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A method utilizing hydrazine to synthesize bisfluorosulfonimide lithium salt

A technology of bisfluorosulfonimide lithium salt and bisfluorosulfonimide, which is applied in the field of synthesizing bisfluorosulfonimide lithium salt with hydrazine, can solve problems such as difficulty in accurate ammonia determination and explosion safety issues. Achieve the effects of high yield, simple reaction steps, and cheap and easy-to-obtain raw materials

Active Publication Date: 2018-04-20
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 synthesis method of bisfluorosulfonamide lithium salt mainly uses ammonia water, ammonium salt or ammonia gas as the source of ammonia, and then adds chlorofluorosulfonyl or fluorosulfuric acid to synthesize bischlorosulfonamide, and then performs fluorination and lithiation Reaction gained bisfluorosulfonamide lithium salt, 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 too much and too little impels generation of unnecessary by-products, 2 ) 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

Method used

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  • A method utilizing hydrazine to synthesize bisfluorosulfonimide lithium salt
  • A method utilizing hydrazine to synthesize bisfluorosulfonimide lithium salt
  • A method utilizing hydrazine to synthesize bisfluorosulfonimide lithium salt

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Embodiment 1

[0040] The preparation method of embodiment 1 resin lithium

[0041] Weigh 10g of the resin shown in formula (1), add 20g of sodium cyanide into the sealed glass tube, heat up to 40-50°C, react for 60-80min, cool the obtained reaction solution to 0-5°C, Slowly add 6N hydrochloric acid solution for hydrolysis reaction, heat up to 50-60°C, and react for 12-24h. After the reaction is completed, slowly add excess lithium hydroxide for neutralization reaction. After the reaction is completed, filter and wash with ethanol or methanol three times. , dried and collected to obtain 13.4g resinous lithium, the yield was not counted.

[0042]

[0043] The specific reaction formula involved in the above-mentioned preparation method is shown in the following formula,

[0044]

Embodiment 2

[0045] The preparation method of embodiment 2 resin lithium

[0046] Weigh 10g of the resin shown in formula (2), add 20g of potassium cyanide into the sealed glass tube, heat up to 40-50°C, react for 60-80min, cool the obtained reaction solution to 0-5°C, Slowly add 6N hydrochloric acid solution for hydrolysis reaction, heat up to 50-60°C, and react for 12-24 hours. After the reaction is completed, slowly add excess lithium carbonate for neutralization reaction. After the reaction is completed, filter and wash with ethanol or methanol three times. After drying, 13.2 g of lithium resin was collected, and the yield was ignored.

[0047]

[0048]The specific reaction formula involved in the above-mentioned preparation method is shown in the following formula,

[0049]

Embodiment 3

[0051] Weigh 30g of hydrazine and 836.1mL of triethylamine, dissolve it in 1500mL of dichloromethane, add it to a three-necked flask, and slowly add 160.6mL of chlorofluorosulfonyl dropwise after the temperature drops to -5°C. The dropping time is 70min. Adding reaction temperature is kept at 0℃~-5℃. After the dropwise addition is completed, the temperature is raised to 35℃, and the reaction is continued for 24 hours. After the reaction is completed, 2000mL distilled water is added for extraction. After collecting the organic phase, add MgSO 4 It was dried, filtered, and the organic solvent was distilled under reduced pressure to obtain 165.4 g of bisfluorosulfonylamine, and the yield (calculated as nitrene) was 98%.

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Abstract

The invention discloses a method for synthesizing imidodisulfuryl fluoride lithium salt by utilizing hydrazine. The method comprises the steps of dissolving nitrene in an organic solvent; subjecting nitrene and sulfuryl chloridefluoride / fluorosulfonic acid to sulfonamide amination reaction to obtain enamine-disulfuryl fluoride; reducing the imidodisulfuryl fluoride to obtain perfluorinated sulfonamide shown in a formula iii; subjecting the obtained perfluorinated sulfonamide and fluorobenzenesulfonyl chloride / fluorosulfonic acid to sulfonamide amination reaction to obtain imidodisulfuryl fluoride; subjecting the obtained imidodisulfuryl fluoride and resin lithium to ion exchange in an organic solvent to obtain imidodisulfuryl fluoride lithium salt as a final product. The raw materials of the method are cheap and easily available. Meanwhile, the method is simple in reaction steps, high in yield and almost free of pollution. The reaction condition of the method is not harsh and dangerous at all. Moreover, the obtained product can be easily purified. Therefore, the method is suitable for mass 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 method for synthesizing bisfluorosulfonimide lithium salt by utilizing hydrazine. Background technique [0002] Lithium bisfluorosulfonyl imide (LiN(SO 2 F) 2 , hereinafter referred to as LiFSI) is an electrolyte substance with wide application prospects. LiFSI 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, its market demand will inevitably increase, and it may grow into a star product among auxiliary salt lithium salt compounds. [0003] The previous synthesis method of bisfluorosulfonamide lithium salt mainly uses ammonia water, ammonium salt or ammonia g...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/086C08F8/44
CPCC01B21/086C01P2002/86C08F8/44
Inventor 金国范金峰王凯张艳张慧李柳斌
Owner NANJING YUANSHU MEDICAL TECH CO LTD