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Preparation method of lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and lithium fluoride, applied in lithium hexafluorophosphate, chemical instruments and methods, lithium compounds, etc., can solve the problems of complex processing technology and difficult product purification, and achieve the effect of simple subsequent processing, resource saving and high purity

Active Publication Date: 2018-02-16
上海绿麟达新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the various solvents that use in the preparation method of existing lithium hexafluorophosphate, although each has advantages but also has unavoidable shortcoming
For example, the organic solvent method should finally obtain LiPF 6 The product also needs to go through processes such as crystallization, separation, low-temperature negative pressure evaporation to remove solvent, recrystallization, and vacuum drying. The subsequent treatment process is complicated, and the removal of impurities and product purification are difficult.

Method used

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  • Preparation method of lithium hexafluorophosphate

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Effect test

Embodiment 1

[0040] In a dry airtight atmosphere with a water content of less than 10ppm, the reactor was filled with anhydrous CO 2 After the gas has been replaced many times, lithium fluoride and liquid carbon dioxide are added to the reaction vessel at a mass ratio of 1:8 and stirred, and the temperature in the reactor is always kept lower than that of CO 2 critical temperature, and a certain pressure to maintain CO 2 In this embodiment, the temperature in the reactor is maintained at 20°C lower than room temperature, and the pressure is 8MPa, and then PF is added to the reaction vessel 5 Gas, the molar ratio of lithium fluoride and phosphorus pentafluoride added is 1:1.5, and then the reaction temperature is controlled at -12°C and the pressure is 5MPa. After the reaction is completed, the temperature of the reactor is raised to room temperature (20°C). The pressure is reduced to normal pressure (1atm), and the excess phosphorus pentafluoride gas and CO are discharged 2 gas, and the ...

Embodiment 2

[0042] In a dry airtight atmosphere with a water content of less than 10ppm, the reactor was filled with anhydrous CO 2 After the gas has been replaced many times, lithium fluoride and liquid carbon dioxide are added to the reaction vessel at a mass ratio of 1:20 and stirred, and the temperature in the reactor is always kept lower than that of CO 2 critical temperature, and a certain pressure to maintain CO 2 liquid state, and then add PF to the reaction vessel 5 Gas, the molar ratio of lithium fluoride to phosphorus pentafluoride added is 1:1.03, the reaction temperature is controlled at 5°C, and the pressure is 6MPa. After the reaction is completed, the temperature of the reactor is raised to room temperature, and the pressure is reduced to normal pressure. Exhaust excess phosphorus pentafluoride gas and CO 2 gas, and the resulting lithium hexafluorophosphate product was collected.

Embodiment 3

[0044] In a dry airtight atmosphere with a water content of less than 10ppm, the reactor was filled with anhydrous CO 2 After the gas has been replaced many times, lithium fluoride and liquid carbon dioxide are added to the reaction vessel at a mass ratio of 1:45 and stirred, and the temperature in the reactor is always kept lower than that of CO 2 critical temperature, and a certain pressure to maintain CO 2 liquid state, and then add PF to the reaction vessel 5 Gas, the molar ratio of lithium fluoride to phosphorus pentafluoride added is 1:6, the reaction temperature is controlled at 26°C, and the pressure is 10MPa. to room temperature), discharge excess phosphorus pentafluoride gas and CO 2 gas, and the resulting lithium hexafluorophosphate product was collected.

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Abstract

The invention discloses a preparation method of lithium hexafluorophosphate. According to the preparation method, lithium fluoride reacts with phosphorus pentafluoride, and liquid carbon dioxide or supercritical carbon dioxide fluid is taken as the reaction solvent. The preparation method is green and environmentally friendly, the resources are saved, and the cost is low. The quality of obtained lithium hexafluorophosphate product is good. The product barely contains any impurity that damages lithium hexafluorophosphate taken as cell electrolyte. The purity is high, the production process is safe, and the preparation method is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of lithium hexafluorophosphate, in particular to a preparation method of lithium hexafluorophosphate used as an electrolyte solution for lithium ion batteries. Background technique [0002] As an electrolyte salt, lithium hexafluorophosphate has good application and environmental performance, and is currently the only commercial lithium-ion battery electrolyte. [0003] The preparation methods of lithium hexafluorophosphate mainly include: [0004] 1. Gas-solid reaction method, generally, the gaseous phosphorus halide compound is passed into a container with LiF solid, and the two can directly react to form LiPF 6 . JP2003578279 reacts a lithium source with diammonium hydrogen phosphate to synthesize lithium hexafluorophosphate through a solid-state thermal process. The gas-solid reaction method does not use any solvent, the process is simple, and it is easy to operate, but generally needs to react und...

Claims

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Application Information

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IPC IPC(8): C01D15/00H01M10/0563H01M10/0525
CPCC01D15/005C01P2006/80C01P2006/82H01M10/0525H01M10/0563Y02E60/10Y02P20/54
Inventor 王农跃茅晓晖李国华
Owner 上海绿麟达新材料科技有限公司
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