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Preparation method of difluoro lithium sulfimide

A technology of lithium bisfluorosulfonyl imide and lithium bischlorosulfonyl imide, applied in the field of preparation of lithium bisfluorosulfonyl imide, can solve the problems of complex product composition, difficult separation, long process route, etc. , to achieve the effect of simple and easy-to-control process route, stable product quality and high product purity

Active Publication Date: 2014-03-26
浙江盛美リ電材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patent No. 7,253,317 uses alkali metal fluoride and bischlorosulfonimide to synthesize bisfluorosulfonimide alkali metal salt in nitromethane, and the product contains monochlorofluorosulfonimide and fluorosulfonamide and other impurities, it is difficult to separate, the yield is low, and it is difficult to obtain solid salt
All of the above process routes have disadvantages such as long process route, complex product composition and difficult further separation of entrained impurities such as ester or potassium ion content in the product, which further affects the industrialization of the product.

Method used

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  • Preparation method of difluoro lithium sulfimide
  • Preparation method of difluoro lithium sulfimide
  • Preparation method of difluoro lithium sulfimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Add 220.0 g (1 mol) lithium bischlorosulfonyl imide, 220.0 g dimethyl carbonate, 52.26 g (2 mol) lithium fluoride and 0.22 g 12-crown-4-ether into a 1000 ml three-necked flask under nitrogen protection. After reacting at 40°C for 8 hours under stirring, it was cooled to room temperature, filtered, and the filtrate was evaporated to remove the solvent to obtain 149 g of white crystals, with a yield of 79.7%. The chlorine content was detected by Swiss Metrohm 848 potentiometric titrator to be 7ppm. The product has been tested by Fourier infrared, at 1401cm -1 ,1386cm -1 ,1190cm -1 ,1225cm -1 ,859cm -1 ,845cm -1 ,783cm -1 ,747cm -1 , by comparing the standard spectrum of bisfluorosulfonimide, it was determined to be the characteristic group of bisfluorosulfonimide.

Embodiment 2

[0050] Add 220.0g (1mol) lithium bischlorosulfonimide, 2200.0g diethyl carbonate, 420.0g (10mol) sodium fluoride and 22g 15-crown-5-ether into a 3000ml three-neck flask under nitrogen protection. Under stirring, react at 100°C for 24 hours, then cool to room temperature, filter, and evaporate the solvent from the filtrate to obtain 155 g of white crystals, with a yield of 82.9%. The Swiss Metrohm 848 potentiometric titrator was used to detect the chlorine content was 5ppm, and the Shimadzu AA-6300 atomic absorption instrument was used to detect the sodium ion 0.7ppm. After Fourier infrared detection, at 1401cm -1 ,1386cm -1 ,1192cm -1 ,1226cm -1 ,859cm -1 ,845cm -1 ,783cm -1 ,747cm -1 , by comparing the standard spectrum of bisfluorosulfonimide, it was determined to be the characteristic group of bisfluorosulfonimide.

Embodiment 3

[0052] Add 220.0g (1mol) lithium dichlorosulfonimide, 200.0g diethyl carbonate and 200g dipropyl carbonate, 290.0g (5mol) potassium fluoride and 22g 18-crown to a 1000ml three-necked flask under nitrogen protection -6-Ether. Under stirring, react at 130° C. for 14 hours, then cool to room temperature, filter, and evaporate the solvent from the filtrate to obtain 153 g of white crystals, with a yield of 81.8%. The Swiss Metrohm 848 potentiometric titrator was used to detect the chlorine content was 2 ppm, and the Shimadzu AA-6300 atomic absorption instrument was used to detect sodium ions and potassium ions at 0.2 ppm. After Fourier infrared detection, at 1401cm -1 ,1386cm -1 ,1190cm -1 ,1225cm -1 ,859cm -1 ,845cm -1 ,783cm -1 ,747cm -1 , by comparing the standard spectrum of bisfluorosulfonimide, it was determined to be the characteristic group of bisfluorosulfonimide.

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Abstract

The invention relates to a preparation method of difluoro lithium sulfimide. The method comprises the following step: in a saturated alkyl carbonate and / or saturated fluoroalkyl carbonate solvent, enabling dichloro lithium sulfimide to react with alkali metal fluoride serving as a fluorinating agent to obtain the difluoro lithium sulfimide under a catalytic condition of a crown ether phase-transfer catalyst adaptive to the alkaline metal fluoride. The preparation method of the difluoro lithium sulfimide disclosed by the invention is simple in process route and easy to realize industrial preparation.

Description

technical field [0001] The invention relates to a preparation method of lithium bisfluorosulfonyl imide. Background technique [0002] Lithium bisfluorosulfonimide referred to in the present invention is a compound with the following structure: [0003] [0004] Lithium bisfluorosulfonyl imide can be used in many fields. It can be used as an electrolyte additive for lithium-ion batteries to improve the cycle performance of lithium-ion batteries. It can also be used as an electrolyte for primary batteries; it can be used as a catalyst for polymerization reactions; it can also be used in industrial fields Internal antistatic agent is used. [0005] Now studies have shown that lithium bisfluorosulfonyl imide is used in the electrolyte of rechargeable lithium batteries, which can effectively reduce the high and low temperature resistance of the SEI layer formed on the surface of the electrode plate at low temperatures, and reduce the lithium battery during placement. capaci...

Claims

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Application Information

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IPC IPC(8): C01B21/086
CPCC07C311/48H01G11/54C07C303/40H01G11/64C07C303/42H01G9/022Y02P20/52Y02E60/13
Inventor 沈鸣沈锦良张先林杨志勇张丽亚吴国栋
Owner 浙江盛美リ電材料有限公司
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