Method for preparing lithium bis (fluorosulfonyl) imide by using organic metal lithium reagent

A technology for lithium bisfluorosulfonimide and fluorosulfonimide acid is applied in the field of preparing lithium bisfluorosulfonimide, which can solve the problems of difficulty in using conventional storage equipment, increase in storage cost and the like, and achieve high yield , The effect of stable product quality

Inactive Publication Date: 2020-08-25
LEE & MAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the liquid hydrogen fluoride required for this method requires special equipment for storage, so this method also has the problem of being difficult to implement with conventional storage equipment, which leads to increased storage costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take a 100mL solvent storage bottle (bottle A) and transfer 33.2mL of 1mol / L (ethyllithium / benzene) solution for use. Take another 50mL solvent storage bottle (bottle B) and transfer 5g of HFSI and 15g of benzene into it, mix well, and set aside. Prepare a 250mL reaction flask, first add 30ml of benzene and a stirrer into the flask, and cool to -10°C, then slowly drop the solutions in bottle A and bottle B into the reaction bottle through capillary tubes to start the reaction. The reaction temperature was maintained at -10°C. The dropwise addition was completed in about 2 hours, after the dropwise addition was completed. The reaction was continued for 1 hour. After the reaction is complete, stop stirring and return to room temperature. At this time, solids will precipitate at the bottom of the bottle. Pour the reaction solvent benzene into a 1000ml bottle (bottle D). The solid was then washed 5 times with 30 mL of benzene. The washing liquid is also collected in bot...

Embodiment 2

[0033]Take a 100mL solvent storage bottle (bottle A) and transfer 21.6mL of 1.6mol / L (n-butyllithium / n-hexane) solution for use. Take another 50mL solvent storage bottle (bottle B) and transfer 5g of HFSI and 15g of n-hexane, mix well, and set aside. Prepare a 250mL reaction bottle, first add 30ml of n-hexane and a stirrer into the bottle, and cool to -15°C, then slowly drop the solutions of bottle A and bottle B into the reaction bottle through capillary tubes to start the reaction. The reaction temperature was maintained at -15°C. The dropwise addition was completed in about 3 hours, after the dropwise addition was completed. The reaction was continued for 1 hour. After the reaction is complete, stop stirring and return to room temperature. At this time, solids will precipitate at the bottom of the bottle. Pour the reaction solvent n-hexane into a 1000ml bottle (bottle D). The solid was then washed 5 times with 30 mL of n-hexane. The washing liquid is also collected in b...

Embodiment 3

[0035] Take a 100mL solvent storage bottle (bottle A) and transfer 21.6mL of 1.6mol / L (phenyllithium / cyclohexane) solution for use. Take another 50mL solvent storage bottle (bottle B) and transfer 5g of HFSI and 15g of cyclohexane, mix well, and set aside. Prepare a 250mL reaction flask, first add 30ml cyclohexane and a stirrer to the flask, and cool to -20°C, then slowly drop the solutions in bottle A and bottle B into the reaction bottle through capillary tubes to start the reaction. The reaction temperature was maintained at -20°C. The dropwise addition was completed in about 2 hours, after the dropwise addition was completed. The reaction was continued for 2 hours. After the reaction is complete, stop stirring and return to room temperature. At this time, solids will precipitate at the bottom of the bottle. Pour the reaction solvent cyclohexane into a 1000ml bottle (bottle D). The solid was then washed 5 times with 30 mL of cyclohexane. The washing liquid is also colle...

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PUM

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Abstract

The invention discloses a method for preparing lithium bis (fluorosulfonyl) imide by using an organic metal lithium reagent. The method comprises the following steps: S1, using the organic metal lithium reagent as a raw material, carrying out mixed reaction with bis (fluorosulfonyl) imide acid to obtain a lithium bis (fluorosulfonyl) imide crude product; S2, performing vacuum pumping on the crudeproduct, adding a poor organic solvent of lithium bis (fluorosulfonyl) imide for multiple times of washing, and then performing vacuum pumping to obtain a solid; and S3, adding an organic solvent intothe solid, extracting, filtering, concentrating, adding a low-polarity aprotic solvent into the concentrated solution, standing, crystallizing, filtering, and carrying out vacuum drying on the crystal to obtain the lithium bis (fluorosulfonyl) imide. The preparation steps are carried out without water under the protection of inert gas. According to the preparation method, high-purity lithium bis(fluorosulfonyl) imide can be prepared, the yield is high, the product quality is stable, and the content of impurities such as potassium ions, sodium ions, calcium ions, fluorine ions, chloride ions,sulfate ions and water in the product is effectively reduced.

Description

technical field [0001] The invention relates to a method for preparing lithium bisfluorosulfonyl imide by using an organometallic lithium reagent. Background technique [0002] Lithium bisfluorosulfonyl imide can be used in many fields, for example, it can be used as an electrolyte additive for secondary 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 catalyst for polymerization reactions; it can also be used It is used as an antistatic agent in the industrial field. 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 lithium bisfluorosulfonyl imide has better stability, and its low temperature performance is excellent, and hydrolysis resistance is good, so lithium bisfluorosulfonyl imide h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/096C01B21/086
CPCC01B21/086C01B21/096C01P2006/80
Inventor 梁海波谢文健苏秋铭张梦辛伟贤陈新滋
Owner LEE & MAN CHEM CO LTD
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