Method for producing alkali salts of bis(fluorosulfonyl)imide

A kind of technology of fluorosulfonyl and alkali metal salt, applied in the field of producing alkali metal salt of bisimide

Pending Publication Date: 2022-02-11
SOLVAY SA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the inventors of the present invention have found that unexpected new impurities are present in the alkali metal salts of fluorosulfonimides obtained according to EP 2 674 395 and EP 2 660 196

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0120] In a 250 mL stirred tank reactor, 40 g of crystallized NH 4 FSI was dissolved in 93 mL of ethyl methyl carbonate. The temperature of the reactor was fixed at 30°C. Add 8.7g of LiOH.H 2 O. Inject N at the bottom of the reactor at a rate of 170g / h 2 gas, and continue on N 2 The reaction was carried out within 8 h while bubbling.

[0121] Ammonium content was titrated by IPC. After reacting for 8h, NH 4 + / NH 3 The content is less than 100ppm.

example 2

[0123] in the absence of N 2 The same reaction as in Example 1 was carried out with bubbling.

[0124] After reacting for 20h, NH 4 + / NH 3 The content is still higher than 10,000ppm.

[0125] Purity analysis

[0126] The reaction mixture that example 1 and 2 obtains is passed potentiometric method (NH 4 + content), capillary electrophoresis and ion chromatography, and 19 F NMR analysis.

[0127] The results are reported in Table 1.

[0128] time NH 4 + / NH 3

Impurities 1* Impurities 2* Impurities 3* Example 1 8h <100ppm

does not exist very low does not exist Example 2 20h 14,000ppm exist exist exist

[0129] *Impurities 1, 2 and 3 were confirmed on the analytical spectrum. Without wishing to be bound by any theory, it is believed that these impurities correspond to by-products of the reaction of ammonia with EMC.

[0130] Without any ammonia removal (Example 2), the reaction time is long and the final pr...

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PUM

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Abstract

The invention relates to a method for producing an alkali salt of bis(fluorosulfonyl)imide, comprising the step of reacting, within a reaction medium, an ammonium salt of bis(fluorosulfonyl)imide with an alkali agent, to produce alkali salt of bis(fluorosulfonyl)imide and ammonia; and simultaneously contacting the reaction medium with an inert gas stream to strip out ammonia.

Description

technical field [0001] The present invention relates to a process for the production of alkali metal salts of bis(fluorosulfonyl)imides. More specifically, the present invention provides a novel process for the production of alkali metal salts of bis(fluorosulfonyl)imides which provides a high purity product. Background technique [0002] Bis(fluorosulfonyl)imide (commonly represented by "FSIH") and salts thereof, especially the lithium salt of bis(fluorosulfonyl)imide (commonly represented by "LiFSI"), can be used in various technical fields used as intermediate compounds or as final compounds. Bis(fluorosulfonyl)imides and salts thereof are especially useful in battery electrolytes. For this type of application, the presence of impurities is an important issue. [0003] The production of bis(fluorosulfonyl)imides and lithium salts of bis(fluorosulfonyl)imides is extensively described in the literature. Of the various techniques described, most employ either HF or metal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086C01B21/092C01B21/093H01M10/0568
CPCC01B21/086C01B21/0926C01B21/0935H01M10/0568H01M10/052
Inventor S·格伦E·瑞伯曼O·比西纳
Owner SOLVAY SA
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