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Preparation method of bis(fluorosulfonyl)imide salt

The technology of bisfluorosulfonimide salt and bisfluorosulfonimide acid is applied in the field of preparation of bisfluorosulfonimide salt, and can solve the problems of difficult to meet the index, content of finished product, acid value, chromaticity difficult to meet the standard, The problems of chromaticity and turbidity increase, to achieve the effect of low halogen ion residue, low chromaticity and acid value, and low turbidity of insoluble matter

Active Publication Date: 2022-02-11
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] One: The corresponding bisfluorosulfonimide salt is generated by reacting bischlorosulfonylimide acid with alkali metal fluoride; the disadvantage of this process is that the amount of alkali metal fluoride is very large, and there are either a large number of by-products The product chlorinated alkali metal salt is generated, or highly corrosive hydrogen chloride is generated, which will cause a serious backlog of three wastes in large-scale production.
[0005] Two: The bisfluorosulfonimide salt is generated by the metathesis reaction of similar salts such as bisfluorosulfonimide organic alkali salts or inorganic alkali salts and corresponding alkali metal chloride salts that can undergo metathesis reactions; this method is due to the metathesis reaction Incomplete conversion will result in a certain amount of difluorosulfonimide organic alkali salt residue or inorganic metal ion residue that is difficult to separate. Among them, organic amines are easy to change color, which will cause the chroma of the final product, and the content index is difficult to reach the standard. Inorganic alkali metal residues will make it difficult to meet the standards for potassium ions and sodium ions
[0006] Three: The corresponding bisfluorosulfonimide salt is generated by directly reacting bisfluorosulfonimide acid with an inorganic base; this method will generate a large amount of by-product water during the reaction, resulting in the raw material bisfluorosulfonimide Hydrolysis or alkaline hydrolysis of acid and product bisfluorosulfonimide salt, impurities such as sulfate and ammonium after hydrolysis will make it difficult to meet the final product content, acid value, chroma and other indicators
[0007] Four: Reaction of bisfluorosulfonylimidic acid with lithium salt; in the reported method, there is a method of using halogenated lithium salt for reaction, which will cause halogen residue; in addition, there is also the use of non-halogenated lithium salt for reaction method, but because the by-product acid cannot be separated from the product in time, the acid value of the final product will be high, and the solvent evaporation process will lead to an increase in indicators such as color and turbidity

Method used

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  • Preparation method of bis(fluorosulfonyl)imide salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] First, 200 grams (1.036 moles) of lithium bisoxalate borate and 100 grams of ethyl acetate were mixed and dissolved in a drop tank, and then 178.4 grams (0.986 moles) of bisfluorosulfonylimidic acid and 1,1 , 800 grams of 2,2-tetrachloroethylene, when the temperature in the reaction vessel drops to -5°C, start to drop the ethyl acetate solution of lithium bisoxalate borate, keep the reaction for 3 hours after the addition, then filter the reaction solution, the filter cake Transferred to a desiccator, dried under reduced pressure to obtain 171.4 grams of bisfluorosulfonimide lithium salt, yield 93%, content 99.91%, acid value 20ppm, chromaticity 8 Hazen, 10% aqueous solution turbidity 2mg / L , turbidity of 10% dimethyl carbonate solution is 2mg / L, chloride ion 2.8ppm, fluoride ion 15ppm, SO4 2- Ion 0.8ppm.

Embodiment 2

[0026] First, 200 grams (0.953 moles) of sodium bisoxalate borate and 100 grams of ethyl propyl ether are mixed and stirred in a dripping tank to dissolve, and then 161 grams (0.890 moles) of bisfluorosulfonylimidic acid and 1 , 900 grams of 1,2-trichloroethylene, when the temperature in the reaction vessel drops to -10°C, start to add the ethyl propyl ether solution of sodium bisoxalate borate dropwise, keep warm for 5 hours after the dropwise addition, and then filter the reaction solution , the filter cake was transferred to a desiccator, and after drying under reduced pressure, 153.1 grams of bisfluorosulfonimide sodium salt was obtained, with a yield of 92%, a content of 99.90%, an acid value of 22 ppm, a chromaticity of 9 Hazen, and a 10% aqueous solution with a turbidity of 3mg / L, turbidity of 10% dimethyl carbonate solution is 3mg / L, chloride ion 2.1ppm, fluoride ion 14ppm, SO4 2- Ion 0.8ppm.

Embodiment 3

[0028] First, mix and dissolve 200 grams (0.885 moles) of potassium bisoxalate borate and 200 grams tetrahydrofuran in a drop tank, then mix 145.5 grams (0.804 moles) of bisfluorosulfonylimidic acid and 1,1,2 , 850 grams of 2-tetrachloroethane, when the temperature in the reaction vessel dropped to -15°C, the tetrahydrofuran solution of potassium bisoxalate borate was added dropwise. In the desiccator, 136.8 grams of difluorosulfonimide potassium salt was obtained after drying under reduced pressure, with a yield of 91%, a content of 99.91%, an acid value of 23 ppm, a chromaticity of 10 Hazen, and a turbidity of 10% aqueous solution of 2 mg / L, 10 The turbidity of % dimethyl carbonate solution is 3mg / L, the chloride ion is 2.5ppm, the fluoride ion is 12ppm, SO4 2- Ion 0.9ppm.

[0029] The following are comparative examples to illustrate the comparative advantages of the present invention.

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Abstract

The invention discloses a preparation method of bis(fluorosulfonyl)imide salt. The preparation method comprises the following steps: firstly, mixing bis(fluorosulfonyl)imidic acid and an inert solvent to obtain a bis(fluorosulfonyl)imidic acid inert solvent solution; and dissolving bis(oxalato)borate with a benign solvent, dropwise adding the bis(oxalato)borate into the bis(fluorosulfonyl)imidic acid inert solvent solution for a reaction, and carrying out direct filtering after the reaction is finished to obtain the bis(fluorosulfonyl)imidic salt. According to the preparation method, byproducts are few, a prepared product and the byproducts are easy to separate, product yield is high, and product quality is excellent.

Description

technical field [0001] The invention relates to the technical field of preparation of electrolyte salts for power batteries and energy storage batteries, in particular to a method for preparing bisfluorosulfonimide salts. Background technique [0002] As the country vigorously promotes the "carbon peak" and "carbon neutral" plans, the new energy industry chain will usher in vigorous development, which includes new energy vehicles, photovoltaics, wind power and other renewable energy storage industries. develop. The development of these industries is inseparable from high-performance power batteries or energy storage batteries. At this stage, liquid ion batteries are the most cost-effective, and the electrolyte salts related to them are the key materials that can determine the excellent performance of batteries. Among the many electrolyte salts, the bisfluorosulfonimide salt has the best overall performance. Among them, bisfluorosulfonimide lithium salt has become the most...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/096C01B21/086
CPCC01B21/096C01B21/086C01P2006/80Y02P20/133Y02E60/10
Inventor 吴国栋李伟锋曹娜袁青海李金生
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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