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
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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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