Methods for preparing phosphorus pentafluoride gas and preparing lithium hexafluorophosphate using the gas
A technology of phosphorus pentafluoride and lithium fluoride, which is applied in the field of preparation of phosphorus pentafluoride gas, can solve the problem of low yield of lithium hexafluorophosphate, and achieve the effects of low production cost, high purity and high production cost
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preparation example Construction
[0026] According to the present invention, the specific preparation method of phosphorus pentafluoride includes: mixing and stirring phosphorus pentachloride and a solvent at minus 50°C to minus 10°C to obtain a phosphorus pentachloride solution, and then, under the protection of an inert gas , in the contact reaction of anhydrous hydrogen fluoride gas and phosphorus pentachloride solution for 2-6 hours.
[0027] The specific preparation method of lithium hexafluorophosphate includes: mixing solid lithium fluoride with a solvent at minus 50°C to minus 10°C 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 (the relative density of acetonitrile (water=1 g / cm 3 ) is 0.79 g / cm 3 ) and 0.8 kg of solid lithium fluoride are added to a cylindrical reaction device B (made of carbon steel material; it can withstand the pressure of 0.5 MPa and the low temperature of minus 50 ℃; the 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 are added to a volume of 100 liters of cylindrical reaction equipment A (prepared by carbon steel materials; can withstand the pressure of 0.5 MPa and minus 50 ℃ low temperature; the aspect ratio is 1.2), and stirred to completely dissolve the phosphorus pentachloride to form a phosphorus pe...
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 kilograms of solid lithium fluoride are added to a cylindrical reaction device B (made of carbon steel material; it can withstand the pressure of 0.5 MPa and minus 50 ℃ low temperature; the aspect ratio is 1.2), and fully stirred to form a suspension for use (the mass ratio of lithium fluoride to acetonitrile is 0.075:1).
[0042] (2) 59.0 liters of acetonitrile solvent and 26.0 kilograms of phosphorus pentachloride are added to a volume of 100 liters of cylindrical reaction equipment A (prepared by carbon steel materials; can withstand the pressure of 0.5 MPa and minus 50 ℃ low temperature; the aspect ratio is 1.2), and stirred to completely dissolve the phosphorus pentachloride to form a phosphorus pentachloride solution (the mass ratio of phosphorus pentachloride to ace...
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