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Preparation method of high-purity imidodisulfuryl fluoride lithium

A technology of fluorosulfonyl and lithium imide is applied in the field of preparation of high-purity lithium bis-imide, which can solve the problems that metal ions are easy to exceed the standard, difficult to separate, and dangerous for lithium perchlorate, and achieves simple operation and increased selectivity. , the effect of easy purification

Active Publication Date: 2018-08-07
LEE & MAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method first lithium tetrafluoroborate and lithium perchlorate cost are higher, secondly lithium perchlorate is more dangerous, makes the safety of reaction not guaranteed, the most important point is because lithium tetrafluoroborate and lithium perchlorate are in solvent There is a large solubility in lithium bis(fluorosulfonyl)imide, which makes it difficult to separate lithium tetrafluoroborate and lithium perchlorate remaining in lithium bis(fluorosulfonyl)imide, resulting in metal ions other than lithium easily exceeding the standard, and difficult to purify

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Under the protection of an inert gas, 12g (0.055mol) of potassium bis(fluorosulfonyl)imide with a purity of ≥99.9% and 8.19g (0.046mol) of lithium p-toluenesulfonate with a purity of ≥99.9% were added to a 250mL reaction flask. Add 100mL of methanol into the reaction bottle, the solid in the reaction bottle first dissolves and becomes clear, and a large amount of white solid is formed immediately, keep mechanical stirring at 25°C, and react for 2h. After the reaction, filter the insoluble matter, take the filtrate, heat it under reduced pressure at 600Pa to 40°C, concentrate the filtrate to 1 / 5 of the original volume, wait for the concentrated liquid to cool to room temperature, add 40 mL of tert-butyl methyl ether to the concentrated liquid, and dissolve a little The product was filtered, the filtrate was concentrated, and then 60 mL of poor organic solvent dichloromethane was added dropwise for recrystallization, then filtered, and vacuum-dried to obtain 7.05 g of whit...

Embodiment 2

[0034]Under the protection of an inert gas, 9.338g (0.046mol) of sodium bis(fluorosulfonyl)imide with a purity of ≥99.9% and 4.69g (0.046mol) of lithium methanesulfonate with a purity of ≥99.9% were added to a 250mL reaction flask, Dissolve with 80mL of acetonitrile, the solid in the reaction bottle first dissolves and becomes clear, and immediately a large amount of white solid is formed, keep mechanical stirring at 25°C, and react for 1.5h. After the reaction, filter the insoluble matter, take the filtrate, heat it under reduced pressure at 600Pa to 40°C, concentrate the filtrate to 1 / 5 of the original volume, wait for the concentrated liquid to cool to room temperature, add 30 mL of ether to the concentrated liquid, and filter a little insoluble matter , concentrated the filtrate, then added 60 mL of poor organic solvent dichloromethane dropwise for recrystallization, filtered again, and dried in vacuo to obtain 7.31 g of white solid powder lithium bis(fluorosulfonyl)imide, ...

Embodiment 3

[0036] Under the protection of an inert gas, 13.14g (0.046mol) of silver bis(fluorosulfonyl)imide with a purity of ≥99.9% and 6.9g (0.046mol) of lithium trifluoromethanesulfonate with a purity of ≥99.9% were added to a 250mL reaction flask , Dissolved with 100mL of ethanol, the solid in the reaction bottle first dissolved and became clear, and a large amount of white solid was formed immediately. At 25°C, keep mechanical stirring, and react for 1.5h. After the reaction, filter the insoluble matter, take the filtrate, heat it under reduced pressure at 600Pa to 40°C, concentrate the filtrate to 1 / 5 of the original volume, wait for the concentrated liquid to cool to room temperature, add 30 mL of THF to the concentrated liquid, and dissolve a little of the insoluble matter Filter, concentrate the filtrate, add 60 mL of poor organic solvent dichloromethane dropwise for recrystallization, filter again, and dry in vacuum to obtain 7.48 g of white solid powder lithium bis(fluorosulfon...

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Abstract

The invention discloses a preparation method of high-purity imidodisulfuryl fluoride lithium. The preparation method includes the steps: taking imidodisulfuryl fluoride salt (MFSI) with the purity higher than or equal to 99.9% as a raw material, and performing replacement reaction on the imidodisulfuryl fluoride salt (MFSI) and lithium sulfonate (RSO3Li) in ester, ketone, alcohol, ether, carbonicester or nitrile reaction solvents to obtain imidodisulfuryl fluoride lithium salt crude solution; filtering and concentrating the crude solution, adding ether organic solvents into concentrated solution, filtering and concentrating the concentrated solution, adding low-polarity non-proton organic solvents into the concentrated solution, and performing standing, crystallization and drying to obtain the high-purity imidodisulfuryl fluoride lithium. R in the lithium sulfonate (RSO3Li) is Ar or CnHxFyOz, n>=1, x, y and z>=0, the R is adjusted according to the solubility of the imidodisulfuryl fluoride salt (MFSI) in reaction solvents. In the preparation steps, anhydrous operation is performed under protection of inert gas. The preparation method has the advantages of simple process, wide substrate selectivity, low cost and high product purity.

Description

technical field [0001] The invention relates to a preparation method of high-purity lithium bis(fluorosulfonyl)imide, belonging to the technical field of chemical synthesis. Background technique [0002] Lithium bis(fluorosulfonyl)imide can be used in various fields, for example, it can be used as an electrolyte additive for lithium-ion batteries to improve the cycle performance of lithium-ion batteries, and it can also be used as an electrolyte for primary batteries; it can be used as a polymerization catalyst; it can also be used It is used as an antistatic agent in the industrial field. [0003] Existing research results have shown that lithium hexafluorophosphate (LiPF 6 ) is currently a relatively successful commercial lithium salt electrolyte, but LiPF 6 Thermal stability and chemical stability are poor, while bis(fluorosulfonyl)imide lithium has better stability, and its low temperature performance is excellent, hydrolytic stability is good, so bis(fluorosulfonyl)im...

Claims

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Application Information

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IPC IPC(8): C01B21/086
CPCC01B21/086C01P2006/80
Inventor 苏秋铭张梦梁海波谢文健辛伟贤陈新滋
Owner LEE & MAN CHEM CO LTD
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