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Preparation method of high-purity lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and high-purity lithium fluoride, which is applied to lithium hexafluorophosphate, chemical instruments and methods, lithium compounds, etc., can solve the problems of low purity of lithium hexafluorophosphate and affect the performance of lithium ion batteries, etc., and achieves a simple and easy-to-control preparation method and improves yield. , the effect of improving the purity

Inactive Publication Date: 2019-07-05
张明东
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of lithium hexafluorophosphate produced by this method is low, which seriously affects the performance of lithium-ion batteries

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A preparation method of high-purity lithium hexafluorophosphate, comprising the steps of:

[0021] (1) Preparation of phosphorus pentafluoride, PCl 3 Fill it into a closed container and maintain it at about 3°C. Place the container on a vibrating table to vibrate, and slowly introduce dry chlorine gas into it from the bottom of the container. Stop feeding chlorine gas after 1 hour of reaction, and continue to fill dry chlorine gas from the bottom of the container The hydrogen fluoride gas 1h reacts to obtain phosphorus pentafluoride, wherein, PCl 3 The molar ratio with chlorine is 1:1.3, PCl 3 The molar ratio to hydrogen fluoride gas is 1:1.2.

[0022] (2) For the preparation of high-purity lithium fluoride, add an appropriate amount of distilled water in the autoclave, then inject liquid ammonia in an equimolar ratio and dry hydrogen fluoride into the autoclave, and react for 60 hours to obtain a high-purity ammonium fluoride solution. Analytical pure lithium nitrat...

Embodiment 2

[0025] A preparation method of high-purity lithium hexafluorophosphate, comprising the steps of:

[0026] (1) Preparation of phosphorus pentafluoride, PCl 3 Fill it into a closed container and maintain it at 5°C. Place the container on a vibrating table to vibrate, and slowly introduce dry chlorine gas into it from the bottom of the container. Stop feeding chlorine gas after 1 hour of reaction, and continue to fill it with dry chlorine gas from the bottom of the container. Hydrogen fluoride gas reacts for 1h to obtain phosphorus pentafluoride, wherein, PCl 3 The molar ratio with chlorine is 1:1.3, PCl 3 The molar ratio to hydrogen fluoride gas is 1:1.3.

[0027] (2) For the preparation of high-purity lithium fluoride, add an appropriate amount of distilled water in the autoclave, then inject liquid ammonia in an equimolar ratio and dry hydrogen fluoride into the autoclave, and react for 40 hours to obtain a high-purity ammonium fluoride solution. Analytical pure lithium nit...

Embodiment 3

[0030] A preparation method of high-purity lithium hexafluorophosphate, comprising the steps of:

[0031] (1) Preparation of phosphorus pentafluoride, PCl 3 Fill it into a closed container and maintain it at about 1°C. Place the container on a vibrating table to vibrate, and slowly introduce dry chlorine gas into it from the bottom of the container. After 1 hour of reaction, stop the introduction of chlorine gas and continue to fill it with dry The hydrogen fluoride gas 1h reacts to obtain phosphorus pentafluoride, wherein, PCl 3 The molar ratio with chlorine is 1:1.3, PCl 3 The molar ratio to hydrogen fluoride gas is 1:1.2.

[0032] (2) For the preparation of high-purity lithium fluoride, add an appropriate amount of distilled water in the autoclave, then inject liquid ammonia in an equimolar ratio and dry hydrogen fluoride into the autoclave, and react for 50 hours to obtain a high-purity ammonium fluoride solution. Analytical pure lithium nitrate was dissolved with hot d...

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Abstract

The invention discloses a preparation method of high-purity lithium hexafluorophosphate, comprising the following steps: preparation of phosphorus pentafluoride, preparation of high-purity lithium fluoride and synthesis of lithium hexafluorophosphate. The high-purity phosphorous pentafluoride and lithium fluoride are prepared by accurately controlling that purity, dosage and reaction condition ofthe raw materials, and the high-purity lithium hexafluorophosphate is obtained by reacting the phosphorous pentafluoride and the lithium fluoride under closed conditions. In the process of reaction, by controlling the excess of chlorine gas and hydrogen fluoride gas relative to PCl3, the yield of phosphorus pentafluoride can be effectively increased and the production cost can be reduced. Lithiumfluoride is heated in a resistance furnace under the protection of nitrogen so as to promote the unreacted ammonium nitrate to decompose into gas completely and release gas, so as to be beneficial toimprove the purity of intermediate product lithium fluoride and the purity of product. The preparation method has the advantages of simple and controllable preparation method, low requirement on production equipment and high purity of the product lithium hexafluorophosphate which is an excellent electrolyte material for a lithium battery and the preparation method has broad prospect.

Description

technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method of high-purity lithium hexafluorophosphate. Background technique [0002] Lithium hexafluorophosphate, whose chemical formula is LiPF 6 Lithium hexafluorophosphate at room temperature is white crystal or powder, strong deliquescence, easily soluble in water, also soluble in organic solvents such as low concentration methanol, ethanol, acetone, carbonates, etc., decomposes when exposed to air or heated, releasing PF 5 And produce white smoke. [0003] Lithium-ion batteries are currently commonly used batteries. They have the characteristics of small size, large capacity, and good stability in repeated charging and discharging. They are widely used in mobile phones, laptop computers, and other electronic products. Among them, lithium hexafluorophosphate is the most important part of the electrolyte composition, accounting for about 43% of the total cost o...

Claims

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Application Information

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IPC IPC(8): C01D15/00H01M10/0568
CPCC01D15/005C01P2006/40C01P2006/80H01M10/0568Y02E60/10
Inventor 张明东曹雪梅
Owner 张明东
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