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A preparing method of lithium bis(fluorosulfonyl)imide

A technology of bisfluorosulfonimide lithium salt and sulfonyl is applied in the field of preparation of bisfluorosulfonimide lithium salt, and can solve the problems of easy explosion safety, flammability and explosion, hidden danger and the like

Active Publication Date: 2016-08-17
NANJING YUANSHU MEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Similar to this method, there are the following disadvantages: 1) most of the ammonia is based on liquid or gas, and the accurate amount of ammonia is difficult to finalize in the process of industrialized mass production. , Another point is that when a large amount of ammonia is used, it is easy to cause an explosion under different temperatures and pressures, making the safety problem always a hidden danger
2) The super alkaline lithium salt solution used in the lithiation reaction of difluorosulfonamide is a flammable and explosive super dangerous chemical reagent, and improper use will have serious consequences

Method used

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  • A preparing method of lithium bis(fluorosulfonyl)imide
  • A preparing method of lithium bis(fluorosulfonyl)imide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step a, weigh 10.7g of benzylamine, add it to a three-neck flask with a constant pressure dropping funnel and a thermometer, dissolve it in 100ml of tetrahydrofuran, and slowly add 1M BH dropwise after the temperature drops to 0°C 3 - 10.2ml of THF, the dropping time is 20min, the temperature of the whole dropping reaction is kept at 0°C-5°C, after the dropwise addition, directly distill under reduced pressure to obtain 12g of the intermediate.

[0028] Step b, add it into a three-neck flask with a constant pressure dropping funnel and a thermometer, dissolve it in 500ml of tetrahydrofuran, and slowly add 141ml of tert-butyl lithium dropwise after the temperature drops to -78°C. The dropping time is 1h, and the whole dropwise The reaction temperature is kept at -75°C to -78°C, and after the dropwise addition is completed, the reaction is continued at -75°C to -78°C for 1 hour. After the reaction is completed, 17.4ml of fluorosulfuryl chloride is slowly added dropwise, an...

Embodiment 2～3

[0032] The reaction steps are the same as in Example 1, except that the starting material in step a is replaced by 4-methylbenzylamine and 3,5-bismethylbenzylamine respectively, and the finally obtained aromatic methyl The yields of bisfluorosulfonimide were 78% and 74%, respectively.

Embodiment 4～5

[0034] The reaction steps are substantially the same as in Example 1, except that the BH in step a 3 -THF was replaced by trimethoxyboron and trihexyloxyboron respectively, and the yields of the finally obtained aromatic methylboronic acid were 88% and 83%, respectively.

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Abstract

A synthetic method of novel lithium bis(fluorosulfonyl)imide is provided. Compared with the prior art, the method is characterized in that the lithium bis(fluorosulfonyl)imide is prepared through reacting an aromatic methylamine that is adopted as an initial compound with organoboron, reacting with halogen sulfonyl to obtain a sulfonyl-containing aromatic methylamine, performing a hydrogenation reduction reaction to obtain bis(fluorosulfonyl)imide, and performing ion exchange with resin lithium. In a final strong base reaction for preparing the lithium bis(fluorosulfonyl)imide, the method adopts a resin lithium ion exchange technique, thus breaking away from convention, and the method researches the possibility that the reaction is performed without a solvent for the first time at home and abroad and synthesizes the lithium bis(fluorosulfonyl)imide in an ion exchange manner. The method has advantages of a simple process, convenience, simple after-treatment, no complex operation, and cyclic use of the resin lithium, and the like.

Description

technical field [0001] The invention belongs to the technical field of lithium-ion battery electrolytes, and in particular relates to a preparation method of bisfluorosulfonimide lithium salt. Background technique [0002] Since the concept of lithium-ion batteries was proposed and its commercial application was realized in the early 1990s, the basic research and application of lithium-ion batteries have rapidly become one of the hot spots in international electrochemical research. Electrolyte is an important element of lithium-ion batteries. By optimizing the electrolyte system, the composition and battery performance of the SEI film (solid electrolyte interphase) at the electrode interface can be improved, the reversible capacity of the electrode can be increased, and the cycle life can be extended. , improve the charge and discharge performance of the electrode. Therefore, the development of an electrolyte with superior performance has great practical significance for im...

Claims

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Application Information

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IPC IPC(8): C01B21/096
CPCC01B21/096
Inventor 金国范金峰王凯
Owner NANJING YUANSHU MEDICAL TECH CO LTD
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