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Preparation method of ethylene sulfate

A technology of vinyl sulfate and diethyl sulfate, applied in the field of preparation of vinyl sulfate, can solve problems such as potential safety hazards for operators, unfavorable industrial application, increase post-processing steps, etc., and achieves elimination of potential safety hazards and low production cost. , the effect of cheap raw materials

Active Publication Date: 2018-10-02
SUZHOU HUAYI NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this patent provides a one-pot method for preparing vinyl sulfate, this method will generate a large amount of hydrogen chloride gas, which will cause great corrosion to the equipment, and will increase the post-processing steps, making the process relatively complicated, and the waste gas will also cause serious damage to the operators. The safety brings great hidden dangers, and at the same time, the relatively expensive rare metal ruthenium catalyst is used, which makes the production cost higher, which is not conducive to industrial application

Method used

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  • Preparation method of ethylene sulfate

Examples

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Effect test

Embodiment 1

[0024] Add ethylene glycol (620g, 10mol) and diethyl sulfate (1540g, 10mol) into a 2L three-necked flask connected with a distillation head and a condenser, add lithium hydroxide (1.2g, 0.05mol), and heat to 35°C , adjust the vacuum degree to 50mmHg, and stir until no ethanol flows out. Cool down to room temperature, add methyl tert-butyl ether until a solid precipitates, cool to 0°C, a large amount of solid precipitates, filter, and recrystallize the filter residue with dichloromethane to obtain 669g of vinyl sulfate, the yield is 54%, and the purity is greater than 99% %.

Embodiment 2

[0026] Add ethylene glycol (620g, 10mol) and diethyl sulfate (1617g, 10.5mol) into a 2L three-neck flask connected with a distillation head and a condenser, add sodium methoxide (2.7g, 0.05mol), and heat to 35°C , adjust the vacuum degree to 50mmHg, and stir until no ethanol flows out. Cool down to room temperature, add methyl tert-butyl ether until a solid precipitates, cool to 0°C, a large amount of solid precipitates, filter, and recrystallize the filter residue with dichloromethane to obtain 459 g of vinyl sulfate, the yield is 37%, and the purity is greater than 99 %.

Embodiment 3

[0028] Add ethylene glycol (620g, 10mol) and diethyl sulfate (1617g, 10.5mol) into a 2L three-necked flask connected with a distillation head and a condenser, add lithium hydroxide (0.6g, 0.025mol), and heat to 35 °C, adjust the vacuum degree to 50mmHg, and stir until no ethanol flows out. Cool down to room temperature, add methyl tert-butyl ether until a solid precipitates, cool to 0°C, a large amount of solid precipitates, filter, and recrystallize the filter residue with dichloromethane to obtain 768g of vinyl sulfate, the yield is 62%, and the purity is greater than 99% %.

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Abstract

The invention discloses a preparation method of ethylene sulfate. The method comprises the steps of: reacting ethylene glycol with diethyl sulfate in the presence of an alkaline catalyst to produce ethylene sulfate, wherein the alkaline catalyst is one of or a combination of several of lithium hydroxide, sodium methoxide, sodium ethoxide, potassium carbonate, sodium carbonate and lithium carbonate. The preparation method provided by the invention can reduce environmental pollution, is more environmental friendly, and has the advantages of simple operation, safety, ideal yield and the like.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of vinyl sulfate. Background technique [0002] Ethylene sulfate, melting point: 99°C, colorless crystal or crystalline powder at room temperature, sensitive to water and high temperature. It is mainly used in the fields of medicine and material intermediates and lithium battery electrolyte additives, and has a broad market prospect. Its structural formula is: [0003] [0004] The method for preparing vinyl sulfate at present mainly is that ethylene glycol and thionyl chloride are raw materials to synthesize vinyl sulfite, and vinyl sulfite obtains product vinyl sulfate through catalytic oxidation; For example, Chinese invention patent CN105481826A discloses a kind of ethylene sulfate The preparation method of the method comprises: controlling the temperature at 0-50°C, dropping thionyl chloride into ethylene glycol, performing esterificatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 周龙王小龙周洋管晓东
Owner SUZHOU HUAYI NEW ENERGY TECH CO LTD
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