of complicated process and low yield, etc.

Inactive Publication Date: 2012-12-05
FUJIAN CHUANGXIN TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] However, the synthesis reaction requires high-pressure hydrogenation reduction, the process is relatively complicated, and the yield is low

Method used

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  • Method for synthetizing 2, 4-butane sulfonic acid lactone
  • Method for synthetizing 2, 4-butane sulfonic acid lactone
  • Method for synthetizing 2, 4-butane sulfonic acid lactone

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add 252 grams (2mol) of anhydrous sodium sulfite and 500ml water into a 1000ml three-necked flask equipped with a stirrer and a thermometer, and stir until they are evenly mixed. Control the reaction temperature not to exceed 50°C, the pH value is 6.5, and ensure the presence of sodium sulfite and sodium bisulfite in the system, add a mixed solution of 72 grams (1mol) of butenol and 20ml of sulfuric acid dropwise within 2 hours, dropwise After completion, continue to stir for 30 minutes, then adjust the pH value to 3.0, concentrate the reaction solution, cool, filter to remove crystalline sodium sulfate, and wash with absolute ethanol several times, combine the filtrate and washing solution to form sodium hydroxybutanesulfonate aqueous solution.

[0022] Add 90ml of concentrated hydrochloric acid and 200ml of absolute ethanol to the aqueous solution of sodium hydroxybutane sulfonate, stir for 15 minutes and freeze in a freezer to 0°C, filter to remove the precipitated s...

Embodiment 2

[0025] Add 150 g (1.5 mol) of anhydrous sodium bisulfite and 500 ml of water into a 1000 ml three-neck flask equipped with a stirrer and a thermometer, so that the sodium bisulfite and water are fully miscible. Control the reaction temperature not to exceed 50°C, and the pH value is 6.5. Add 72 grams (1mol) of butenol solution dropwise within 2 hours. After the dropwise addition, continue to stir for 30 minutes. After adjusting the pH value to 3.0, the reaction solution is Concentrate, cool, filter to remove crystalline sodium sulfate, and wash several times with absolute ethanol. The filtrate and the washing solution are combined to form an aqueous solution of sodium hydroxybutane sulfonate.

[0026] Add 90ml of concentrated hydrochloric acid and 200ml of absolute ethanol to the aqueous solution of sodium hydroxybutane sulfonate, stir for 15 minutes, place in a freezer to freeze to 0°C, remove the precipitated sodium chloride by filtration, and wash the sodium chloride crysta...

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PUM

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Abstract

The invention relates to a method for preparing 2, 4-butane sulfonic acid lactone by using butenol (crotyl alcohol) as raw materials, sulfonating the butenol to be hydroxy butane sulfonate with hydrosulphite, acidizing the hydroxy butane sulfonate to be hydroxy butane sulfonic acid, and finally dehydrating in vacuum at high temperature. The method is low in cost, mild in conditions, simple and convenient to operate, easy to control and high in yield, and is a synthetizing process suitable for industrialization, and raw materials are easy to obtain.

Description

technical field [0001] The invention relates to a method for preparing sultone derivatives, in particular to a method for synthesizing 2,4-butane sultone. Background technique [0002] Derivatives of sultones such as amines, alcohols, phenols, thiols, and thiamines are very effective detergents, lubricants, foaming agents, antibacterial agents, and antistatic additives for polyamide fibers, and are widely used in dyes Gluing and dyeing and finishing in industrial and textile industries, additives for photosensitive materials and lithium-ion battery electrolytes, etc. [0003] 2,4-butane sultone is a typical sulfoalkylation reagent. According to different starting materials, there are generally two methods for preparing 2,4-butane sultone: [0004] (1) Synthetic route using butylene chloride as raw material: [0005] First, sulfur dioxide is used to sulfonate butene into chlorobutanesulfonic acid, and finally dehydrochlorination and cyclization into 2,4-butane sultone. The ...

Claims

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Application Information

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IPC IPC(8): C07D327/04
Inventor 黄当睦吴茂祥刘新平
Owner FUJIAN CHUANGXIN TECH DEV CO LTD
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