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A kind of preparation method of bistrifluoromethanesulfonylimide lithium salt

A technology of benzyl bis-trifluoromethyl sulfonamide and lithium sulfonimide is applied in the preparation of sulfonic acid amide, organic chemistry and other directions, which can solve the problems of explosion safety, difficulty in determining the exact amount of ammonia, and achieve the reaction rate. The effect of fast, cheap raw materials and high yield

Active Publication Date: 2018-08-10
NANJING YUANSHU MEDICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The previous synthetic method of bistrifluoromethanesulfonamide lithium salt mainly uses ammoniacal liquor, ammonium salt or ammonia gas as the source of ammonia, then adds trifluoromethanesulfonyl chloride etc. to synthesize lithium dichlorosulfonylamide, and then carries out fluorine Lithium salt of two trifluoromethanesulfonamide lithium salts obtained in the reaction of lithiation and lithiation, this type of method has the following disadvantages: 1) in the process of industrialized mass production, the accurate amount of ammonia is difficult to finalize, and too much or too little promotes the formation Unnecessary by-products, 2) When ammonia is used in large quantities, it is easy to cause explosions under different temperatures and pressures, making safety issues always a hidden danger

Method used

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  • A kind of preparation method of bistrifluoromethanesulfonylimide lithium salt
  • A kind of preparation method of bistrifluoromethanesulfonylimide lithium salt
  • A kind of preparation method of bistrifluoromethanesulfonylimide lithium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Weigh 10g of the resin shown in the following formula (1) and add 40g of sodium hydrosulfide into 100ml of acetocyanide, react at room temperature for 4-6h, after the reaction is complete, add 50g of lithium carbonate to continue the reaction for 2-3h, after the reaction is complete, cool down To room temperature, the resulting solid was filtered, washed three times with 5ml of distilled water, and then washed three times with 5ml of ethanol, collected and dried to obtain 11.3g of resin lithium shown in formula (2), and the yield was not counted.

[0032]

Embodiment 2

[0034] Same as Example 1, except that organic solvent 100mL acetocyanide is replaced by 100mL tetrahydrofuran, and 50g lithium carbonate is replaced by 50g lithium hydroxide to obtain resin lithium shown in 13.8g formula (2), and the yield is not counted.

Embodiment 3

[0036] Same as Example 1, except that the organic solvent 100mL acetocyanide is replaced by 100mL 1,2-dimethoxyethyl ether, and 50g lithium carbonate is replaced by 50g lithium hydroxide to obtain resin lithium shown in 12.5g formula (2), Yield does not count.

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Abstract

The invention discloses a preparation method of LiN(CF3SO2)2 salt. The preparation method comprises the following steps: benzene methanamine is dissolved in an organic solvent and subjected to a sulfonamide reaction with trifluoromethyl sulfonyl chloride or trifluoromethyl sulfonyl fluoride, benzyl bis(trifluoromethyl sulfamide) is obtained and reduced, and bis(trifluoromethyl sulfamide) is obtained; the obtained bis(trifluoromethyl sulfamide) and resin lithium are subjected to ion exchange in an anhydrous solvent, and a final product LiN(CF3SO2)2 salt is obtained. According to the method, raw materials are low in price and easy to obtain, reaction procedures are simple, the yield is high, nearly no pollution is caused, rigid and dangerous reaction conditions are avoided, the product is easy to purify, and the method is suitable for large-scale production in China.

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 bistrifluoromethanesulfonylimide lithium salt. Background technique [0002] Lithium bistrifluoromethanesulfonyl imide (LiN(CF 3 S0 2 ) 2 , hereinafter referred to as LiTFSI) is an electrolyte substance with wide application prospects. LiTFSI has suitable conductivity, high thermal stability and electrochemical stability; the probability of side reactions is small, and corrosive gases such as HF will not be generated. An indispensable high-tech product in the electrolyte of lithium-ion secondary batteries. With the continuous development of the lithium battery industry, it can also be used as a catalyst and ionic liquid for multiple purposes, and its market demand is bound to increase. [0003] The previous synthetic method of bistrifluoromethanesulfonamide lithium salt mainly uses ammoniacal liquor, ammonium salt o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C311/48C07C303/40C07C303/36
CPCC07C303/36C07C303/40C07C311/48
Inventor 金峰王凯金国范
Owner NANJING YUANSHU MEDICAL TECH CO LTD
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