Method for preparing bis(fluorosulfonyl)lithium imine

A technology of lithium fluorosulfonyl and imide, applied in the field of preparation of lithium bisimide, which can solve the problems of inability to obtain high-purity lithium bis(fluorosulfonyl)imide, poor thermal and chemical stability, and hindering applications

Inactive Publication Date: 2016-04-27
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lithium hexafluorophosphate (LiPF6) is a commercially successful electrolyte lithium salt under the current technical conditions, but the poor thermal and chemical stability of LiPF6 hinders its application in high power and high energy storage batteries.
This method must be operated in a vacuum box, and the yield of bis(fluorosulfonyl)imide lithium is only 48.6%, and high-purity bis(fluorosulfonyl)imide lithium cannot be obtained

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: two (fluorosulfonyl) imide potassium purification

[0025] Add 100 g (0.46 mol) of potassium bis(fluorosulfonyl)imide into a 500 ml one-necked flask, add 100 ml of ethanol and 100 ml of ethyl acetate as a solvent, and stir mechanically for 1 min. Filter out the insoluble matter and take the filtrate. An appropriate amount of triethylamine was added to make the pH of the filtrate neutral. The resulting filtrate was concentrated at 60°C under reduced pressure with proper stirring. Return to normal pressure when a small amount of crystallization can be observed in the filtrate. The temperature of the solution at this time was slowly lowered to -25° C., and allowed to stand for 24 hours to obtain crystals. A large number of crystals obtained were separated, washed three times with dichloromethane, and the washed crystals were dried at 40° C. under vacuum for 24 hours to obtain a white powder of potassium bis(fluorosulfonyl)imide with a purity >99.9%.

[00...

Embodiment 2

[0027] Embodiment 2: Preparation of bis(fluorosulfonyl)imide lithium

[0028] In a 250ml single-necked flask, add 10g (0.046mol) potassium bis(fluorosulfonyl)imide with a purity of ≥99.9% obtained in Example 1, add 50ml solvent (20ml ethyl acetate, 15ml butyl acetate, 15ml acetonitrile), mechanically Stir until completely dissolved to obtain potassium bis(fluorosulfonyl)imide solution. Another 4.3g (0.046mol) lithium tetrafluoroborate was dissolved in 50ml solvent (5ml dichloromethane, 15ml ethyl acetate, 15ml butyl acetate, 15ml acetonitrile) to obtain a lithium tetrafluoroborate solution. Slowly add the potassium bis(fluorosulfonyl)imide solution dropwise into the lithium tetrafluoroborate solution at 40°C, keep mechanical stirring, and react for 30 minutes. After the reaction, filter out the insoluble matter, take the filtrate, heat it under reduced pressure at 650Pa to 50°C, and concentrate the filtrate to 1 / 4 of its original volume. The concentrated solution was added t...

Embodiment 3

[0030] Embodiment 3: Preparation of bis(fluorosulfonyl)imide lithium

[0031] Add 10g (0.046mol) potassium bis(fluorosulfonyl)imide with a purity of ≥99.9% obtained in Example 1 into a 250ml single-necked flask, add 75ml of solvent (25ml ethyl acetate, 25ml butyl acetate, 25ml acetonitrile), and mechanically stir Until it is completely dissolved, a potassium bis(fluorosulfonyl)imide solution is obtained. Another 4.9 g (0.046 mol) of lithium perchlorate was dissolved in 75 ml of solvent (5 ml of dichloromethane, 20 ml of ethyl acetate, 25 ml of butyl acetate, and 25 ml of acetonitrile) to obtain a lithium perchlorate solution. Slowly add the potassium bis(fluorosulfonyl)imide solution dropwise into the lithium perchlorate solution at 40°C, keep mechanical stirring, and react for 30 minutes. After the reaction, filter out the insoluble matter, take the filtrate, heat it under reduced pressure at 650Pa to 50°C, and concentrate the filtrate to 1 / 4 of its original volume. The con...

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PUM

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Abstract

The invention discloses a method for preparing high-purity bis(fluorosulfonyl)lithium imine. According to the method, bis(fluorosulfonyl)imine metal salt with purity greater than or equal to 99.9% is taken as a raw material, and is reacted with lithium tetrafluoroborate or ithium perchlorate, and an obtained crude product is performed with steps of underpressure distillation, concentration, and extractive crystallization to obtain the high-purity bis(fluorosulfonyl)lithium imine.

Description

technical field [0001] The invention belongs to the field of fluorine chemical industry, and in particular relates to a preparation method of lithium bis(fluorosulfonyl)imide. Background technique [0002] The lack of fossil energy is a major problem facing the world economy. Due to the serious shortage of oil resources, the research and development of new alternative energy is the strategic development goal of all countries in the world. Due to its high energy density and volume specific energy, secondary lithium-ion batteries have developed rapidly in the past ten years, and are widely used in new energy electric vehicles, large-capacity energy storage devices and other fields. Lithium hexafluorophosphate (LiPF6) is a commercially successful electrolyte lithium salt under the current technical conditions, but the poor thermal and chemical stability of LiPF6 hinders its application in high power and high energy storage batteries. Therefore, the research and development of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/48C07C303/36H01M10/0566
CPCY02E60/10
Inventor 张庆华何逸波詹晓力陈丰秋赵卫娟徐卫国
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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