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1. CN111533728 - Preparation method of ethylene sulfate

Office
China
Application Number 202010649010.3
Application Date 08.07.2020
Publication Number 111533728
Publication Date 14.08.2020
Grant Number 111533728
Grant Date 13.10.2020
Publication Kind B
IPC
C07D 327/10
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
DHETEROCYCLIC COMPOUNDS
327Heterocyclic compounds containing rings having oxygen and sulfur atoms as the only ring hetero atoms
10two oxygen atoms and one sulfur atom, e.g. cyclic sulfates
CPC
C07D 327/10
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
DHETEROCYCLIC COMPOUNDS
327Heterocyclic compounds containing rings having oxygen and sulfur atoms as the only ring hetero atoms
10two oxygen atoms and one sulfur atom, e.g. cyclic sulfates
Applicants DONGYING HI-TECH SPRING CHEMICAL INDUSTRY CO., LTD.
东营市海科新源化工有限责任公司
Inventors YAN ZENGWEI
燕增伟
WU LEILEI
吴雷雷
LIN HAI
林海
CHEN KAIDI
陈凯迪
Agents 青岛清泰联信知识产权代理有限公司 37256
Title
(EN) Preparation method of ethylene sulfate
(ZH) 硫酸乙烯酯的制备方法
Abstract
(EN) The invention discloses a preparation method of ethylene sulfate, and belongs to the technical field of lithium ion battery electrolyte additives. The method comprises the following steps: 1) dropwiseadding ethylene glycol into thionyl chloride, heating to 50-80 DEG C, keeping the temperature for 2-4 hours, and vacuumizing to obtain a reaction solution containing ethylene sulfite; 2) rectifying and purifying the reaction solution containing the ethylene sulfite under a vacuum condition; 3) mixing the ethylene sulfite with the purity of more than 99.2% with dichloroethane, dropwise adding a sodium hypochlorite solution into the mixed solution, stirring after dropwise adding, and standing to obtain an organic phase; 4) adjusting the pH value of the organic phase to 7-8, adding a catalyst, dropwise adding a sodium hypochlorite solution to perform an oxidation reaction, keeping the temperature for 1-1.5 h, and performing standing and liquid separation to obtain an ethylene sulfate crude product, and 5) dehydrating the ethylene sulfate crude product, recrystallizing and drying to obtain ethylene sulfate. The ethylene sulfate prepared by the method is high in yield and high in purity.
(ZH) 本发明公开了硫酸乙烯酯的制备方法,属于锂离子电池电解液添加剂技术领域。所述方法包括:1)将乙二醇滴加至二氯亚砜中,升温至50~80℃保温2~4h,进行抽真空处理,得到含亚硫酸乙烯酯的反应液;2)将含亚硫酸乙烯酯的反应液在真空条件下精馏提纯;3)将纯度大于99.2%的亚硫酸乙烯酯和二氯乙烷混合,在混合液中滴加次氯酸钠溶液,滴加完成后进行搅拌、静置,得到有机相;4)调节有机相的pH值至7~8后加入催化剂,滴加次氯酸钠溶液进行氧化反应,保温1~1.5h,静置分液,得到硫酸乙烯酯粗品;5)将硫酸乙烯酯粗品进行脱水、重结晶和干燥,得到硫酸乙烯酯。本发明提供的方法硫酸乙烯酯收率高、纯度高。
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