A kind of preparation method of bis(trifluoromethylsulfonyl)imide lithium salt

A technology of lithium trifluoromethylsulfonyl and bisfluorosulfonyl imide, which is applied in the field of preparation of lithium diimide salt, can solve the problems of difficult separation of by-products, complicated reaction steps, and difficult operation, so as to improve the product Performance and cost competitiveness, improved product purity, and reduced separation difficulty

Active Publication Date: 2021-02-05
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this re-synthesis method, the reaction steps are complicated and the yield is low, so the method cannot realize industrial production;
[0005] 2. Use elemental ammonia or ammonium ions as the nitrogen source, then add trifluoromethylsulfonyl chloride to synthesize bistrifluorosulfonyl imide, and then perform lithiation reaction to obtain bis(trifluoromethylsulfonyl)imide Lithium salt, in the process of industrialized mass production, the excessive amount of ammonia is too much to promote the formation of unnecessary by-products, and elemental ammonia, such as ammonia gas, is easy to cause explosions under different temperatures and pressures, making safety problems hidden dangers;
In this method, because the raw material trifluoromethanesulfonamide used in the first step is expensive, and trifluoromethanesulfonyl fluoride is a highly corrosive gas, a high-pressure reactor of special material is required and the operation is very difficult, so this method also Unable to achieve industrial production
[0007] As mentioned above, the current bisfluorosulfonimide salt synthesis process still has disadvantages such as cumbersome process, long process, low product conversion rate, difficult separation of by-products, need for special equipment and use of highly corrosive and expensive raw materials, etc., resulting in Difficult operation, high energy consumption, environmental pollution and other defects make LiTFSI unable to realize industrial application

Method used

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  • A kind of preparation method of bis(trifluoromethylsulfonyl)imide lithium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] First, cool 3L (1.5mol) of 0.5mol ethyllithium n-butyl ether solution to -70°C~-50°C, start to feed trifluoromethane gas, adjust the gas flow according to the reaction temperature, and control the reaction temperature at -70°C~- 50°C, stop the ventilation when the reaction temperature does not change significantly, the reaction time is 3 hours, and the trifluoromethyllithium ether solution is obtained. The synthesis of the reaction solution is complete and it is ready for use; In n-butyl ether, prepare a lithium bisfluorosulfonyl imide solution, then slowly add the solution dropwise to the synthesized trifluoromethyllithium n-butyl ether solution, and control the reaction temperature between -30°C and 0°C During the dropwise addition process, white lithium fluoride solids will be precipitated, and after the lithium bisfluorosulfonimide solution is added dropwise, the reaction will end for two hours; the reaction solution is filtered, and the obtained filtrate is concentr...

Embodiment 2

[0032] First, mix 2.5 mol n-butyllithium hexane solution 2L (4.5 mol) with diethyl ether (2L) and cool to -70°C ~ -50°C, start to feed trifluoromethane gas, adjust the gas flow rate according to the reaction temperature, the reaction temperature Control the temperature at -70°C to -50°C, and stop ventilation when the reaction temperature has no obvious change. The reaction time is 5 hours, and the synthesis of the trifluoromethyllithium reaction solution is completed and is ready for use. Then 374 g (2.0 mol) of lithium bisfluorosulfonimide was dissolved in ether to prepare a lithium bisfluorosulfonyl imide ether solution, and then the solution was slowly added dropwise to the synthesized lithium trifluoromethyl ether solution , control the reaction temperature between -30°C and 0°C, white lithium fluoride solids will precipitate during the dropwise addition, and the reaction will end after two hours of adding the lithium bisfluorosulfonyl imide solution dropwise. The reaction...

Embodiment 3

[0034] First, mix 1L (2.0mol) of 2mol tert-butyllithium pentane solution with tert-butyl ether and cool it to -70°C~-50°C, then start to feed trifluoromethane gas, adjust the gas flow rate according to the reaction temperature, and control the reaction temperature At -70°C to -50°C, stop ventilation when there is no significant change in the reaction temperature, the reaction time is 3 hours, the synthesis of the trifluoromethyllithium reaction solution is completed, and it is ready for use; first, 178g of lithium bisfluorosulfonyl imide (0.95 mol) was dissolved in n-butyl ether to prepare lithium bisfluorosulfonimide solution, and then slowly added the solution dropwise to the synthesized trifluoromethyllithium n-butyl ether solution, controlling the reaction temperature at -30°C to Between 0°C, white lithium fluoride solids will precipitate during the dropping process, and the reaction will end after two hours of adding the lithium bisfluorosulfonyl imide solution dropwise. ...

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Abstract

The invention provides a preparation method of bis(trifluoromethylsulfonyl)imide lithium salt, which is characterized in that trifluoromethane gas is passed into the non-polar lithium alkyl lithium salt under anhydrous, nitrogen protection and low temperature conditions. React in solvent solution to prepare trifluoromethyllithium. After the reaction is completed, slowly add bisfluorosulfonyl imide lithium solution to the trifluoromethyllithium solution under low temperature conditions. During the dropping process, white solids will be precipitated. Finally, the reaction solution was filtered, and the filtrate was evaporated to dryness under reduced pressure to obtain a white solid wet salt, which was dried in vacuo to obtain bis(trifluoromethylsulfonyl)imide lithium salt. The present invention has the advantages of realizing the one-pot synthesis of lithium bis(trifluoromethylsulfonyl)imide, which greatly simplifies the process route compared with the traditional method, reduces the difficulty of separating products and by-products in the reaction process, and improves product purity. Thereby further reducing production costs, improving product performance and cost competitiveness, and providing feasible technical support for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery electrolytes, in particular to a preparation method of bis(trifluoromethylsulfonyl)imide lithium salt. Background technique [0002] Lithium bis(trifluoromethylsulfonyl)imide (hereinafter referred to as LiTFSI), with a density of 1.334g / cm3 and a melting point of 234°C. LiTFSI has suitable electrical conductivity, high thermal stability, high electrochemical stability, and the probability of side reactions Small and other characteristics, will not produce corrosive gases such as HF, is an indispensable high-tech product in the electrolyte of lithium-ion secondary batteries. In addition to the field of lithium batteries, it also has broad application prospects in the fields of ionic liquids, antistatic and medicine. In particular, the preparation of new and new rare earth Lewis acid catalysts for the anion displacement reaction through the corresponding trifluoromethanesulfonate also h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/40C07C311/48
CPCC07C303/40C07F1/02C07C311/48
Inventor 吴国栋李伟锋陆海媛曹娜杨建新孙秋婷杨志勇张先林
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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