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