Preparation method of lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and lithium fluoride, used in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc.

Inactive Publication Date: 2012-03-21
四川省黄铭锂能源新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a lithium hexafluorophosphate A hydrofluoric acid-free preparation method, the lithium hexafluorophosphate prepared by this method has high purity, low water content, low content of free acid and metal impurities

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Dissolve and disperse 142 g of phosphorus pentoxide solid in 500 ml of dimethyl carbonate, add 480 g of sodium fluoride solid, stir and control the reaction temperature at 10°C, react to obtain phosphorus pentafluoride gas, dry and mix with The lithium fluoride suspension formed by suspending 28g of lithium fluoride solid in 500 ml of dimethyl carbonate organic solvent was fully reacted and enriched, and kept at a temperature of 5°C, stirred for 3 hours to obtain a clear solution; then the clear solution was evaporated, concentrated and separated Obtain white crystals, and dry them in vacuum at 70°C and 0.5 MPa for 3 hours; redissolve the resulting solids in 500 ml of dimethyl carbonate to obtain a clear solution, concentrate and separate the clear solution to obtain white crystals, and dry them at 70°C, Dry in vacuum at 0.5 MPa for 3 hours to obtain high-purity lithium hexafluorophosphate.

Embodiment 2

[0022] Dissolve and disperse 158 g of phosphorus pentoxide solid in 700 ml of cyclohexane, add 600 g of calcium fluoride solid, stir and control the reaction temperature at 240 ° C, react to obtain phosphorus pentafluoride gas, dry and mix with 29 The lithium fluoride suspension formed by suspending g lithium fluoride solid in 500 ml dimethyl carbonate organic solvent was fully reacted and enriched and kept at a temperature of 5°C, stirred for 4 hours to obtain a clear solution, and then the clear solution was separated to obtain white crystals , and dried at 80°C and 0.7 MPa vacuum for 3 hours, and the resulting solid was redissolved in 500 ml of dimethyl carbonate to obtain a clear solution. The clear solution was concentrated and separated to obtain white crystals. Dry for 3 hours to obtain high-purity lithium hexafluorophosphate.

Embodiment 3

[0024] Dissolve and disperse 142 g of phosphorus pentoxide solids in 1000 ml of diethyl carbonate, add 480 g of ammonium fluoride solids, stir and control the reaction temperature at -30°C, react to obtain phosphorus pentafluoride gas, dry and mix with The lithium fluoride suspension formed by suspending 26 g of lithium fluoride solid in 800 ml of diethyl carbonate organic solvent was fully reacted and enriched, and the reaction temperature was kept at 120 ° C and stirred for 5 hours to obtain a clear solution; then the clear solution was White crystals were isolated and dried at 80°C and 0.2 MPa in vacuum for 3 hours; the resulting solids were redissolved in 800 ml of diethyl carbonate organic solution to obtain a clear solution, which was concentrated by evaporation and separated to obtain white crystals , and dried at 80°C and 0.2 MPa vacuum for 3 hours to obtain high-purity lithium hexafluorophosphate.

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Abstract

The invention discloses a preparation method of lithium hexafluorophosphate, comprising the following steps of: (1) dissolving a phosphorus pentoxide solid and dispersing in an organic solvent to prepare a mixed solution with the phosphorus pentoxide content of 1-100wt%, adding a fluorine compound with fluorine and phosphorus in the mass ratio of (4.0-6.0):1, controlling the reaction temperature between 30 DEG C below zero and 240 DEG C to prepare a phosphorus pentafluoride gas and drying; (2) suspending a lithium fluoride solid in the organic solvent to prepare a lithium fluoride suspension with fluorine and phosphorus in the mass ratio of 1: (0.5-2); (3) sufficiently reacting and enriching the prepared phosphorus pentafluoride gas and the lithium fluoride suspension; (4) concentrating and separating to obtain a solid and drying; (5) saturating and dissolving the dried solid in the organic solvent to obtain a clear solution; and (6) repeating the step (4) to obtain the lithium hexafluorophosphate. The lithium hexafluorophosphate prepared by using the method provided by the invention has high purification, small water content and low content of free acid and metal impurities.

Description

technical field [0001] The invention relates to a preparation method of lithium hexafluorophosphate. Background technique [0002] Lithium-ion batteries have the advantages of high platform voltage, good cycle performance, wide operating temperature range, high energy density, and no memory effect. They are widely used in mobile communications, portable electronic products, power tools, and weapon assembly. They are currently used in power vehicles It also has broad application prospects. Electrolyte and its electrolyte are the key raw materials of lithium batteries and directly affect the performance of the prepared battery. Therefore, the electrolyte must meet the following requirements: high electrical conductivity, stable chemical and electrochemical properties, wide usable temperature range and low price. Lithium hexafluorophosphate meets the above requirements and can be used as an excellent electrolyte, but lithium hexafluorophosphate products must be subject to stri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455
Inventor 黄铭黄博
Owner 四川省黄铭锂能源新材料有限公司
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