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Trifluoromethanesulfinate purification method

A technology of trifluoromethyl sulfinic acid and sodium trifluoromethyl sulfinate, which is applied in the field of purification of trifluoromethyl sulfinic acid, can solve the problem of not being suitable for large-scale promotion and use, complex preparation process, and many inorganic salts. and other problems, to achieve the effect of low cost of purification equipment and purified raw materials, simple preparation process and simple operation method

Inactive Publication Date: 2016-08-31
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such as Chinese Patent No. 200880118035.8 discloses a method for preparing trifluoromethylsulfinic acid. Although it can produce high-purity trifluoromethylsulfinic acid, it uses more inorganic salts and is difficult to purify, resulting in the preparation of The process is complicated, and the preparation efficiency is low
The preparation equipment and raw materials used are more, the preparation cost is higher, and the waste phenomenon is serious, so it is not suitable for large-scale promotion and use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] In a 2000ml three-necked flask equipped with a stirrer, add 300g of 60-70% sodium trifluoromethanesulfinate industrial product, 20g of anhydrous magnesium sulfate, 500g of ethyl acetate solvent, and stir at 20-30°C for 0.5h, Stop stirring, filter the discharge, collect the filtrate, put the filter cake back into the flask, add 500g of ethyl acetate solvent to the flask, stir at 20-30°C for 0.5h, stop stirring, filter the discharge, collect the filtrate, and filter the cake Then put it back into the flask, add 300g ethyl acetate solvent, stir at 20-30°C for 0.5h, stop stirring, filter the discharge, collect the filtrate, rinse the filter cake with a small amount of ethyl acetate solvent, remove the filter cake , collect three filtrates and the filtrate solution of rinsing, evaporate to dryness with rotary evaporator under negative pressure, reclaim ethyl acetate solvent, recycle, add 1000g deionized water in the kettle, dissolve sodium trifluoromethyl sulfinate solid, An...

Embodiment 2

[0041] In a 2000ml three-necked flask equipped with a stirrer, add 300g of 60-70% sodium trifluoromethanesulfinate industrial product, 20g of anhydrous magnesium sulfate, 500g of acetonitrile solvent, stir at 20-30°C for 0.5h, stop stirring , filter the output, collect the filtrate, put the filter cake back into the flask, add 500g of acetonitrile solvent to the flask, stir at 20-30°C for 0.5h, stop stirring, filter the output, collect the filtrate, and put the filter cake back into the Add 300g of acetonitrile solvent to the flask, stir at 20-30°C for 0.5h, stop stirring, filter the discharge, collect the filtrate, rinse the filter cake with a small amount of acetonitrile solvent, remove the filter cake, collect the filtrate three times and rinse The filtrate solution was evaporated to dryness with a rotary evaporator under negative pressure, and the acetonitrile solvent was recovered for recycling. 1000g of deionized water was added to the kettle to dissolve the sodium triflu...

Embodiment 3

[0043] In a 2L reaction kettle, add 300kg of 60-70% sodium trifluoromethanesulfinate industrial product, 20kg of anhydrous magnesium sulfate, 500kg of ethyl acetate solvent, stir at 20-30°C for 0.5h, stop stirring, and discharge Filtrate, collect the filtrate, put the filter cake back into the flask, add 500kg ethyl acetate solvent to the flask, stir at 20-30°C for 0.5h, stop stirring, filter the discharge, collect the filtrate, and put the filter cake back into the flask Add 300kg of ethyl acetate solvent to the flask, stir at 20-30°C for 0.5h, stop stirring, filter the discharge, collect the filtrate, rinse the filter cake with a small amount of ethyl acetate solvent, remove the filter cake, collect and filter three times liquid and rinsed filtrate solution in the reaction kettle, evaporated to dryness under reduced pressure, reclaim the solvent ethyl acetate, and recycle, add 1000kg deionized water to the kettle, dissolve the sodium trifluoromethylsulfinate solid to obtain t...

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Abstract

The invention discloses a trifluoromethanesulfinic acid purification method. The method comprises the following steps: mixing and stirring a sodium trifluoromethanesulfinate industrial product, anhydrous magnesium sulfate and a solvent, carrying out suction filtration while stirring, collecting the filtrate, putting a filter cake in an original stirred reaction kettle, further adding the solvent, carrying out suction filtration while stirring, collecting the filtrate, collecting all the filtrates and filtrate solutions after leaching and putting all the filtrates and filtrate solutions after leaching in the kettle, carrying out reduced-pressure drying, recovering the solvent, adding deionized water to obtain a sodium trifluoromethanesulfinate water solution; then sending the sodium trifluoromethanesulfinate water solution to a dryer for spray drying, thus obtaining the sodium trifluoromethanesulfinate powder product with content of 95% or above. The method has the beneficial effects that high content sodium trifluoromethanesulfinate is extracted from the sodium trifluoromethanesulfinate industrial product by using the solvent and high content sodium trifluoromethanesulfinate without inorganic salts, such as bromide ions, is obtained after the solvent is removed, thus meeting the production requirements of lithium ion battery electrolyte bis(trifluoromethane)sulfonimide lithium salt.

Description

technical field [0001] The subject of the present invention is a process for the purification of trifluoromethylsulfinic acid. [0002] The present invention is directed to the preparation of high-purity trifluoromethylsulfinic acid salts, and more particularly the preparation of alkali metal trifluoromethylsulfinic acid. Background technique [0003] The air pollution in big cities in my country can no longer be ignored. Gasoline vehicle emissions are one of the main sources of pollution. Already 16 cities in my country have been listed among the 20 cities with the most serious air pollution in the world. my country's current car ownership is an average of 10 cars per 1,000 people, and the number of cars will increase tenfold. Therefore, in order to save energy and reduce carbon dioxide emissions, electric vehicles will gradually become a trend in the development of automobiles and inevitable. The biggest technical bottleneck in the development of electric vehicles is the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C313/04
CPCC07C313/04
Inventor 刘方丁亮单晓军王成双张天峰
Owner YANCHENG INST OF TECH
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