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Preparation method of lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and hydrofluoric acid, applied in lithium hexafluorophosphate, chemical instruments and methods, phosphorus compounds, etc., can solve the problems of side effects of battery stability, corrosion of sealed battery casings, etc.

Inactive Publication Date: 2003-05-21
FOOSUNG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In particular, when HF reacts with organic solvents, it will also affect the corrosion of the case for sealing the battery, which has a negative effect on the stability of the battery.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0043] The present invention having above-mentioned numerous characteristics relates to a kind of lithium hexafluorophosphate (LiPF 6 ) preparation method, the yield is as high as 90% or above, the purity is as high as 99.8% or above, the moisture content is as low as 20ppm or below, and the free HF content is as low as 150ppm or below.

[0044] Japanese patent application publication level 4-175216 discloses a kind of using PCl 5 React with HF to synthesize PF 5 Gas method, HF and LiF solutions are prepared in separate containers and then fed into the synthesized PF 5 Gas preparation of LiPF 6 . This preparation method is carried out under the following conditions: molar ratio of HF to LiF: 10-20, reaction temperature: -30-0°C, input PF 5 Flow rate: 5-30 L / h, prepared LiPF 6 Particle size: 1-6mm. The disadvantage of this method is the use of expensive LiF as a raw material. Another disadvantage is that the lithium hexafluorophosphate (LiPF 6 ) yields below 70%. The r...

Embodiment 1

[0054] dry anhydrous hydrofluoric acid

[0055] A PFA resin bubbling tube was inserted into a carbon steel container having a volume of 20 kg, and 18 kg of hydrofluoric acid (boiling point: 19.2° C., moisture content: 100 ppm) was added to the container.

[0056] Submerge the container in a water bath maintained at a temperature of 0-10°C.

[0057] Pass into the container with a purity of 99% or more, a concentration of 99% or more, by driving F 2 F produced by the electrolytic reactor 2 gas, bubbled and exposed to hydrofluoric acid, F under reaction conditions 2 The flow rate was 61 g / h and the contact time was 30 minutes.

[0058] distilled anhydrous hydrofluoric acid

[0059] will be loaded into the F 2 The container of dry HF is heated to 60-130°C.

[0060] Distill HF by evaporation, condensation, while maintaining the internal pressure of the vessel at 1×10 5 Pa (gauge pressure). The moisture content of the distilled HF was analyzed by nephelometric method. The r...

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Abstract

A method of preparing lithium hexafluoro phosphate (LiPF6) using phosphorous pentachloride (PCl5), lithium chloride (LiCl), and hydrogen fluoride (HF) as raw materials. The method includes the steps of: (a) reacting the phosphorous pentafluoride with the hydrogen fluoride to prepare phosphorous pentafluoride (PF5), and (b) reacting the phosphorous pentafluoride with the lithium chloride in a hydrogen fluoride to prepare the lithium hexafluoro phosphate. Anhydrous hydrogen fluoride, from which moisture was removed by treating with F2 gas, is used in the steps (a) and (b), and the step (b) further comprises contacting the reaction system of the step (b) with F2 gas. Accordingly, as the method adopts relatively cheap raw materials, it enables lithium hexafluoro phosphate (LiPF6) to be prepared at a high yield and purity.

Description

technical field [0001] The present invention relates to high yield, high purity lithium hexafluorophosphate (LiPF 6 ) preparation method, this material is a basic element that constitutes a lithium ion storage battery and a lithium polymer battery. Background technique [0002] Lithium-ion batteries or lithium polymer batteries are mainly composed of lithium oxide anodes (such as LiCoO 2 , LiNiO 2 , LiMn 2 o 4 etc.), a carbonaceous material cathode (such as graphite) and an electrolytic solution (composed of an electrolyte dissolved in an organic solvent). Examples of organic solvents include non-aqueous solvents such as a mixed solvent of ethylene carbonate (hereinafter referred to as "EC") and dimethyl carbonate (hereinafter referred to as "DMC"), EC and diethyl carbonate (hereinafter referred to as " DEC") mixed solvents, etc. In addition, lithium hexafluorophosphate is generally used as an electrolyte. [0003] When the battery is charged, lithium ions enter and a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/455C01D15/00C01D17/00H01M10/05H01M10/0568
CPCC01D15/005H01M10/0568H01M10/0525Y02E60/122Y02E60/10C01D17/00
Inventor 罗斗灿禹炳元朴淳弘李骏浩
Owner FOOSUNG
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