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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

Pending Publication Date: 2022-07-22
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Excessive impurity content in it will increase the internal resistance of the battery, rapidly decay the capacity, reduce the cycle life, and even affect the safety of the battery
But the contriver finds, the purity of sodium hexafluorophosphate product in the prior art is on the low side, can't meet the requirement of the further development of sodium ion battery

Method used

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preparation example Construction

[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 .

[...

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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Abstract

The invention discloses a low-temperature synthesis method of high-purity sodium hexafluorophosphate, which comprises the following steps: dissolving sodium fluoride in an organic solvent solution of Freon to obtain a solution; introducing phosphorus pentafluoride gas into the solution, carrying out low-temperature vacuum reaction for a set time, recovering to normal pressure, and evaporating Freon and the organic solvent to obtain sodium hexafluorophosphate; the reaction temperature of the low-temperature vacuum is-50 to 10 DEG C, and the reaction pressure is-0.2 to 0 MPa. Freon is adopted as a solvent, conditions are mild, the process is simple, and the cost can be effectively reduced; in addition, the Freon liquid can be evaporated by controlling the pressure, and the purity of the sodium hexafluorophosphate can be greatly improved. The reaction process and the subsequent solvent evaporation process are both carried out at low temperature, so that the decomposition of sodium hexafluorophosphate at high temperature can be effectively avoided, and the yield is improved.

Description

technical field [0001] The invention belongs to the technical field of batteries, and in particular relates to a low-temperature synthesis method of high-purity sodium hexafluorophosphate. Background technique [0002] The statements herein merely provide background related to the present invention and do not necessarily constitute prior art. [0003] New energy vehicles and large-scale energy storage are in urgent need of secondary batteries with high energy density and high safety. Na-ion batteries have promising application prospects in the field of energy storage due to their potential cost advantages. Sodium hexafluorophosphate is an important electrolyte salt in the electrolyte of sodium ion battery, which requires high purity. If the impurity content is too high, the internal resistance of the battery will increase, the capacity will decay rapidly, the cycle life will be reduced, and even the safety of the battery will be affected. However, the inventor found that ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D13/00
CPCC01D13/00
Inventor 冯金奎安永灵
Owner SHANDONG UNIV
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