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Purification method of lithium bis(fluorosulfonyl)imide

A bisfluorosulfonyl imide lithium salt and bisfluorosulfonyl imide lithium technology are applied in the purification field of bisfluorosulfonyl imide lithium salt, which can solve the problem of unsatisfactory product indicators, long evaporation time, and difficult product production salt crystallization

Active Publication Date: 2021-11-02
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the current lithium bisfluorosulfonyl imide in the desolventization process, if the lithium bisfluorosulfonyl imide is mixed with a good solvent according to the existing technology, and then evaporated to a small amount of solvent, the product is still difficult to form a salt and crystallize, and it takes a long time to evaporate time and require higher temperatures to eventually solidify into salt
And because there are many by-products in the purification process with high temperature, the by-products are difficult to separate, and even repeated purifications will reduce the purification efficiency and cause problems such as unsatisfactory product indicators due to repeated operations. The present invention provides a bisfluorosulfonimide The purification method of lithium salt, described method comprises:

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Provide 500 grams of crude product of bisfluorosulfonimide lithium salt, wherein, the purity of bisfluorosulfonimide lithium salt is 79% (in terms of ion chromatographic peak area percentage), sodium ion 15ppm, potassium ion 110ppm, chlorine content 100ppm, acid The value is 450ppm, the moisture is 130ppm, the turbidity of 10% dimethyl carbonate solution is 50mg / L, and the chromaticity is 25Hazen.

[0055]Mix the crude bisfluorosulfonimide lithium salt with 750 grams of 1,1,2,2-tetrachloroethylene in a reaction flask, then add 750 grams of divinyl ether dropwise under stirring conditions, and control The internal temperature is 0°C. Stir and dissolve for 1 hour after the dropwise addition, and then filter with a 0.1mm microporous membrane. The obtained filtrate is transferred to a distillation vessel connected with a fractionating head and has a stirring function, and is distilled under reduced pressure while stirring. Vacuum degree ≤ -0.065MPa, the temperature of the r...

Embodiment 2

[0058] Provide 500 grams of crude bisfluorosulfonyl imide lithium salt, the target is purity 86% (in terms of ion chromatographic peak area percentage), sodium ion 22ppm, potassium ion 31ppm, chlorine content 160ppm, acid value 816ppm, moisture 330ppm, 10% carbonic acid The turbidity of the dimethyl ester solution is 100 mg / L, and the chromaticity is 30 Hazen.

[0059] Mix the crude salt with 750 grams of 1,1,2-trichloroethylene in a reaction flask, then add 750 grams of methyl formate dropwise under stirring conditions, and control the internal temperature at 10°C during the dropping process. Stir and dissolve for 1 hour, then filter with a 0.2mm microporous membrane, transfer the obtained filtrate to a distillation vessel connected to a fractionating head and has a stirring function, start stirring and distill under reduced pressure, the vacuum degree is ≤ -0.075MPa, and put it in the condenser tube The temperature of the freezing liquid is the same as the boiling point of m...

Embodiment 3

[0062] Provide 500 grams of bisfluorosulfonimide lithium salt crude product, the target is purity 90% (calculated by ion chromatographic peak area percentage), sodium ion 24ppm, potassium ion 50ppm, chlorine content 200ppm, acid value 1010ppm, moisture 330ppm, 10% carbonic acid The turbidity of the dimethyl ester solution is 25 mg / L, and the chromaticity is 28 Hazen.

[0063] Mix the crude salt with 750 grams of 1,1,2-trichloroethane in the reaction flask, then add 750 grams of methyl acetate dropwise under stirring conditions, and control the internal temperature at 15°C during the dropping process, and the dropping is completed Stir and dissolve for 1 hour, then filter with a 0.3mm microporous membrane, transfer the obtained filtrate to a distillation vessel with a stirring function connected to a fractionating head, start stirring and distill under reduced pressure, vacuum degree ≤ -0.085MPa, condenser tube The temperature of the refrigerated liquid in the medium is the sam...

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Abstract

The invention relates to a purification method of lithium bis(fluorosulfonyl)imide, which comprises the following steps of: (1) adding a good solvent into a mixture of crude lithium bis(fluorosulfonyl) imide and an inert solvent, and filtering to obtain filtrate; and (2) distilling the filtrate to obtain finished lithium bis(fluorosulfonyl)imide, the boiling point of the inert solvent being 20 DEG C or above higher than that of the good solvent. The finished lithium bis(fluorosulfonyl)imide meets the combination of one or more of the following items: the ion chromatography content is more than or equal to 99.9%, the sodium ion content is less than or equal to 10ppm, the potassium ion content is less than or equal to 10ppm, the chlorine content is less than or equal to 10ppm, the acid value is less than or equal to 100ppm, the water content is less than or equal to 100ppm, the turbidity of a 10% dimethyl carbonate solution is less than or equal to 20mg / L, and the chromaticity is less than or equal to 20Hazen.

Description

technical field [0001] The invention relates to an electrolyte salt for a power battery and an energy storage battery, in particular to a method for purifying bisfluorosulfonimide lithium salt. 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 lithium-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 them, lithium bisfluorosulfonyl imide (LiFSI) is the only one among many electrolyte salts that is recognized by industry experts at home and abroad as a new generation of lithiu...

Claims

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Application Information

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IPC IPC(8): C01B21/086
CPCC01B21/086C01P2006/80
Inventor 吴国栋沈鸣陆海媛张丽亚周立新
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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