A kind of synthetic method of high-purity 1,4-butane sultone

Abstract

The invention discloses a method for synthesizing high-purity 1,4-butane sultone. The steps are as follows: 1. Add 4-chlorobutanol and sodium sulfite solution into an alcohol solvent, heat up to reflux for 6 hours, After the reflux is completed, the mixed solution A is obtained. Concentrate the mixed solution A to recover the alcohol solvent, then add hydrochloric acid to acidify, concentrate until the material becomes viscous, then add the alcohol solvent, precipitate sodium chloride crystals, filter, and concentrate the filtrate to recover the alcohol Solvent to obtain 4-hydroxybutanesulfonic acid; 2. Continuous flash dehydration of 4-hydroxybutanesulfonic acid at a vacuum degree of 1-8mmHg and a temperature of 130-165°C to obtain industrial grade 1,4-butane 3. Add azeotrope to industrial grade 1,4-butane sultone, and recover the azeotrope by fractional distillation at normal pressure, then carry out fractional distillation under reduced pressure at a vacuum of 2-4mmHg, and collect 120 ‑121 °C fraction to obtain high-purity 1,4‑butane sultone. The method is simple and environment-friendly, greatly improves the sulfonation yield, and greatly improves the purity and yield of 1,4-butane sultone.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing high-purity 1,4-butane sultone. Background technique [0002] 1,4-Butane sultone is a sulfonating agent, mainly used to synthesize biological buffers and sulfonic acid resins. In recent years, 1,4-butane sultone has gained attention because it can be used as a lithium battery additive. [0003] The report on the synthesis of 1,4-butane sultone was first seen in the 1950s. It was synthesized by dehydrochlorination and cyclization of 4-chlorosulfonyl chloride and copper oxide at 150-160 °C, see DE860637. Later, 1,4-butane sultone was synthesized by dehydration of 4-hydroxybutanesulfonic acid, see DE887341. This method is simple and convenient, and has become the main method for synthesizing 1,4-butane sultone, so the preparation of 4- Hydroxybutanesulfonic acid becomes the key to the synthesis of 1,4-butane sultone. There are also many methods...

AI Technical Summary

Problems solved by technology

Using tetrahydrofuran and acetyl chloride to synthesize 4-chlorobutanol acetate under the catalysis of Lewis acid is a safe and applicable method, but the disadvantage is that 1,4-dichlorobutane and 1,4-butanediol di Acetate and other by-products, so the yield is <80%

The sulfonation of 4-chlorobutanol acetate and sodium sulfite will produce sodium chloride and sodium acetate, and the separation of sodium chloride and sodium acetate is difficult, resulting in environmental problems

[0005] Another method sees sulfonation of 4-chlorobutanol and sodium sulfite to synthesize sodium 4-hydroxybutanesulfonate and then acidifies it into 4-hydroxybutanesulfonic acid. This route has no patent report, but it is in An.chan.Soc. 76 5357-60 19 reported that 4-chlorobutanol was reacted with sodium sulfite solution for 7 days to obtain sodium 4-hydroxybutanesulfonate, but the yield was extremely low, only 58%