Preparation method of lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and hexafluorophosphoric acid, which is applied to the manufacture of chemical instruments and methods, phosphorus compounds, and final products, can solve the problems of poor safety of lithium hexafluorophosphate, and achieve the effects of easy control, sufficient reaction, and reduced production costs

Active Publication Date: 2011-08-31
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a preparation method of lithium hexafluorophosphate to solve the problem of poor safety in the production process of lithium hexafluorophosphate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation method of lithium hexafluorophosphate of the present embodiment comprises the following steps:

[0015] (1) Preparation of hexafluorophosphoric acid

[0016] In a 5L closed reaction vessel with magnetic stirring, jacket insulation, and a cooler at the gas outlet, add 1000g of anhydrous hydrofluoric acid under nitrogen protection, cool to -10°C, and slowly and evenly add 500g of pentachloro Phosphate, reaction to obtain hexafluorophosphoric acid and hydrogen chloride gas, hexafluorophosphoric acid exists in anhydrous hydrogen fluoride as a solid; the generated hydrogen chloride gas is discharged into the hydrochloric acid absorption system, and a part of HF gas is entrained when the hydrogen chloride gas is discharged, and passes through the condenser at the gas outlet Condensation, the resulting HF can be recycled

[0017] (2) Preparation of hydrogen fluoride solution of lithium fluoride

[0018] In a reaction kettle with magnetic stirring and cooling ...

Embodiment 2

[0023] The preparation method of lithium hexafluorophosphate of the present embodiment comprises the following steps:

[0024] (1) Preparation of hexafluorophosphoric acid

[0025] In a 5L closed reaction vessel with magnetic stirring, jacket insulation, and a cooler at the gas outlet, add 400g of anhydrous hydrofluoric acid under nitrogen protection, cool to -20°C, and slowly and evenly add 400g of pentachloro Phosphate, reaction to obtain hexafluorophosphoric acid and hydrogen chloride gas, hexafluorophosphoric acid exists in anhydrous hydrogen fluoride as a solid; the generated hydrogen chloride gas is discharged into the hydrochloric acid absorption system, and a part of HF gas is entrained when the hydrogen chloride gas is discharged, and passes through the condenser at the gas outlet Condensation, the resulting HF can be recycled

[0026] (2) Preparation of hydrogen fluoride solution of lithium fluoride

[0027] In a reaction kettle with magnetic stirring and cooling j...

Embodiment 3

[0032] Mother liquor returns and utilizes the method for producing lithium hexafluorophosphate to comprise the following steps:

[0033] 1250g of the mother liquor after crystallization and filtration in the reaction kettle of Example 1 was returned to 500g to make hexafluorophosphoric acid, and 55g of high-purity lithium fluoride was added to the remaining 750g under stirring to form anhydrous hydrogen fluoride solution of lithium fluoride, and the reaction of Example 1 was repeated Process, obtain 300g lithium hexafluorophosphate product.

[0034] Test results of product technical indicators: purity greater than 99.9%, free acid (calculated by HF) 95ppm, moisture (Karl Fischer method) 15ppm, alkali metal ion content (calculated by K, Na) 3ppm, heavy metal ion content (calculated by Fe) 2ppm, insoluble content 500ppm.

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Abstract

The invention provides a preparation method of a lithium hexafluorophosphate, which comprises the following steps: firstly, reacting a phosphorus pentachloride with an anhydrous hydrogen fluoride to form mixed liquid of the phosphorus pentachloride and the anhydrous hydrogen fluoride; secondly, preparing anhydrous hydrogen fluoride solution of lithium fluoride; and finally, adding the anhydrous hydrogen fluoride solution of the lithium fluoride into the mixed liquid of the phosphorus pentachloride and the anhydrous hydrogen fluoride, and sequentially performing reaction, crystallization, separation and drying to obtain a pure lithium hexafluorophosphate product. The preparation method of the invention has the advantages of mild reaction, high safety and purity of the lithium hexafluorophosphate product of over 99.9 percent; and the mother liquor can be reclaimed and reused so that the cost is reduced.

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 salts known to be useful as electrolytes for secondary Li-ion batteries include LiAsF 6 、LiPF 6 、LiCF 3 SO 3 , LiClO 4 , Li(CF 3 SO 3 ) 2 N. LiBF 4 etc., where LiPF 6 It is widely used commercially because of its good comprehensive performance. [0003] At present, the most industrialized production method of lithium hexafluorophosphate is generally the reaction of phosphorus pentafluoride and lithium fluoride in hydrogen fluoride solution of lithium fluoride to generate lithium hexafluorophosphate. There are two main methods for preparing phosphorus pentafluoride, one is Use red phosphorus or phosphorus pentoxide as a raw material to prepare phosphorus pentafluoride, such as the Chinese patent No. 01115040.8, and the Chinese patent applications whose...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/058C01B25/455
CPCY02E60/12Y02E60/10Y02P70/50
Inventor 李世江侯红军杨华春薛旭金于贺华陈宏伟尚钟声闫春生李云峰李凌云
Owner DO FLUORIDE CHEM CO LTD
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