Lithium bis(fluorosulfonyl)imide preparation method

The technology of bisfluorosulfonimide lithium salt and bisfluorosulfonimide is applied in the field of preparation of bisfluorosulfonimide lithium salt, which can solve the problems of poor product crystallinity, influence on yield, complicated process, etc. The effect of low cost, fast response and thorough response

Active Publication Date: 2018-05-08
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] For the purification process after lithiation, the published literature mainly uses a single solvent for direct crystallization, and the obtained product has poor crystallinity, and most of them are powder products, which is not conduciv

Method used

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  • Lithium bis(fluorosulfonyl)imide preparation method

Examples

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Comparison scheme
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Example Embodiment

[0030] Example 1

[0031] Add 1020g of bischlorosulfonimide to a 1000mL reaction flask, and blow nitrogen to make the whole system in an anhydrous atmosphere under a nitrogen atmosphere. Under normal pressure, turn on the stirring and heat the system to 75~85℃ for 6 hours. , The solid bischlorosulfonimide in the system gradually melts into a liquid state. A total of 400g of anhydrous HF gas was slowly introduced under stirring. After a total of about 6 hours of reaction, the system is gradually cooled to room temperature, the gas in the system is released, the generated white smoke HCl gas is absorbed with lye, and the excess HF is absorbed at the same time. After all the HCl gas is released, the system is heated When the temperature reaches 50°C, use a water pump with an alkali absorption device in the middle to perform vacuum extraction to extract the remaining HF gas from the system. After the extraction is completed, the system is distilled under reduced pressure to obtain ...

Example Embodiment

[0032] Example 2

[0033] Under normal pressure, a total of 181 g of bisfluorosulfonimide was added to a 500 mL reaction flask, and a total of 400 g of anhydrous dichloromethane was added, and the bisfluorosulfonimide was dissolved into a homogeneous system with stirring. Place the system in a cold water bath. When the temperature of the system drops below 20℃, add a total of 180g of thionyl chloride, stir for 1h, weigh out 38g of lithium carbonate solid, and add it to the reaction system in batches. At the same time, control the system temperature well to ensure that the system temperature does not exceed 30°C. After the addition of the lithium carbonate is complete, continue to stir and react for 3 hours, during which the temperature is maintained between 20°C and 30°C. After the reaction is completed, a solid filter cake is obtained by filtration, and the solid is transferred to the reaction flask with a total of 1200g of anhydrous dichloromethane Washed three times, and fina...

Example Embodiment

[0035] Example 3

[0036] Under normal pressure, a total of 181 g of bisfluorosulfonimide was added to a 500 mL reaction flask, a total of 400 g of anhydrous toluene was added, and the bisfluorosulfonimide was dissolved into a homogeneous system with stirring. Place the system in a cold water bath. When the temperature of the system drops below 20°C, add a total of 180g of thionyl chloride, stir for 1h, weigh out 25.5g of anhydrous lithium hydroxide solid, and add them to the reaction system in batches. When adding lithium hydroxide, control the system temperature at the same time to ensure that the system temperature does not exceed 30°C. After the addition of the lithium hydroxide is completed, continue to stir the reaction for 3 hours, during which the temperature is maintained between 20°C and 30°C. After the reaction is completed, a solid filter cake is obtained by filtration, and the solid is transferred to the reaction flask and washed with a total of 1200g of anhydrous to...

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Abstract

The invention discloses a lithium bis(fluorosulfonyl)imide preparation method. The method comprises the following steps that 1, BCSA is introduced into anhydrous hydrogen fluoride gas, and bis(fluorosulfonyl)imide is obtained; 2, bis(fluorosulfonyl)imide is mixed with a first organic solvent, a water removal agent is added, the mixture is mixed to be uniform, lithium salt is added, a reaction is conducted, after the reaction is completed, filtration is conducted, and a crude lithium bis(fluorosulfonyl)imide product is obtained; 3, the crude lithium bis(fluorosulfonyl)imide product is cleaned with a second organic solvent, the first organic solvent is added, purification is conducted, and lithium bis(fluorosulfonyl)imide granules are obtained. Accordingly, when a fluorination reaction is conducted, hydrogen fluoride serves as a fluorinated reagent and a solvent, the solvent cost and steps of recycling and the like are omitted, the method has the advantages that the cost is low, raw materials are easy to obtain, HCl gas generated through the reaction can only need to be absorbed with alkali liquor, and after the reaction is completed, the high-purity bis(fluorosulfonyl)imide can be obtained in a reduced pressure distillation mode.

Description

technical field [0001] The invention belongs to the technical field of lithium batteries, and in particular relates to a preparation method of bisfluorosulfonyl imide lithium salt. 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. Fluorine is the most electronegative element in the periodic table of elements, adding fluorine to the compound can often change its physical and chemical properties greatly. Because of this, many fluorine-containing lithium compounds are used in batteries to improve the performance of batteries, such as lithium hexafluorophosphate (LiPF 6 ) and lithium bis(trifluoromethyl)sulfonylimide (LiTFSI), etc. US Patent US5916475 discloses a LiPF 6 LiTFSI and LiTFSI have better thermal and chemical stabi...

Claims

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Application Information

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IPC IPC(8): C01B21/086
Inventor 张忠如杨勇
Owner XIAMEN UNIV
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