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Method for preparing ethylene sulfate

A technology of vinyl sulfate and ethylene glycol, applied in organic chemistry and other directions, can solve the problems of unsatisfactory acid value and moisture content, low molar yield, and many three wastes, etc., and achieve low acid value of products, short reaction routes, and safety. high effect

Active Publication Date: 2019-05-21
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

[0004] The invention provides a preparation method of vinyl sulfate, which aims to overcome the high cost, low molar yield, low purity, unsatisfactory acid value and moisture content of existing vinyl sulfate preparation methods in the prior art, and excessive three wastes. Not enough

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of preparation method of vinyl sulfate, it comprises the steps:

[0022] (1) Synthesis of vinyl sulfate

[0023] Add 200g of ethylene glycol into the four-neck flask, start stirring, add 1000mL of chloroform to the reaction flask, and slowly add 457g of sulfuryl chloride dropwise at room temperature (the molar ratio of ethylene glycol to sulfuryl chloride is 1:1.05) , control the drop rate of sulfonyl chloride so that the reaction temperature in the reactor does not exceed 30°C, the temperature of the reaction solution rises obviously when the dropwise addition is just started, and when the sulfonyl chloride added dropwise is half of the total amount, the temperature of the reaction solution begins to drop After the sulfuryl chloride was added dropwise, the temperature of the reaction solution dropped to 5°C. The sulfuryl chloride was added dropwise for 1.5 hours, and the color of the reaction solution changed from colorless to light yellow during the reaction. ...

Embodiment 2

[0027] A kind of preparation method of vinyl sulfate, it comprises the steps:

[0028] (1) Synthesis of vinyl sulfate

[0029] Add 200g of ethylene glycol into the four-necked flask, start stirring, add 900mL of chloroform to the reaction flask, and slowly add 521g of sulfonyl chloride dropwise at room temperature (the molar ratio of ethylene glycol to sulfonyl chloride is 1:1.2) , control the drop rate of sulfonyl chloride so that the reaction temperature in the reactor does not exceed 30°C, the temperature of the reaction solution rises obviously when the dropwise addition is just started, and when the sulfonyl chloride added dropwise is half of the total amount, the temperature of the reaction solution begins to drop After the sulfuryl chloride was added dropwise, the temperature of the reaction solution dropped to 5°C. The sulfuryl chloride was added dropwise for 1.5 hours, and the color of the reaction solution changed from colorless to light yellow during the reaction. ...

Embodiment 3

[0033] A kind of preparation method of vinyl sulfate, it comprises the steps:

[0034] (1) Synthesis of vinyl sulfate

[0035] Add 200g of ethylene glycol into the four-neck flask, start stirring, add 1100mL of chloroform to the reaction flask, and slowly add 435g of sulfuryl chloride dropwise at room temperature (the molar ratio of ethylene glycol to sulfuryl chloride is 1:1) , control the drop rate of sulfonyl chloride so that the reaction temperature in the reactor does not exceed 30°C, the temperature of the reaction solution rises obviously when the dropwise addition is just started, and when the sulfonyl chloride added dropwise is half of the total amount, the temperature of the reaction solution begins to drop After the sulfuryl chloride was added dropwise, the temperature of the reaction solution dropped to 5°C. The sulfuryl chloride was added dropwise for 1.5 hours, and the color of the reaction solution changed from colorless to light yellow during the reaction. Th...

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Abstract

The invention relates to a method for preparing ethylene sulfate. The method comprises the following steps: S1, carrying out a nucleophilic substitution reaction: carrying out the nucleophilic substitution reaction on ethylene glycol and sulfonyl chloride, which are used as starting raw materials, with trichloromethane as solvent to obtain crude ethylene sulfate; and S2, refining and purifying: dissolving the crude ethylene sulfate in trichloromethane, heating and refluxing the obtained solution under the protection of nitrogen to completely dissolve the crude ethylene sulfate, performing cooling recrystallization, performing filtration, and carrying out reduced pressure drying on the obtained filter cake to obtain the crude ethylene sulfate. Compared with the prior art, the method for preparing the ethylene sulfate from the ethylene glycol and sulfonyl chloride through a one-step reaction without a catalyst has the advantages of short reaction route, mild reaction conditions, simple synthesis process, easiness in operation, high safety, simple and easily-available raw materials, low cost and few byproducts; and the prepared product has the advantages of high purity, low moisture content, low acid value, and suitableness for being industrially produced.

Description

technical field [0001] The invention relates to a preparation method of a sulfuric acid ester compound vinyl sulfate, an electrolyte additive for lithium batteries, and belongs to the technical field of preparation of electrolyte additive compounds for lithium batteries. Background technique [0002] Lithium-ion batteries are widely used due to their incomparable advantages such as small size, good safety performance, light weight, high specific performance, high voltage, long life, and no pollution. In recent years, with the rapid development of my country's new energy vehicle market, the demand for power lithium batteries has increased significantly. With the continuous improvement of the market's energy performance requirements for lithium batteries, the research and development of lithium ion battery electrolytes and functional additives has attracted much attention. [0003] The structure of sulfuric acid ester compounds is very similar to the new additives of lithium b...

Claims

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Application Information

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IPC IPC(8): C07D327/10
Inventor 宋朝阳王靖陈亮刘淑君张秀丽徐莱陈立霞
Owner 武汉松石科技股份有限公司
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