The preparation method of vinyl sulfate

A technology of vinyl sulfate and vinyl sulfite, which is applied in the field of preparation of vinyl sulfate, can solve the problems of low yield and low purity of vinyl sulfate, and achieve the effects of high molar yield, improved purity, and improved utilization rate

Active Publication Date: 2020-10-13
DONGYING HI TECH SPRING CHEM IND
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Problems solved by technology

[0004] The present invention aims at the technical problem that the yield of vinyl sulfate is low and the purity is not high in the above-mentioned background technology, the invention provides a kind of preparation method of vinyl sulfate, the yield of the prepared vinyl sulfate is high, the purity is high, and can Reduce the disposal of three wastes

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  • The preparation method of vinyl sulfate
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  • The preparation method of vinyl sulfate

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preparation example Construction

[0029] The invention provides a kind of preparation method of vinyl sulfate, comprises the steps:

[0030] 1) Add ethylene glycol dropwise to thionyl chloride at room temperature, raise the temperature to 50~80°C for 2~4 hours after the dropwise addition, and then carry out vacuum treatment to obtain a reaction solution containing vinyl sulfite;

[0031] 2) Purify the vinyl sulfite-containing reaction liquid in step 1) by rectification and purification under vacuum conditions to obtain vinyl sulfite with a purity greater than 99.2%;

[0032] 3) Mix vinyl sulfite with a purity greater than 99.2% in step 2) and ethylene dichloride, add sodium hypochlorite solution dropwise to the obtained mixed solution for premixing, stir and stand after the dropwise addition, and make The aqueous phase and the organic phase are separated, and the aqueous phase is separated to obtain the organic phase;

[0033] The whole process of the premixing is carried out under normal pressure, and the te...

Embodiment 1

[0059] Before starting work, purge and test the overall system, turn on the acid absorption system, weigh 2950kg of thionyl chloride into the synthesis reaction kettle, add 1300kg of industrial grade ethylene glycol dropwise, and control the temperature of the system not to exceed 30°C, which takes 8 hours After the dropwise addition, continue to stir for 2 hours, then raise the temperature to 50°C and keep it warm for 4 hours. Gas chromatography detects that there is no raw material ethylene glycol remaining. At this time, the system is a light brown clear solution. A reaction liquid containing vinyl sulfite was prepared (the content of vinyl sulfite was 98.2%).

[0060] Transfer the reaction solution containing vinyl sulfite after the reaction to the rectification tank, keep the pressure in the tank at -0.1MPa, control the reflux ratio to 5:1, and continue to extract the former fraction. When the ES content reaches more than 99.2%, Switch to the intermediate product reflux t...

Embodiment 2

[0075] Before starting work, purge and test the overall system, turn on the acid absorption system, weigh 2790kg of thionyl chloride into the synthesis reaction kettle, add 1185kg of industrial grade ethylene glycol dropwise, and control the temperature of the system not to exceed 25°C, which takes 8 hours After the dropwise addition, continue to stir for 3 hours, then raise the temperature to 65°C and keep it warm for 2 hours. Gas chromatography detects that there is no raw material ethylene glycol remaining. At this time, the system is a light brown clear solution. A reaction solution containing vinyl sulfite was prepared (the content of vinyl sulfite was 98.4%).

[0076] After the reaction, the reaction solution containing vinyl sulfite is transferred to the rectification tank, the pressure in the tank is kept at -0.095MPa, the reflux ratio is controlled at 5:1, and the fraction before extraction is continued. When the ES content reaches more than 99.2%, Switch to the inter...

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Abstract

The invention discloses a preparation method of vinyl sulfate, and belongs to the technical field of electrolyte additives for lithium ion batteries. The method comprises: 1) adding ethylene glycol dropwise into thionyl chloride, raising the temperature to 50-80° C. for 2-4 hours, and performing vacuum treatment to obtain a reaction solution containing vinyl sulfite; 2) adding The reaction solution of vinyl sulfite is rectified and purified under vacuum conditions; 3) Mix vinyl sulfite with a purity greater than 99.2% and dichloroethane, add sodium hypochlorite solution dropwise to the mixture, and stir after the addition is completed, Stand still to obtain the organic phase; 4) Adjust the pH value of the organic phase to 7~8, then add the catalyst, dropwise add sodium hypochlorite solution for oxidation reaction, keep warm for 1~1.5h, stand still to separate the liquid, and obtain the crude product of vinyl sulfate; 5) The crude vinyl sulfate is dehydrated, recrystallized and dried to obtain vinyl sulfate. The method provided by the invention has high yield and high purity of vinyl sulfate.

Description

technical field [0001] The invention relates to the technical field of electrolyte additives for lithium ion batteries, in particular to a preparation method of vinyl sulfate. Background technique [0002] Vinyl sulfate can be used as an electrolyte additive for lithium-ion batteries. Adding vinyl sulfate to the lithium-ion battery electrolyte can effectively inhibit the initial capacity decline of the lithium-ion battery, increase the initial discharge capacity, reduce the expansion of the battery after high-temperature storage, improve the charge-discharge performance of the battery, and prolong the cycle life of the battery. [0003] At present, the methods for producing vinyl sulfate mainly include the direct addition method of sulfur trioxide and ethylene oxide, and the synthesis method of ethylene glycol and thionyl chloride. The direct addition of sulfur trioxide and ethylene oxide to prepare vinyl sulfate is to add sulfuric anhydride and ethylene oxide to dioxane fo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 燕增伟吴雷雷林海陈凯迪
Owner DONGYING HI TECH SPRING CHEM IND
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