Method for preparing potassium hexafluoro phosphate

A technology of lithium hexafluorophosphate and phosphorus pentachloride, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems affecting product purity, fast battery capacity decay, and shortened cycle life

Inactive Publication Date: 2006-10-25
TIANJIN CHEM RES & DESIGN INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] During the preparation of lithium hexafluorophosphate, the raw materials such as phosphorus pentachloride, anhydrous hydrogen fluoride, and lithium fluoride usually contain certain impurities such as water, alkali metals, and heavy metal ions, especially phosphorus pentachloride, which is easy to absorb moisture and produces deliquescence. , the product contains PCl 3 , POCl 3 If the above-mentioned impurities are brought into the lithium hexafluorophosphate product, and the product is prepared into an electrolyte and used in a lithium-ion battery, it will cause an increase in the internal resistance of the battery, a rapid decay of the battery capac

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In a 10L airtight reactor with stirring and jacket insulation, add 1000g of phosphorus pentachloride, heat up to 160°C while stirring, and keep this temperature. At this time, phosphorus pentachloride begins to sublimate, and the sublimation gas is introduced into another A 5L with stirring, cooling jacket, filled with 10gCl 2 Cooling in the cooling equipment.

[0038] After the sublimation is completed, slowly add 600g of anhydrous hydrogen fluoride with a water content of less than 10ppm after rectification and purification to the second reactor to react with phosphorus pentachloride to produce PF 5 Mixed gas with HCl.

[0039] In the third 3L reactor with stirring and cooling jacket, 110g of purified lithium fluoride was dissolved in 2000g of anhydrous hydrogen fluoride to form an anhydrous hydrogen fluoride solution of LiF, which was mixed with the imported PF under stirring. 5 React with HCl gas, after the reaction is completed, cool and crystallize, filter and d...

Embodiment 2

[0041] 2500 g of the mother liquor after crystallization and filtration in Example 1 was added with 110 g of purified lithium fluoride and anhydrous hydrogen fluoride under stirring to form an anhydrous hydrogen fluoride solution of LiF. The reaction process in Example 1 was repeated. Obtain 600g of lithium hexafluorophosphate product. Test results: the free acid (calculated by HF) of the product is 98ppm, the moisture (Karl Fischer method) is 5ppm, the content of alkali metal ions (calculated by K and Na) is 3ppm, the content of heavy metal ions (calculated by Fe) is 2ppm, and the insoluble matter in DME 500ppm.

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PUM

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Abstract

The invention relates to Li ion battery technique, a lithium hexafluoro- phosphate preparing method, characterized in comprising the process steps of: using easy sublimation property of phosphorus pentachloride, heating and sublimating it to remove nonvolatile components, refining industrial anhydrous hydrogen fluoride to remove water and heavy metal impurities; reacting them with each other to prepare mixed gas of phosphorus pentachloride and hydrogen chloride; leading the mixed gas into anhydrous hydrogen fluoride of lithium fluoride, reacting, crystallizing and separating and drying to obtain pure lithium hexafluoro-phosphate.

Description

technical field [0001] The present invention relates to lithium ion battery technology, specifically a preparation method of lithium hexafluorophosphate. Background technique [0002] Lithium hexafluorophosphate is an important electrolyte salt of lithium-ion battery electrolyte. The preparation method of lithium hexafluorophosphate generally includes two methods. [0003] The first method is to prepare PF by reacting red phosphorus and fluorine gas 5 gas, then react with anhydrous hydrogen fluoride solution of lithium fluoride, crystallize, separate and dry to obtain lithium hexafluorophosphate product. Such as JP-A-2001-122604; 122605; 163610. [0004] The second method is to react phosphorus pentachloride with anhydrous hydrogen fluoride to generate a mixed gas of phosphorus pentafluoride and hydrogen chloride, then react with anhydrous hydrogen fluoride solution of lithium fluoride, and obtain lithium hexafluorophosphate product through reaction, crystallization, sepa...

Claims

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Application Information

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IPC IPC(8): C01B25/455C01B25/30
Inventor 赵庆云宁延生郭西凤
Owner TIANJIN CHEM RES & DESIGN INST
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