Low-temperature synthesis method of high-purity sodium hexafluorophosphate
A technology of sodium hexafluorophosphate and its synthesis method, which is applied in the direction of sodium/potassium compounds, chemical instruments and methods, alkali metal compounds, etc., and can solve the problems that cannot meet the requirements of the development of sodium ion batteries, affect battery safety, and reduce cycle life, etc. problems, to achieve the effect of mild conditions, increase yield, and avoid decomposition
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[0013] As recorded in the background art, the purity of the existing sodium hexafluorophosphate product is low and cannot meet the requirements of further development of sodium ion batteries, and then a low-temperature synthesis method of high-purity sodium hexafluorophosphate is provided, comprising the following steps :
[0014] Dissolve sodium fluoride in Freon solution to obtain a solution;
[0015] Pour phosphorus pentafluoride gas into the solution, return to normal pressure after the low temperature vacuum reaction for a set time, evaporate freon and organic solvent to obtain sodium hexafluorophosphate;
[0016] The low temperature vacuum reaction temperature is -50-10°C, and the vacuum pressure is -0.2-0MPa.
[0017] In some embodiments, the freon is selected from one, two or three of dichlorodifluoromethane, monofluorotrichloromethane, or difluoromonochloromethane.
[0018] Preferably, in the solution, the concentration of sodium fluoride is 0.05-10 mol L -1 .
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Embodiment 1
[0022] A low-temperature synthesis method of high-purity sodium hexafluorophosphate, comprising the steps:
[0023] Dissolve 1moL of sodium fluoride powder in 100mL of dichlorodifluoromethane liquid, and then filter to remove insoluble matter to obtain a solution;
[0024] Add 2moL of phosphorus pentafluoride to the above solution, stir the reaction at 0 °C for 15h under the pressure of -0.1MPa, and then gradually reduce the pressure. After the dichlorodifluoromethane is evaporated, sodium hexafluorophosphate can be obtained. The product, sodium hexafluorophosphate, had a purity of 99.95% and a yield of 93.2%.
Embodiment 2
[0026] A low-temperature synthesis method of high-purity sodium hexafluorophosphate, comprising the steps:
[0027] Dissolve 1moL of sodium fluoride powder in 100mL of fluorotrichloromethane liquid, and then filter to remove insoluble matter to obtain a solution;
[0028] Add 1.2moL of phosphorus pentafluoride to the above solution, stir the reaction at 5 °C for 4h under the pressure of -0.08MPa, and then gradually reduce the pressure. After the monofluorotrichloromethane is evaporated, high purity can be obtained. The sodium hexafluorophosphate product, the purity of sodium hexafluorophosphate was 99.94% and the yield was 92.4%.
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