Composition of bis(fluorosulfonyl)imide lithium salt

A composition, fluorosulfonyl technology, applied in the direction of lithium compounds, nitrogen compounds, alkali metal compounds, etc., can solve the problems of reducing the overall performance and stability of lithium-ion batteries

Pending Publication Date: 2021-01-26
ARKEMA FRANCE SA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, impurities carrying labile protons lead to a decrease in the overall performance and stability of Li-ion batteries due to their interference with electrochemical reactions

Method used

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  • Composition of bis(fluorosulfonyl)imide lithium salt

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Experimental program
Comparison scheme
Effect test

Embodiment approach

[0014] According to one embodiment, the mass content of acetic acid in the composition is greater than or equal to 0.1 ppm, preferably greater than or equal to 1 ppm, advantageously greater than or equal to 10 ppm, relative to the total weight of the composition.

[0015] According to one embodiment, the mass content of acetic acid in the composition ranges from 0.1 ppm to 300 ppm, preferably from 0.1 ppm to 200 ppm, advantageously from 0.1 ppm to 150 ppm, even more advantageously from 0.1 ppm to 100 ppm, relative to the composition of total weight.

[0016] The above compositions may also include:

[0017] - less than or equal to 20 ppm, preferably less than or equal to 15 ppm, advantageously less than or equal to 10 ppm of Cl by weight - the content of ions relative to the total weight of the composition; and / or

[0018] - less than or equal to 200 ppm by weight, preferably less than or equal to 50 ppm, advantageously less than or equal to 30 ppm of F - content, relative ...

Embodiment 1

[0130] A solution of 134 g LiFSI in 823 g butyl acetate (obtainable eg according to the method described in WO 2015 / 158979). The LiFSI concentration was about 10% by weight, and the water content of the solution was 3% by weight. The water content of this solution is higher than the solubility of water in butyl acetate due to the association of the lithium salt with water. The first concentration by evaporating the solvent was performed with a rotary evaporator at 40° C. under reduced pressure (P<30 mbar). A solution was obtained with a solids content of 42% by weight and a water content (measured by titration) of 430 ppm by weight. The final concentration is carried out in a WFSP (wiped film short path) evaporator at a temperature of 80° C. and a vacuum of 0.5 mbar. The concentrate was taken up in dichloromethane. LiFSI crystallizes rapidly. After 1 hour of contact time, solid LiFSI was obtained and recovered by filtration and dried under vacuum for at least 24 hours. Th...

Embodiment 2

[0133] Example 2 (Compared):

[0134] A solution of 53 g LiFSI in 640 g butyl acetate (obtained eg according to the method described in WO 2015 / 158979). The water content was 3.2% by weight. The solution was evaporated under vacuum at 70°C. A solution was obtained with a solids content of 40% by weight and a water content of 1050 ppm by weight. The final concentration is carried out in a WFSP (wiped film short path) evaporator at a temperature of 80° C. under a vacuum of 0.5 mbar.

[0135] The concentrate was taken up in dichloromethane. LiFSI crystallizes rapidly. After 1 hour of contact time, 44 g of LiFSI were obtained and recovered by filtration and dried under vacuum for at least 24 hours.

[0136] Residual solvent analysis was as follows:

[0137] weight% headspace NMR Butyl acetate 0.15 0.16 Dichloromethane 0.07 0.07 Acetic acid not detected 0.055 Butanol not detected not detected

[0138] Headspace measurements ...

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Abstract

The invention relates to a composition containing: at least 99.75% by weight of bis(fluorosulfonyl)imide lithium salt; and acetic acid in a content by mass strictly greater than 0 and less than or equal to 400 ppm.

Description

technical field [0001] The present invention relates to compositions based on lithium salts of bis(fluorosulfonyl)imides. Background technique [0002] Sulfonylimide anions are increasingly used in the field of energy storage or in the form of ionic liquids in the form of inorganic salts in batteries or organic salts in supercapacitors due to their extremely low alkalinity. field. As the battery market is expanding substantially and reducing the cost of battery fabrication has become a major challenge, inexpensive large-scale methods for the synthesis of this type of anion are required. [0003] In the specific field of lithium-ion batteries, the most widely used salt is LiPF 6 , but this salt has many disadvantages such as limited thermal stability, susceptibility to hydrolysis and thus lower battery safety. Recently, carrying FSO 2– Novel salts of the group have been investigated and have shown many advantages, such as better ion conductivity and resistance to hydrolys...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086C01B21/093C01B21/092C01D15/00H01M10/056
CPCC01B21/086C01B21/0923C01B21/0935C01D15/00H01M10/0568H01M10/0525Y02E60/10C01B21/0926H01M2300/0005
Inventor G.施密特R.泰西尔J-L.库图里尔
Owner ARKEMA FRANCE SA
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