Methods for preparing phosphorus pentafluoride gas and preparing lithium hexafluorophosphate using the gas
A technology of phosphorus pentafluoride and phosphorus pentachloride is applied in chemical instruments and methods, phosphorus halide/oxyhalide, inorganic chemistry and other directions, can solve the problem of low yield of lithium hexafluorophosphate, etc., and achieves low production cost, low purity, high purity effect
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preparation example Construction
[0026] According to the present invention, the specific preparation method of phosphorus pentafluoride includes: at minus 50- minus 10° C., mixing phosphorus pentachloride with a solvent and stirring uniformly to obtain a phosphorus pentachloride solution, and then, under the protection of an inert gas , in contacting anhydrous hydrogen fluoride gas with phosphorus pentachloride solution for 2-6 hours.
[0027] The specific preparation method of the lithium hexafluorophosphate includes: at minus 50- minus 10 ℃, mixing solid lithium fluoride with a solvent to obtain a lithium fluoride solution, and under the protection of an inert gas, contacting phosphorus pentafluoride gas with the lithium fluoride solution React for 2.5-6 hours.
[0028] Preferably, the above two reactions can be carried out in two reaction devices respectively, and the two reactions can be carried out simultaneously, for example, the reaction for preparing phosphorus pentafluoride is carried out in reactor ...
Embodiment 1
[0033] This example is used to illustrate the preparation of phosphorus pentafluoride and lithium hexafluorophosphate provided by the present invention.
[0034] (1) 20 liters of acetonitrile solvent (relative density of acetonitrile (water = 1 g / cm) 3 ) is 0.79 g / cm 3 ) and 0.8 kg of solid lithium fluoride were added to a 100-liter cylindrical reaction device B (made of carbon steel material; can withstand a pressure of 0.5 MPa and a low temperature of minus 50 ° C; aspect ratio 1.2), and fully stirred to form a suspension for use (the mass ratio of lithium fluoride to acetonitrile is 0.05:1).
[0035] (2) 21.3 liters of acetonitrile solvent and 9.25 kilograms of phosphorus pentachloride were added to a 100 liter cylindrical reaction device A (made of carbon steel material; 0.5 MPa pressure and minus 50 liters) lined with PTFE ℃ of low temperature; the aspect ratio is 1.2), and stir to completely dissolve the phosphorus pentachloride to form a phosphorus pentachloride solut...
Embodiment 2
[0040] This example is used to illustrate the preparation of phosphorus pentafluoride and lithium hexafluorophosphate provided by the present invention.
[0041] (1) 25 liters of acetonitrile solvent and 1.5 kg of solid lithium fluoride were added to a 100-liter cylindrical reaction device B (made of carbon steel material; it can withstand a pressure of 0.5 MPa and minus 50 ℃ of low temperature; the aspect ratio is 1.2), and fully stirred to form a suspension for use (the mass ratio of lithium fluoride and acetonitrile is 0.075:1).
[0042] (2) 59.0 liters of acetonitrile solvent and 26.0 kg of phosphorus pentachloride were added to a 100-liter cylindrical reaction device A (made of carbon steel material; it can withstand a pressure of 0.5 MPa and minus 50 ℃ of low temperature; the aspect ratio is 1.2), and stir to completely dissolve the phosphorus pentachloride to form a phosphorus pentachloride solution (the mass ratio of phosphorus pentachloride and acetonitrile is 0.55:1)...
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