Preparation method of ethyl methyl carbonate solution containing ethylene sulfate

A technology of ethyl methyl carbonate and vinyl sulfate, which is applied in the field of improving the preparation method of ethyl methyl carbonate solution, can solve problems such as unfavorable occupational health and hygiene, environmental dust pollution, inconvenient operation, etc., and achieves benefits for occupational health and hygiene, The process route is simple and controllable, solving the effect of low packaging efficiency

Pending Publication Date: 2021-11-23
江苏瀚康新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The packaging of vinyl sulfate solid finished products is very inconvenient. Accurate weighing and measurement is labor-intensive, the efficiency is very low, and there is a risk of exposure. First, it may cause environmental dust pollution, which is not conducive to occupational health and hygiene. Second, it may lead to the introduction of foreign matter in the packaging process
During the storage process of solid packaging, there will also be agglomeration, which will cause inconvenience in use
When the user uses vinyl sulfate to configure the electrolyte, the solid feeding also has problems such as difficult accurate measurement and inconvenient operation.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] This embodiment adopts the following preparation method: add 50 grams of vinyl sulfite, 300 grams of ethyl methyl carbonate and 0.6 grams of 5% ruthenium trichloride aqueous solution into a three-necked flask, stir evenly with a magnet in a 0-degree low-temperature bath, and drop Add the calcium hypochlorite aqueous solution of 242 grams 15% available chlorine content, control reaction system temperature in the dropwise addition process and be less than 5 degree, continue low-temperature stirring reaction 2 hours after dropwise addition finishes. Stand still to separate the liquids, and then wash the organic phase with 200 grams of pure water for 4 times, the temperature of the washing process is controlled at 2-8 degrees, and the obtained organic phase is first dried with anhydrous sodium sulfite, and then dried with molecular sieves to obtain 327 grams of 13.5% Ethyl methyl carbonate solution of mass concentration vinyl sulfate, detection moisture 5ppm, free acid 8ppm....

Embodiment 2

[0023] This embodiment adopts the following preparation method: add 50 grams of vinyl sulfite, 250 grams of ethyl methyl carbonate and 0.5 grams of 5% ruthenium trichloride aqueous solution into a three-necked flask, stir evenly with a magnet in a 0-degree low-temperature bath, and drop Add the sodium hypochlorite aqueous solution of 280 grams 13% available chlorine content, control reaction system temperature in the dropwise addition process and be less than 5 degree, continue low-temperature stirring reaction 2 hours after dropwise addition finishes. Stand to separate the liquids, and wash the organic phase with 150 grams of pure water for 5 times, the temperature of the washing process is controlled at 2-8 degrees, and the obtained organic phase is first dried with anhydrous magnesium sulfite, and then dried with molecular sieves to obtain 260 grams of 15.4% mass concentration vinyl sulfate ethyl methyl carbonate solution, detected moisture 6ppm, free acid 7ppm.

Embodiment 3

[0025] This embodiment adopts the following preparation method: add 50 grams of vinyl sulfite, 400 grams of ethyl methyl carbonate and 1 gram of 5% ruthenium trichloride aqueous solution into a three-necked flask, stir evenly with a magnet in a 0-degree low-temperature bath, and drop Add the potassium hypochlorite aqueous solution of 400 grams 9% available chlorine content, control reaction system temperature during dropwise addition and be less than 5 degree, continue low-temperature stirring reaction 2 hours after dropwise addition finishes. Stand to separate the liquids, and wash the organic phase with 300 grams of pure water for 3 times, the temperature of the washing process is controlled at 2-8 degrees, and the obtained organic phase is first dried with anhydrous calcium chloride, and then dried with molecular sieves to obtain 385 grams of 12.3% mass concentration of ethyl methyl carbonate solution of vinyl sulfate, detected moisture 5ppm, free acid 8ppm.

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PUM

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Abstract

The invention discloses a preparation method of a methyl ethyl carbonate solution containing ethylene sulfate, and relates to improvement of a preparation method of a lithium ion battery electrolyte, in particular to improvement of the preparation method of the methyl ethyl carbonate solution containing the ethylene sulfate. The technical scheme adopted by the invention comprises the following steps: adding ethylene sulfite, methyl ethyl carbonate and a trace amount of ruthenium trichloride aqueous solution into a reaction kettle, and uniformly conducting stirring at low temperature; and S2, dropwise adding a hypochlorite aqueous solution into the reaction kettle at low temperature to obtain a methyl ethyl carbonate crude product solution of ethylene sulfate, carrying out low-temperature water washing and liquid separation on the ethyl methyl carbonate crude product solution of ethylene sulfate for multiple times, and adding a dehydrating agent into the organic phase after water washing and liquid separation, and conducting drying to obtain a methyl ethyl carbonate solution finished product. According to the invention, the problems of low packaging efficiency, easy caking during storage, inconvenient use and the like of the ethylene sulfate solid product are solved, and the use convenience of the ethylene sulfate as the lithium ion battery electrolyte additive can be obviously improved.

Description

technical field [0001] The invention relates to an improvement of a method for preparing an electrolyte of a lithium ion battery, in particular to an improvement of a method for preparing an ethyl methyl carbonate solution containing vinyl sulfate. Background technique [0002] Vinyl sulfate is an excellent electrolyte additive material for lithium-ion batteries. Since the central sulfur atom of vinyl sulfate is more electronegative, the reducibility at the graphite negative electrode interface is stronger than that of the corresponding carbonate, so a more stable solid electrolyte phase interface film (SEI film) is preferentially formed at the electrode interface at the initial stage of charging, It is used to prevent lithium ions from reacting with carbon negative electrodes or other substances during charging and discharging, thereby inhibiting the decline in the initial capacity of lithium-ion batteries, increasing the initial discharge capacity, reducing the expansion o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/10H01M10/0525H01M10/0567
CPCC07D327/10H01M10/0525H01M10/0567H01M2300/0025Y02E60/10
Inventor 陈群姜飞张正洪孙西船曹国华
Owner 江苏瀚康新材料有限公司
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