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Preparation method of lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and phosphorus trifluoride, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of difficulty in obtaining high-purity lithium hexafluorophosphate, high content of impurities in raw materials, and many conditions and parameters. Purity requirements, mild reaction conditions effect

Active Publication Date: 2010-06-09
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of preparing phosphorus pentafluoride and further preparing lithium hexafluorophosphate by using red phosphorus or phosphorus pentoxide as raw material is difficult to obtain high-purity lithium hexafluorophosphate due to the high impurity content of the raw material; and preparing phosphorus pentafluoride by reacting hydrogen fluoride and phosphorus pentachloride and further The method for preparing lithium hexafluorophosphate, because the reaction of phosphorus pentachloride and anhydrous hydrogen fluoride to produce phosphorus pentafluoride is a violent exothermic reaction, improper operation can easily cause explosion, and the safety is poor
The patent application with publication number CN1188072A discloses a method for preparing phosphorus pentafluoride by fluorination of phosphorus trichloride, which has the advantages of relatively sufficient reaction and high utilization rate of raw materials, but there are many conditional parameters to be controlled in the reaction , the reaction proceeds intermittently

Method used

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Embodiment 1

[0012] The preparation method of lithium hexafluorophosphate of the present embodiment comprises the following steps:

[0013] (1) Take 110g of phosphorus trichloride and 130g of anhydrous hydrogen fluoride, add them into the gas-liquid mixer slowly within 1 hour in proportion, react at 50°C, and continuously generate phosphorus trifluoride and hydrogen chloride gas.

[0014] (2) Phosphorus trifluoride, hydrogen chloride, and excess hydrogen fluoride gas generated in step (1) continuously enter the phosphorus pentafluoride reaction generator, and 72g chlorine gas is continuously fed into the reactor simultaneously to keep the reaction system at 35°C In a dry environment, phosphorus trifluoride, chlorine gas and hydrogen fluoride gas continuously react in the reactor to generate phosphorus pentafluoride gas, and the resulting phosphorus pentafluoride gas is cooled and refined at -40°C to remove excess hydrogen fluoride and other impurity gases. The refined gas includes phosphor...

Embodiment 2

[0018] The preparation method of lithium hexafluorophosphate of the present embodiment comprises the following steps:

[0019] (1) Take 220g of phosphorus trichloride and 260g of anhydrous hydrogen fluoride, add them into the gas-liquid mixer slowly within 1 hour in proportion, react at 60°C, and continuously generate phosphorus trifluoride and hydrogen chloride gas.

[0020] (2) Phosphorus trifluoride, hydrogen chloride, and excess hydrogen fluoride gas generated in step (1) continuously enter the phosphorus pentafluoride reaction generator, and 144g chlorine gas is continuously passed into the reactor simultaneously to keep the reaction system at 70°C In a dry environment, phosphorus trifluoride, chlorine gas and hydrogen fluoride gas in the reactor react continuously to generate phosphorus pentafluoride gas, and the resulting phosphorus pentafluoride gas is cooled and refined at 0°C to remove excess hydrogen fluoride and other impurity gases, and then refined The final gas,...

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Abstract

The invention provides a preparation method of lithium hexafluorophosphate. The method comprises the following steps of: (1) reacting phosphorus trichloride and anhydrous hydrogen fluoride to generate phosphorus trifluoride and hydrogen chloride; (2) continuously leading gas generated in the step (1) and a redundant hydrogen fluoride gas into a phosphorus pentafluoride reaction generator, and meanwhile, continuously leading a chlorine gas to react and generate a phosphorus pentafluoride gas; and (3) reacting the phosphorus pentafluoride and lithium fluoride to produce the lithium hexafluorophosphate. The reaction condition of the preparation method is easy to control, and the purity of a prepared product is larger than 99.9 percent and can meet the requirement on the electrolyte purity of lithium batteries.

Description

technical field [0001] The invention relates to a preparation method of lithium ion battery electrolyte salt, in particular to a preparation method of lithium hexafluorophosphate. Background technique [0002] Lithium hexafluorophosphate (LiPF 6 ) as an electrolyte salt for lithium-ion secondary batteries has the advantages of high conductivity, good chemical and electrochemical stability, and good safety. Therefore, lithium hexafluorophosphate is dissolved in some non-aqueous organic solvents to form an electrolytic solution for lithium-ion secondary batteries. liquid. In order to maintain the performance of the battery, such as the service life, the purity of the electrolyte in the electrolyte is very high. The method of preparing phosphorus pentafluoride and further preparing lithium hexafluorophosphate by using red phosphorus or phosphorus pentoxide as raw material is difficult to obtain high-purity lithium hexafluorophosphate due to the high impurity content of the ra...

Claims

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Application Information

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IPC IPC(8): C01B25/455
Inventor 李云峰罗成果闫春生贾雪峰舒伟峰李凌云刘松邵俊华
Owner DO FLUORIDE CHEM CO LTD