Preparation method of lithium bis (fluorosulfonyl) imide

A technology of lithium bisfluorosulfonyl imide and bisfluorosulfonyl imide salt, which is applied in the field of preparation of lithium bisfluorosulfonyl imide, can solve the problem of high residual chloride ion and acetate, harsh process conditions and poor product quality. drop and other issues

Pending Publication Date: 2020-09-04
SHANGHAI HUAYI GRP CO +1
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AI Technical Summary

Problems solved by technology

The fluorination reaction of the intermediate bischlorosulfonimide generally requires the introduction of a catalyst, and because the fluorination reaction is difficult to complete, and the catalyst and fluorinating reagents remain, it is very easy to cause excessive metal ions, chloride ions or hydrogen fluoride in the product, affecting the product Application in Electrolyte
[0006] Chinese patents CN104925765 and CN106976849 introduce reagents such as thionyl chloride and acid anhydride to dehydrate after the lithiation reaction. The dehydration reaction time is long, and it is easy to cause excessive chloride ion and acetate residues in the product.
[0008] In order to overcome the defects of harsh process conditions, inconvenient operation, and ineffective control of impurity ions in the existing LiFSI preparation methods, there is an urgent need in this field for a simple method for preparing lithium bisfluorosulfonyl imide to solve the problem of chlorine and water in the LiFSI production process. Introduce the problem of product quality degradation and further improve the purity and / or yield of the product

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  • Preparation method of lithium bis (fluorosulfonyl) imide

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[0013] The invention provides a kind of preparation method of lithium bisfluorosulfonyl imide, comprising the following steps:

[0014] (1) In the presence of an ammonia source, an organic solvent, a fluoride salt and an initial amount of sulfuryl fluoride, while slowly introducing an organic base, continue to feed a surplus of sulfuryl fluoride until the end of the reaction, and the reaction solution is directly distilled under reduced pressure Afterwards, the intermediate bisfluorosulfonyl imide salt is obtained;

[0015] The method of the invention comprises the steps of introducing ammonia source, organic solvent, fluoride salt and sulfuryl fluoride into the reaction vessel.

[0016] The ammonia source may be a conventional ammonia source in the art. In an example of the present invention, the ammonia source is selected from ammonia gas, ammonium fluoride, and ammonia in acetonitrile solution, preferably ammonium fluoride.

[0017] The amount of the ammonia source introd...

Embodiment 1

[0050] Add 14.8 g of ammonium fluoride and 300 g of acetonitrile into a 1000 ml round bottom flask equipped with a stirrer, an air inlet, a constant pressure dropping funnel, and a thermometer, and the dropping funnel is preloaded with 161.6 g of triethylamine. Seal the system, cool to 10°C, vacuumize to 0.09MPa, and then inject sulfuryl fluoride gas to return to normal pressure. Triethylamine was added dropwise within 1 h. At the same time, sulfuryl fluoride was continuously introduced to the calculated amount of 82 g, and the reaction was completed after stirring for 14 hours. The reaction liquid is distilled under high vacuum and reduced pressure, and after recovering acetonitrile, triethylamine and triethylamine hydrofluoric acid salt, difluorosulfonimide triethylamine is obtained.

[0051] Add 54 g of acetonitrile and 12 g of lithium oxide powder to the above bisfluorosulfonimide triethylamine salt, and stir at room temperature for 4 h. After filtration, the filtrate wa...

Embodiment 2

[0053] Add 14.8 g of ammonium fluoride and 300 g of acetonitrile into a 1000 ml round bottom flask equipped with a stirrer, an air inlet, a constant pressure dropping funnel, and a thermometer, and the dropping funnel is preloaded with 114.6 g of tetramethylpropylenediamine. Seal the system, cool to 10°C, vacuumize to 0.09MPa, and then inject sulfuryl fluoride gas to return to normal pressure. Triethylamine was added dropwise within 1 h. Sulfuryl fluoride was continuously fed to 82 g, and it took 13 hours to complete the reaction. The reaction solution is distilled under high vacuum and reduced pressure to recover acetonitrile, triethylamine and hydrogen fluoride tetramethylpropylenediamine salt to obtain bisfluorosulfonimide tetramethylpropylenediamine salt.

[0054] Add 80 g of acetonitrile and 12 g of lithium oxide powder to the above bisfluorosulfonimide tetramethylpropanediamine salt, and stir at room temperature for 5 h. Filtration, precipitation and concentration of t...

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Abstract

The invention discloses a preparation method of lithium bis (fluorosulfonyl) imide. The preparation method comprises the following steps: (1) in the presence of an ammonia source, an organic solvent,fluoride salt and an initial amount of sulfuryl fluoride, slowly introducing organic alkali while continuously introducing the balance of sulfuryl fluoride until the reaction is finished, and directlycarrying out reduced pressure distillation on the reaction solution to obtain an intermediate, namely the difluorosulfonyl imide salt; and (2) in the presence of an organic solvent, adding lithium oxide powder into the intermediate imidodisulfuryl fluoride salt, filtering, concentrating, adding a non-aqueous poor solvent, and crystallizing to obtain lithium bis (fluorosulfonyl) imide.

Description

technical field [0001] The invention relates to a method for preparing lithium bisfluorosulfonyl imide. The method of the invention has no water molecules in the whole process, thereby advantageously reducing the risk of thermal deterioration and decomposition of lithium salts in the presence of water molecules. 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 current synthesis method of LiFSI is mainly divided into two steps: the first step is to synthesize bisfluorosulfonimid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086
CPCC01B21/086C01P2006/80
Inventor 杨伟领卢磊宋芬粟小理
Owner SHANGHAI HUAYI GRP CO
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