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
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[0039] Example 1
[0040] In a dry and airtight atmosphere with a water content of less than 10ppm, use anhydrous CO in the reactor 2 After replacing the gas for many times, add lithium fluoride and liquid carbon dioxide into the reaction vessel according to the mass ratio of 1:8 and stir to keep the temperature in the reactor lower than CO. 2 Critical temperature, and a certain pressure to maintain CO 2 In this embodiment, the temperature in the reactor is kept below room temperature 20°C and the pressure is 8MPa, and then PF is added to the reaction vessel 5 Gas, the molar ratio of lithium fluoride to phosphorus pentafluoride is 1:1.5, and then the reaction temperature is controlled to -12°C and the pressure is 5MPa. After the reaction is completed, the reactor temperature is increased to room temperature (20°C), The pressure is reduced to normal pressure (1atm), and excess phosphorus pentafluoride gas and CO are discharged 2 Gas, collect the resulting lithium hexafluorophosphate...
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[0041] Example 2
[0042] In a dry and airtight atmosphere with a water content of less than 10ppm, use anhydrous CO in the reactor 2 After replacing the gas for many times, add lithium fluoride and liquid carbon dioxide into the reaction vessel according to the mass ratio of 1:20 and stir to keep the temperature in the reactor lower than 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 added lithium fluoride to phosphorus pentafluoride is 1:1.03, the reaction temperature is controlled at 5°C and the pressure is 6MPa. After the reaction is completed, the reactor temperature is increased to room temperature and the pressure is reduced to normal pressure. Exhaust excess phosphorus pentafluoride gas and CO 2 Gas, collect the resulting lithium hexafluorophosphate product.
Example Embodiment
[0043] Example 3
[0044] In a dry and airtight atmosphere with a water content of less than 10ppm, use anhydrous CO in the reactor 2 After replacing the gas for many times, add lithium fluoride and liquid carbon dioxide into the reaction vessel according to the mass ratio of 1:45 and stir to keep the temperature in the reactor lower than 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 is 1:6, the reaction temperature is controlled to 26℃, the pressure is 10MPa, after the reaction is over, the reactor pressure is reduced to normal pressure (the temperature can also be reduced at the same time) To room temperature), discharge excess phosphorus pentafluoride gas and CO 2 Gas, collect the resulting lithium hexafluorophosphate product.
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