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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 conducive to subsequent use (CN104085864)
There is also a method of dissolving first, then performing a series of treatments, then removing the dry solvent, and finally adding other solvents. The process is complicated and affects the yield (CN106241757)

Method used

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  • Lithium bis(fluorosulfonyl)imide preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add a total of 1020g of dichlorosulfonimide into a 1000mL reaction bottle, and blow nitrogen to make the whole system under the protective atmosphere of nitrogen and anhydrous conditions. Under normal pressure, start stirring, and heat the system to 75-85°C for 6 hours. , the solid bischlorosulfonimide in the system gradually melted into a liquid state. In the state of stirring, a total of 400 g of anhydrous HF gas was slowly introduced. After a total of about 6 hours of reaction, the system was gradually cooled to room temperature, and the gas in the system was released. The generated white smoke HCl gas was absorbed with lye, and the excess HF was absorbed at the same time. After all the HCl gas was released, the system was heated up. To 50°C, use a water pump with an alkali absorption device in the middle to carry out decompression extraction to extract the residual HF gas in the system. After the extraction was completed, the system was distilled under reduced pres...

Embodiment 2

[0033] Under normal pressure, add a total of 181 g of bisfluorosulfonimide to a 500 mL reaction bottle, add a total of 400 g of anhydrous dichloromethane, and stir to dissolve the bisfluorosulfonimide into a homogeneous system. Place the system in a cold water bath, and when the temperature of the system drops below 20°C, add a total of 180 g of thionyl chloride, stir for 1 hour, weigh a total of 38 g of lithium carbonate solids, and add them to the reaction system in batches. After adding lithium carbonate At the same time, control the system temperature to ensure that the system temperature does not exceed 30 °C. After the addition of lithium carbonate is completed, 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, filter the solid filter cake, transfer the solid to the reaction bottle, and use a total of 1200g of anhydrous dichloromethane Washed 3 times, and finally filtered to obtain a...

Embodiment 3

[0036]Under normal pressure, add a total of 181 g of bisfluorosulfonimide to a 500 mL reaction bottle, add a total of 400 g of anhydrous toluene, and stir to dissolve the bisfluorosulfonimide into a homogeneous system. Place the system in a cold water bath, and when the temperature of the system drops below 20°C, add a total of 180 g of thionyl chloride, stir for 1 hour, weigh a total of 25.5 g of anhydrous lithium hydroxide solid, and add it to the reaction system in batches. When adding lithium hydroxide, control the temperature of the system at the same time to ensure that the temperature of the system does not exceed 30°C. After the lithium hydroxide is added, continue to stir and react for 3 hours while maintaining the temperature between 20°C and 30°C. After the reaction, filter the solid filter cake, transfer the solid to the reaction bottle, and wash with a total of 1200g of anhydrous toluene 3 times, and finally filtered to obtain a filter cake, and after drying, a 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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