Method for preparing lithium fluorosulfonate by using organic metal lithium reagent

A lithium fluorosulfonate, organometallic technology, applied in the directions of alkali metal compounds, chemical instruments and methods, lithium halide, etc., to achieve the effect of high yield and stable product quality

Active Publication Date: 2021-04-30
LEE & MAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since none of these patents mentioned the preparation method using metal organic lithium reagent as lithium source, the present invention pr

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Take a 100mL solvent storage bottle (bottle A) and transfer 60mL (0.06mol) of 1mol / L (ethyllithium / benzene) solution, and set aside. Take another 100mL solvent storage bottle (bottle B) and transfer 5g (0.05mol) of fluorosulfonic acid and 50mL of perfluorohexane, mix thoroughly, and set aside. Prepare a 1000mL reaction bottle, first add 50mL perfluorohexane and a stirrer to the bottle, and cool to -10°C, then slowly drop the bottle A and bottle B solutions into the 1000mL reaction bottle through the capillary to start the reaction. The reaction temperature was maintained at -10°C. The dropwise addition was completed in about 2.5 hours, after the dropwise addition was completed. The reaction was continued for 1 hour. After the reaction is complete, stop stirring and slowly return to room temperature. At this time, solids will precipitate at the bottom of the bottle, and the reaction solvent is poured out of a 1000ml bottle (bottle D). The solid was then washed with pe...

Embodiment 2

[0038]Take a 100mL solvent storage bottle (bottle A) and transfer 39.1mL (0.0625mol) of a 1.6mol / L (n-butyllithium / n-hexane) solution for use. Take another 100mL solvent storage bottle (bottle B) and transfer 5g (0.05mol) of fluorosulfonic acid and 50mL of perfluorohexane, mix thoroughly, and set aside. Prepare a 1000mL reaction bottle, first add 50ml perfluorohexane and a stirrer to the bottle, and cool to -15°C, then slowly drop the solution from bottle A and bottle B into the reaction bottle through a capillary tube 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 slowly return to room temperature. At this time, solids will precipitate at the bottom of the bottle, and the reaction solvent perfluorohexane is poured out of a 1000ml bottle (bottle D). The solid was th...

Embodiment 3

[0040] Take a 100mL solvent storage bottle (bottle A) and transfer 35.9mL (0.0575mol) of a 1.6mol / L (phenyllithium / cyclohexane) solution for use. Take another 100mL solvent storage bottle (bottle B) and transfer 5g (0.05mol) of fluorosulfonic acid and 50mL of perfluorohexane, mix thoroughly, and set aside. Prepare a 1000mL reaction bottle, first add 50mL perfluorohexane and a stirrer to the bottle, and cool to -20°C, then slowly drop the bottle A and bottle B solutions into the reaction bottle through the capillary 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 was completed, stop stirring and return to room temperature. At this time, solids would precipitate at the bottom of the bottle, and the reaction solvent cyclohexane was poured out of a 1000ml bottle (bottle D). The solid was then washed ...

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PUM

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Abstract

The invention discloses a method for preparing lithium fluorosulfonate by using an organometallic lithium reagent, which comprises the following steps: (1) slowly mixing and reacting the organometallic lithium reagent serving as a lithium source with fluorosulfonic acid under a low-temperature condition in the presence of perfluorohexane serving as a solvent to obtain a lithium fluorosulfonate crude product; and washing the crude product with a reaction solvent for 5 times; (2) carrying out vacuum pumping on the crude product, adding a poor organic solvent of lithium fluorosulfonate, washing for three times, and carrying out vacuum pumping on the poor organic solvent to obtain a solid; (3) adding carbonate, nitrile and alcohol organic solvents into the solid, extracting, filtering, concentrating, adding a low-polarity aprotic solvent into the concentrated solution, and carrying out static crystallization; and (4) filtering the crystals again, and carrying out vacuum drying to obtain the lithium fluorosulfonate product. The preparation steps are carried out without water under the protection of inert gas. According to the preparation method provided by the invention, the lithium fluorosulfonate 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, sulfate ions and water in the product can be effectively reduced.

Description

technical field [0001] The invention relates to a method for preparing lithium fluorosulfonate by using an organic metal lithium reagent, belonging to the technical field of chemical synthesis. Background technique [0002] 1. Lithium fluorosulfonate abbreviated as LiFSO 3 , the molecular weight is 106.1. Pure lithium fluorosulfonate is a white solid. It is a chemical substance that can be widely used in the field of electronic batteries. It is widely used and high-purity lithium fluorosulfonate is suitable for non-aqueous electrolyte additives for secondary lithium-ion batteries. It has the characteristics of electrochemical stability and thermal stability in the electrolyte, which can improve the cycle performance and high-temperature storage performance of the secondary lithium-ion battery, and can inhibit the gas production of the electrolyte during use, thereby improving the secondary lithium-ion battery. In some fields, it has been shown that it will replace electro...

Claims

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Application Information

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IPC IPC(8): C01D15/00
CPCC01D15/00C01D15/04
Inventor 梁海波谢文健苏秋铭辛伟贤陈新滋
Owner LEE & MAN CHEM CO LTD
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