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Ethylene sulfate preparation method

A technology of vinyl sulfate and ethylene glycol, which is applied in electrochemical generators, electrical components, circuits, etc., can solve the problems of not meeting the requirements of green chemical development, high cost, and many wastes, so as to reduce battery expansion and reduce Production cost, effect of suppressing the rate of decline

Inactive Publication Date: 2020-02-21
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above-mentioned invention patent applications all need to use metal chloride catalysts, the cost is high, and there are many three wastes, which do not meet the development requirements of green chemistry

Method used

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Examples

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Embodiment 1

[0025] This embodiment provides a preparation method of vinyl sulfate, the preparation method is: add 100 grams of ethylene glycol and 300 grams of dichloromethane to the reaction kettle, add 200.2 grams of trimethylamine, stir and mix evenly, and add Slowly introduce (5mL / min) 181.9 grams of sulfuryl fluoride, slightly heat the reaction system to 30°C, stir and react for 18 hours, after the reaction is completed, filter to obtain 500.19 grams of organic phase containing vinyl sulfate, and distill out the disulfide under reduced pressure. Methane chloride and drying gave 191.58 g of vinyl sulfate, with a yield of 95.8%, a purity of 99.92%, a water content of 20 ppm, and an acid value of 10 ppm.

Embodiment 2

[0027] This embodiment provides a method for preparing vinyl sulfate. The preparation method is as follows: add 100 grams of ethylene glycol and 300 grams of acetone to the reaction kettle, add 342.7 grams of triethylamine, stir and mix evenly, and slowly add Pass in (4mL / min) 181.9 grams of sulfuryl fluoride, heat the reaction system to 40°C, stir and react for 24 hours, after the reaction is completed, filter to obtain 500.19 grams of organic phase containing vinyl sulfate, dichloromethane is distilled off under reduced pressure , and dried to obtain 192.18 grams of vinyl sulfate, with a yield of 96%, a purity of 99.93%, a water content of 18 ppm, and an acid value of 8 ppm.

Embodiment 3

[0029] The present embodiment provides a preparation method of vinyl sulfate. The preparation method is as follows: add 100 grams of ethylene glycol and 300 grams of acetonitrile into the reaction kettle, add 206.8 grams of tetramethylethylenediamine, stir and mix evenly, and add Slowly pour (2mL / min) 181.9 grams of sulfuryl fluoride into the solution, heat the reaction system to 60°C, stir and react for 36 hours, after the reaction is completed, filter to obtain 500.19 grams of organic phase containing vinyl sulfate, which is evaporated under reduced pressure Dichloromethane, drying to obtain vinyl sulfate 193.18 grams, yield 96.5%, purity 99.95%, water content 15ppm, acid value 6ppm.

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Abstract

The invention relates to an ethylene sulfate preparation method, which comprises: dissolving ethylene glycol in an aprotic organic solvent, adding an aprotic organic alkali, introducing sulfuryl fluoride, stirring while reacting, filtering after the reaction is completed, and carrying out evaporating concentrating and drying on the filtrate to obtain ethylene sulfate. According to the invention, the ethylene sulfate prepared by the method has extremely high purity of more than 99.9%, low moisture content of less than or equal to 20 ppm and low acid value of less than or equal to 10 ppm, and effectively changes the influence of the moisture and the acid value in an electrolytic solution on the cycle performance and the storage stability of a battery.

Description

technical field [0001] The invention relates to the technical field of lithium ion battery electrolyte additives, in particular to a preparation method for lithium ion battery electrolyte additive vinyl sulfate. Background technique [0002] With the continuous advancement of lithium-ion battery technology, the requirements for electrolyte additives in lithium-ion batteries are also getting higher and higher. It is necessary for electrolyte additives to suppress the decline in the initial capacity of the battery, increase the initial discharge capacity, and reduce high temperature. The battery expansion caused by the environment also needs to improve the charge and discharge performance and cycle times of the battery. Electrolyte additives are an important part of lithium secondary batteries. Excellent electrolyte additives have positive electrochemical effects in lithium secondary batteries, which can improve the kinetic characteristics of the battery, thereby significantly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/10H01M10/0567H01M10/0525
CPCC07D327/10H01M10/0567H01M10/0525Y02E60/10
Inventor 赵经纬许磊信勇刘杜孙安乐
Owner JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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