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Method for preparing imidodisulfuryl fluoride lithium salt by means of phthalimide

A technology of bisfluorosulfonimide lithium salt and phthalophthalosulfonamide is applied in the field of lithium ion battery electrolyte, which can solve the problems of explosion safety, difficulty in setting the exact amount of ammonia, etc., and achieves cheap raw materials and high yield , the effect of easy availability of raw materials

Active Publication Date: 2016-09-07
NANJING YUANSHU MEDICAL TECH CO LTD
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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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  • Method for preparing imidodisulfuryl fluoride lithium salt by means of phthalimide
  • Method for preparing imidodisulfuryl fluoride lithium salt by means of phthalimide
  • Method for preparing imidodisulfuryl fluoride lithium salt by means of phthalimide

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Embodiment 1

[0041] Embodiment 1 A kind of preparation method of resin lithium

[0042] 1) Weigh 10g of the resin shown in formula (1), add it into a sealed glass tube, lower the temperature to 5°C, slowly add 20g of concentrated sulfuric acid, and raise the temperature to 30-40°C for 1 hour. After the reaction is complete, After the temperature dropped to 0-5°C, 20g of lithium hydroxide was added to carry out neutralization reaction. After the band reaction was completed, it was filtered, washed with ethanol or methanol three times, dried, and 13.8g of lithium resin was collected, and the yield was not counted.

[0043]

[0044] The specific reaction formula involved in the above-mentioned preparation method is as follows:

[0045]

Embodiment 2

[0047] Weigh 10g of the resin shown in formula (2), add it into a sealed glass tube, lower the temperature to 5°C, add 20g of concentrated sulfuric acid slowly, raise the temperature to 30-40°C and react for 1 hour, after the reaction is completed, the temperature will drop After reaching 0-5°C, 10 g of lithium carbonate was added to carry out neutralization reaction. After the band reaction was completed, filter, wash with ethanol or methanol three times, dry, and collect 13.1 g of resin lithium salt, the yield was not counted.

[0048]

[0049] The specific reaction formula involved in the above-mentioned preparation method is as follows:

[0050]

Embodiment 3

[0052] Weigh 14.7g of phthalimine and 19.5mL of triethylamine, dissolve it in 150mL of dichloromethane, add it into a three-necked flask, and slowly add 8.8mL of chlorofluorosulfonyl dropwise after the temperature drops to -20°C. For 20 minutes, the temperature of the entire dropwise addition reaction was kept at -20°C to -10°C. After the dropwise addition was completed, the temperature was raised to 35°C, and the reaction was continued for 12 hours. After the reaction was completed, 200 mL of distilled water was added for extraction. After collecting the organic phase, pour MgSO4 was added to dry it, filtered, and the organic solvent was distilled off under reduced pressure to obtain 22 g of phthalofluorosulfonamide, and the yield (calculated as phthalimine) was 96%.

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Abstract

The invention discloses a method for preparing imidodisulfuryl fluoride lithium salt. The method comprises the steps of dissolving phthalimide in an organic solvent for sulfamide reaction with sulfuryl chloride fluoride or fluorosulfonic acid so that phthalic fluorine sulfonamide is obtained, and reducing the phthalic fluorine sulfonamide to obtain secondary fluorosulfonamide the chemical formula of which is shown in formula iii; reducing the secondary fluorosulfonamide under the acid or alkaline condition to obtain primary flursulamid acid salt or flursulamid the chemical formula of which is shown in formula iv, conducting sulfamide reaction between the primary flursulamid acid salt or flursulamid and sulfuryl chloride fluoride or fluorosulfonic acid to obtain imidodisulfuryl fluoride, and then conducting ion exchange with resin lithium to obtain the final product imidodisulfuryl fluoride lithium salt. The raw materials are cheap and easy to obtain, reaction process is simple, yield is high, pollution is basically avoided, no harsh or dangerous reaction condition is required, product purification is easy, and the method is suitable for domestic mass production.

Description

technical field [0001] The invention belongs to the technical field of lithium ion battery electrolytes, and in particular relates to a method for preparing bisfluorosulfonimide lithium salt by using phthalimide. 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 gas as...

Claims

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Application Information

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