Lithium bis-fluoro-sulfonimide dechlorinating and purifying method

A technology of bisfluorosulfonyl imide lithium and a purification method, which is applied in the direction of nitrosyl chloride, nitrogen and non-metallic compounds, can solve the problems of lithium-ion battery performance degradation, large fluctuations in chloride ion content, and high chloride ion residues. Achieve the effect of low cost, high efficiency purity and high product purity

Active Publication Date: 2018-08-07
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High residual chloride ions will lead to a sharp decline in the performance of lithium-ion batteries
[0005] At present, the relevant patents on lithium bisfluorosulfonylimide are mainly concentrated in the direction of synthesis. Most of the purification methods used are directly recrystallizing the crude product, lacking a special chlorine removal process, which often leads to chlorine in the product. The ion content fluctuates greatly, and the product performance is unstable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add a total of 187 g of the crude bissulfonyl fluoride imide into a 500 mL reaction flask, add a total of 300 g of dichloromethane, stir and mix to disperse the crude product. Weigh a total of 150 g of thionyl chloride and add it to the system, control the temperature below 30°C, connect the exhaust gas absorption device, and absorb the exhaust gas with aqueous sodium hydroxide solution. After stirring and reacting for 24 hours, the water in the crude product was removed, and then the system was filtered to obtain a filter cake.

[0028] The resulting filter cake was transferred to a 500 mL reaction flask, washed with 200 g of anhydrous dichloromethane and suction filtered, and the filter cake was sucked dry to obtain a white solid. Put the white solid into a 500mL single-necked flask, add 150g of anhydrous diethyl ether in total, stir and dissolve for 0.5h, add triethylamine to adjust the pH to 7.4, remove the insoluble matter by filtration, and obtain a colorless and ...

Embodiment 2

[0030] Add a total of 187 g of the crude bissulfonyl fluoride imide into a 500 mL reaction flask, add a total of 300 g of dichloroethane, stir and mix to disperse the crude product. Weigh a total of 150 g of thionyl chloride and add it to the system, control the temperature below 30°C, connect the exhaust gas absorption device, and absorb the exhaust gas with aqueous sodium hydroxide solution. After stirring and reacting for 24 hours, the water in the crude product was removed, and then the system was filtered to obtain a filter cake.

[0031] The resulting filter cake was transferred to a 500 mL reaction flask, washed with 200 g of anhydrous ethane and suction filtered, and the filter cake was sucked dry to obtain a white solid. Put the white solid in a 500mL single-necked flask, add 150g of anhydrous diethyl ether in total, stir and dissolve for 0.5h, add anhydrous pyridine to adjust the pH to basic 8, remove insoluble matter by filtration, and obtain a colorless and transpa...

Embodiment 3

[0033] Add a total of 187 g of the crude bissulfonyl fluoride imide into a 500 mL reaction flask, add a total of 300 g of toluene, stir and mix to disperse the crude product. Weigh a total of 150 g of thionyl chloride and add it to the system, control the temperature below 30°C, connect the exhaust gas absorption device, and absorb the exhaust gas with aqueous sodium hydroxide solution. After stirring and reacting for 24 hours, the water in the crude product was removed, and then the system was filtered to obtain a filter cake.

[0034] The resulting filter cake was transferred to a 500 mL reaction flask, washed with 200 g of anhydrous toluene and suction filtered, and the filter cake was sucked dry to obtain a white solid. Put the white solid in a 500mL single-necked flask, add 150g of anhydrous diethyl ether in total, stir and dissolve for 0.5h, pass in dry ammonia gas to adjust the pH to alkaline 12, filter to remove insoluble matter, and obtain a colorless and transparent ...

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PUM

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Abstract

The invention discloses a lithium bis-fluoro-sulfonimide dechlorinating and purifying method. In the method disclosed by the invention, a dewatering temperature is lower, a water reaction type dewatering agent thionyl chloride is utilized to ensure that all generated products are gas and the products are prevented from going bad in a dewatering process; as the dewatering agent directly reacts withwater, crystallization water subjected to molecular complexation can also be successfully removed. According to the method disclosed by the invention, a crude product is dissolved by an organic solvent, water-free alkali is utilized and added to adjust a system pH to be larger than 7, and spin drying of a system is facilitated after acid is removed; furthermore, the used water-free alkali can prevent water from being generated again after reaction; meanwhile, chloride in the system is also effectively removed.

Description

technical field [0001] The invention belongs to the technical field of electrochemical energy systems, and in particular relates to a chlorine removal and purification method for lithium bisfluorosulfonyl imide. Background technique [0002] Since the concept of lithium-ion batteries was proposed and its commercial application was realized in the 1990s, the research on the basis and related applications of lithium-ion batteries has gradually become one of the hot spots in international electrochemical research. Lithium bisfluorosulfonyl imide has the advantages of high electrochemical stability, good thermal stability, high conductivity, and low corrosion rate (such as US Patent US5916475), and can be widely used in electrolytes, and has great potential in the application of lithium batteries. good prospects. [0003] There are many reports (such as U.S. Patent US4315935, Chinese patent documents CN103384641A, CN103347811A, CN101980955, CN101654229) to the method for synthe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086
CPCC01B21/086C01P2006/80
Inventor 张忠如廖颖闫俊美杨勇
Owner XIAMEN UNIV
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