Preparation method of lithium bis (fluorosulfonyl) imide

A technology of bisfluorosulfonimide lithium and bisfluorosulfonimide triethylamine salt is applied in the field of preparation of bisfluorosulfonimide lithium, and can solve the problems of complex process, low yield, easy residual impurity ions, etc. problem, to achieve the effect of high safety, easy operation, fast and thorough response

Pending Publication Date: 2022-05-17
SINOPHARM CHEM REAGENT
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to solve the defects in the prior art such as complex process, low yield, and easy residu

Method used

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Experimental program
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Effect test

Embodiment 1

[0032] Add 141 g of bisfluorosulfonimide triethylamine salt, 13 g of lithium hydroxide, and 140 g of acetonitrile into a 500 mL round bottom flask equipped with a stirrer, a thermometer, and connected to a vacuum distillation device. Stir the reaction at 20°C while distilling under reduced pressure at a vacuum of 2000Pa, and gradually increase the vacuum to 200Pa to remove the triethylamine and water generated by the reaction. After reacting for 3 hours, there was no bisfluorosulfonimide triethylamine salt in the reaction solution. Add acetonitrile to the reaction solution under nitrogen protection and filter, concentrate the filtrate under reduced pressure, add 200 g of dichloromethane to stir and crystallize, filter, and vacuum dry to obtain 91.7 g of lithium bisfluorosulfonyl imide, with a yield of 98% and a purity of more than 99.9%.

Embodiment 2

[0034] Add 141 g of bisfluorosulfonimide triethylamine salt, 12 g of lithium hydroxide, and 140 g of acetonitrile into a 500 mL round bottom flask equipped with a stirrer, a thermometer, and connected to a vacuum distillation device. Stir the reaction at 10°C while distilling under reduced pressure at a vacuum of 2000Pa, and gradually increase the vacuum to 200Pa to remove triethylamine and water generated by the reaction. After reacting for 3 hours, the mass content of bisfluorosulfonimide triethylamine salt in the reaction liquid was 0.5%. The reaction liquid was added with acetonitrile under nitrogen protection and filtered, the filtrate was concentrated under reduced pressure, 200 g of dichloromethane was added to stir and crystallize, filtered, and vacuum-dried to obtain 88.8 g of lithium bisfluorosulfonyl imide, with a yield of 95% and a purity of more than 99.9%.

Embodiment 3

[0036]Add 141 g of bisfluorosulfonimide triethylamine salt, 13 g of lithium hydroxide, and 140 g of dimethyl carbonate into a 500 mL round bottom flask equipped with a stirrer, a thermometer, and connected to a vacuum distillation device. Stir the reaction at 60°C while distilling under reduced pressure at a vacuum of 2000Pa, and gradually increase the vacuum to 200Pa to remove the triethylamine and water generated by the reaction. After reacting for 3 hours, there was no bisfluorosulfonimide triethylamine salt in the reaction solution. Add dimethyl carbonate to the reaction solution under the protection of nitrogen and filter it, concentrate the filtrate under reduced pressure, add 200 g of dichloromethane to stir and crystallize, filter, and dry in vacuum to obtain 90.7 g of lithium bisfluorosulfonyl imide, with a yield of 97% and a purity of more than 99.9 %.

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Abstract

The invention belongs to the technical field of lithium ion battery electrolyte salt synthesis, and particularly relates to a preparation method of lithium bis (fluorosulfonyl) imide. Comprising the following steps: (1) in the presence of an organic solvent, mixing bis (fluorosulfonyl) imide triethylamine salt and an alkaline lithium salt, carrying out a stirring reaction, carrying out reduced pressure distillation, and removing triethylamine and water generated in the reaction until no bis (fluorosulfonyl) imide triethylamine salt exists in a reaction solution; and (2) filtering the reaction liquid after the reaction in the step (1) under the protection of nitrogen, concentrating the filtrate, adding a poor solvent, crystallizing, filtering and drying to obtain the product lithium bis (fluorosulfonyl) imide. The preparation method disclosed by the invention is simple and convenient to operate, the lithium ion exchange reaction is thorough, and the product is easy to crystallize and separate, so that the generated lithium bis (fluorosulfonyl) imide is high in yield and high in purity.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery electrolyte salt synthesis, and in particular relates to a preparation method of lithium bisfluorosulfonyl imide. Background technique [0002] Electrolyte lithium salt, as a key part of lithium battery electrolyte, has a great influence on the electrochemical performance of the electrolyte. Lithium bisfluorosulfonyl imide (LiFSI) vs LiPF 6 It has higher electrochemical stability and thermal stability, good adaptability to lithium metal electrodes and graphite electrodes, and is environmentally friendly, low temperature performance, and high safety performance. It is currently the most industrialized lithium battery new electrolyte lithium salt . [0003] The synthesis method of LiFSI reported in the literature is mostly divided into two steps: the first is to synthesize bisfluorosulfonimide (HFSI) or bisfluorosulfonimide salt; the second is to prepare lithium bisfluorosulfonimide th...

Claims

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Application Information

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IPC IPC(8): C01B21/096C01B21/086
CPCC01B21/096C01B21/086C01P2006/80Y02E60/10
Inventor 杨伟领吴孝兰顾小焱夏晓晗
Owner SINOPHARM CHEM REAGENT
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