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Preparation method of lithium fluorosulfonate

A technology of lithium fluorosulfonate and fluorosulfonic acid, applied in the field of preparation of lithium fluorosulfonate, can solve the problems of irritation and corrosiveness, unfavorable post-processing purification, raw material limitation, etc., and achieves high safety and high product yield , The effect of reasonable production cost

Active Publication Date: 2021-04-30
ZHUHAI LEE & MAN MATERIALS SCI CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although fluorosulfonic acid can react with various lithium salts to prepare lithium fluorosulfonic acid, the raw material fluorosulfonic acid is a kind of high-risk chemical, which is highly irritating and corrosive, and white smoke will come out when exposed to the air. Hydrogen fluoride gas is released by the reaction of water vapor, which is extremely harmful
If the reaction uses an organic lithium salt as a raw material, the organic matter produced by the reaction will be fluorinated by fluorosulfonic acid immediately to produce a side reaction, and a large amount of impurities will be produced, which is not conducive to the post-treatment purification in the next step, so it can only be limited to the use of inorganic lithium as the raw material. raw material
Therefore, there are certain raw material limitations in this method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Purification of Potassium Fluorosulfonate:

[0031] Under inert gas protection, in 1000mL bottle, add 100g (0.724mol) potassium fluorosulfonate salt KFSO3 (M=138.16) (CAS: 13455-22-6) (CAS: 13455-22-6) of market purchase, first add 400mL ethylene glycol monomethyl ether as The solvent is stirred and dissolved completely, then add 400mL of ethyl acetate and continue to stir to produce some insolubles, filter the insolubles, concentrate the filtrate under reduced pressure until a small amount of solids appear, return to normal pressure, then add 500ml of dichloromethane and The temperature of the solution was lowered to -15°C, and the crystal was obtained by standing still for 24 hours. After separation, the crystal was washed with dichloromethane, and finally the solid was vacuum-dried to obtain a white powder of potassium fluorosulfonate with a purity ≥ 98.5%.

[0032] (2) Purification of sodium fluorosulfonate:

[0033] Under the protection of an inert gas, add 10...

Embodiment 2

[0035] Under the protection of an inert gas, in a 500mL reaction flask, place 30.38g (0.2mol) of lithium hexafluorophosphate (M=151.91) dissolved in 150mL of methanol, control the temperature to 40°C, and add dropwise 30.40g (0.22mol) of lithium hexafluorophosphate (M=151.91) dissolved in 200mL of methanol Potassium fluorosulfonate (KFSO 3 ), the dropwise addition process generates potassium hexafluorophosphate precipitation, continue to stir for 8 hours after the dropwise addition, and then adopt decompression vacuum to dry the reaction solvent. After the solid was obtained, 250 mL of dimethyl carbonate was added to dissolve it, and potassium hexafluorophosphate was removed by filtration. After the obtained filtrate was concentrated to a slurry state, 300 mL of dichloromethane was added for static crystallization, and a white solid product was precipitated. After filtration and vacuum drying, 18.59 g lithium fluorosulfonate, yield 87.6%. (Test result: ICP-OES (ppm): Na + =2...

Embodiment 3

[0037]Under the protection of an inert gas, in a 500mL reaction flask, place 37.80g (0.2mol) of lithium saccharin dissolved in 100mL of acetonitrile, control the temperature to 30°C, and add dropwise 26.85g (0.22mol) of sodium fluorosulfonate dissolved in 250mL of acetonitrile under stirring Salt (NaFSO 3 ), the dropwise addition process generates sodium saccharin precipitation, after the dropwise addition is completed, continue to stir for 16 hours, and then adopt decompression vacuum to dry the reaction solvent. After obtaining the solid, add 250 mL of dimethyl carbonate to dissolve and filter to remove sodium saccharin. After the obtained filtrate is concentrated to a slurry state, add 300 mL of dichloroethane for static crystallization, and a white solid product is precipitated. After filtration and vacuum drying, 18.95 g is obtained Lithium fluorosulfonate, yield 89.3%. (Test result: ICP-OES (ppm): Na + =48.6ppm, K + =8.9ppm, Fe 2 + = 2.1ppm, Ca 2+ =15.8ppm; IC: F ...

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Abstract

The invention discloses a preparation method of lithium fluorosulfonate, which comprises the following steps: (1) taking metal fluorosulfonate (MFSO3) with the purity of >=98.5% as a raw material, and carrying out metathesis exchange reaction with organic lithium salt in an ester, alcohol, nitrile or amide solvent; (2) generating insoluble organic metal salt precipitate, pumping in vacuum, extracting by using a poor solvent of an organic metal salt, filtering, separating, concentrating under reduced pressure, adding a low-polarity aprotic solvent into the concentrated solution, standing, crystallizing, and carrying out vacuum drying to obtain the high-purity lithium fluorosulfonate product. The preparation method of the high-purity lithium fluorosulfonate is simple in post-reaction treatment method, high in product yield, high in purity and capable of effectively reducing the content of impurities such as potassium ions, sodium ions, calcium ions, chloride ions and moisture in the product. The preparation method provided by the invention has the characteristics of simple operation steps, reasonable production cost, high safety, wide substrate selection range, low cost and high product purity.

Description

technical field [0001] The invention relates to a preparation method of lithium fluorosulfonate, which belongs 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 electrolytic additives that seriously pollut...

Claims

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Application Information

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IPC IPC(8): C01D15/04H01M10/0567H01M10/0525
CPCC01D15/04H01M10/0567H01M10/0525C01P2006/80H01M10/0568C01D15/00Y02E60/10
Inventor 梁海波辛伟贤谢文健陈志强陈新滋
Owner ZHUHAI LEE & MAN MATERIALS SCI CO LTD
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