Preparation method of lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and hexafluorophosphate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of high impurity content of LiPF6 products and unsuitability for industrial production, and achieve simple preparation methods, cost saving, and improved safety effect

Active Publication Date: 2013-08-28
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But using this method to prepare LiPF 6 The product has high impurity content and is not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] At room temperature, add 5.67gLiF and 105.27g HF to a tetrafluoro reaction vessel with a jacket, and stir overnight to completely dissolve LiF in HF, then add KPF 6 42.02g, put low-temperature cooling medium into the jacket, control the temperature at 10°C, stir for 24 hours, quickly filter, and freeze the obtained filtrate, the freezing temperature is -20°C, and the freezing time is 12 hours, then filter the filtrate , the quality of the obtained filtrate is 92.24g, and the obtained lithium hexafluorophosphate product is dried, and the quality of the obtained product is 20.56g, and the LiPF in the filtrate 6 The content is 13.24%, and the resulting product yield is 98.89%, wherein the potassium ion content is 1250ppm. The resulting product was dissolved in ether, after precision filtration, crystallization by evaporation and drying, the product purity of the final high-purity product obtained was 99.96%, the water content was 4.8ppm, the acid content was 24ppm, and the...

Embodiment 2

[0023] At room temperature, 2.23g of LiF was added to a tetrafluoro reaction vessel with a jacket, and 92.24g of the filtrate obtained in Example 1 was added to it, and stirred overnight to completely dissolve LiF in HF, and then add KPF 6 16.38g, put low-temperature cooling medium into the jacket, control the temperature at 10°C, stir for 24 hours, filter quickly, and freeze the obtained filtrate, the freezing temperature is -20°C, the freezing time is 12 hours, and then filter the filtrate , the quality of the obtained filtrate is 67.02g. After drying the lithium hexafluorophosphate product, the quality of the obtained product is 16.02g. LiPF in the filtrate 6 The content is 13.22%, and the dry solid yield of the obtained lithium hexafluorophosphate is 98.89%, wherein the potassium ion content is 1118ppm. The obtained product was dissolved in ether, after precision filtration, crystallized by evaporation and dried, the product purity of the final product obtained was 99.32%,...

Embodiment 3

[0027] At room temperature, add 5.62g LiF and 106.12g HF to a tetrafluoro reaction vessel with a jacket, and stir overnight to fully dissolve LiF in HF, and then add NH 4 PF 6 36.07g, a low-temperature cooling medium was introduced into the jacket, the temperature was controlled at 10°C, and after stirring for 24 hours, it was quickly filtered, and the resulting filtrate was frozen at -20°C, and the freezing time was 12 hours, and then the filtrate was filtered , the quality of the obtained filtrate is 92.53g. After drying the lithium hexafluorophosphate product, the quality of the obtained product is 20.12g. LiPF in the filtrate 6The content is 13.18%, and the resulting product yield is 99.15%, wherein the potassium ion content is 1126ppm. Gained product is dissolved in acetonitrile, after precision filtration, the product purity of gained product after crystallization by evaporation and drying is 99.35%, and water content is 3.2ppm, K + The content is 4ppm, NH 4 + The co...

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Abstract

The invention relates to a preparation method of lithium hexafluorophosphate. The preparation method is characterized by comprising the following steps of: (1) enabling hexafluorophosphate MPF6 to react with a raw material, namely, halogenated lithium salt LiF to obtain fluoride MF and lithium hexafluorophosphate LiPF6, wherein M is Li, Na, K, NH4 and Ag; (2) performing a reaction under a closed condition and in a dry inert gas atmosphere of which the water content is smaller than 10ppm, and stirring for 2-24 hours to generate a lithium hexafluorophosphate solution, wherein the water content of a solvent is smaller than 10ppm, and the reaction temperature is between 0 DEG C and 15 DEG C; and (3) dissolving the MF in the solvent by using the solubility of the MF in the solvent, precisely filtering, removing undissolved substances including the fluoride MF and the like in a filtering manner, condensing and crystallizing to obtain a lithium hexafluorophosphate solid, and drying the lithium hexafluorophosphate solid to obtain a lithium hexafluorophosphate product.

Description

technical field [0001] The invention relates to the technical field of manufacturing lithium ion battery materials, in particular to a preparation method of lithium hexafluorophosphate. Background technique [0002] Lithium-ion secondary batteries are mainly composed of lithium oxide anodes (such as: LiMnO 4 etc.), carbon anode materials (such as: graphite, etc.) and electrolyte. Among them, the electrolyte solution of the lithium-ion secondary battery mainly contains organic solvents and electrolytes, and the organic solvents that form the electrolyte mainly include dimethyl carbonate (DMC), diethyl carbonate (DEC), ethylene carbonate (EC) and the like. Lithium hexafluorophosphate is the most important electrolyte lithium salt used in lithium-ion secondary batteries due to its good conductivity and electrochemical stability. At present, the preparation methods of lithium hexafluorophosphate are mainly traditional method, solvent method and replacement method. [0003] Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455
Inventor 王坤刘红光郭西凤叶学海安峰袁莉张玥赵洪刘大凡赵庆云
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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