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Preparation method of lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and lithium fluoride, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems affecting battery safety, fast battery capacity decay, and shortened cycle life, and achieve good economic value and social value , Good product quality and low production cost

Active Publication Date: 2011-04-13
MORITA NEW ENERGY MATERIALS ZHANGJIAGANG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003]Lithium hexafluorophosphate is an important electrolyte salt of lithium-ion battery electrolyte, which requires high purity (usually not less than 99.5%), and impurities such as water , the content of alkali metals, heavy metals and other impurities such as PCl3 and POCl3 must be strictly controlled, otherwise the internal resistance of the battery will increase, the battery capacity will decay quickly, the cycle life will be shortened, and even the safety of the battery will be affected

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The preparation method according to the lithium hexafluorophosphate of the present embodiment comprises the following steps:

[0017] (1) Preparation of high-purity hydrogen fluoride liquid: In a closed SUS316 container, add 5000kg of anhydrous hydrogen fluoride under nitrogen protection, heat through the jacket of the stainless steel container, and control the temperature at 25°C. The distilled hydrogen fluoride gas is condensed through the condenser , the condensation temperature is controlled at -15°C, and high-purity hydrogen fluoride liquid is obtained by condensation. The distillation condensation time was 4 hours.

[0018] (2) Preparation of lithium fluoride solution: Take 500 kg of hydrogen fluoride liquid obtained in step (1) and add it to the second synthesis reactor, then add 20 kg of high-purity lithium fluoride with a purity of 99.9% or more through an automatic feeder, and stir thoroughly , the temperature is controlled around 0°C.

[0019] (3), ...

Embodiment 2

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

[0024] (1) Return 535 kg of the crystallized mother liquor in Example 1 to the second synthesis reactor, add 14 kg of high-purity lithium fluoride, stir well, and control the temperature at around 0°C.

[0025] (2) Add 115 kg of phosphorus pentachloride to the first synthesis reactor of stainless steel (SUS316), and then add 70 kg of high-purity hydrogen fluoride liquid. PF 5 and hydrogen chloride gas to obtain PF 5 170.1kg of mixed gas with hydrogen chloride gas is collected in a stainless steel container; excess hydrogen fluoride is absorbed by the condensate water of the condensing device, and different by-products hydrofluoric acid are produced according to needs.

[0026] (3), preparation of lithium hexafluorophosphate product: the PF obtained in step (2) 5 Pass 170.1kg of hydrogen chloride gas into the second synthes...

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PUM

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Abstract

The invention relates to a preparation method of lithium hexafluorophosphate. The preparation method comprises the following steps of: (1) distilling to obtain hydrogen fluoride liquid of which the purity is over 99.99 weight percent; (2) reacting the high-purity hydrogen fluoride liquid with phosphorus pentachloride to obtain mixed gas of the phosphorus pentafluoride and hydrogen chloride; (3) introducing the mixed gas of the phosphorus pentachloride and the hydrogen chloride into hydrogen fluoride and lithium fluoride, reacting at a certain temperature and under certain pressure to obtain solution of lithium hexafluorophosphate, exhausting hydrogen chloride gas at regular time, and absorbing by using water to prepare byproduct hydrochloric acid; and (4) crystallizing and separating, namely filtering the solution of lithium hexafluorophosphate, delivering filtrate into a crystallizing slot, separating the lithium hexafluorophosphate out at the temperature of between -70 and 80 DEG C, filtering, and performing primary drying and secondary drying to obtain a lithium hexafluorophosphate product, wherein the residual hydrogen fluoride gas is displaced by nitrogen. The preparation method has readily available raw materials and is easy to operate, the purity of the obtained lithium hexafluorophosphate product is over 99.9 percent, the moisture is lower than 10ppm, and the production requirements of lithium ion electrolytic cells are met.

Description

technical field [0001] The invention relates to a preparation method of lithium hexafluorophosphate. Background technique [0002] Lithium-ion batteries have outstanding advantages such as high working voltage, high energy density (light weight), low self-discharge rate, no memory effect, long cycle life and no pollution. In recent years, it has quickly occupied many fields with its incomparable advantages over other batteries, and is widely used in well-known mobile phones, notebook computers, small cameras, electric vehicles and other products. With the industrialization of electric vehicles, the amount of lithium-ion batteries is bound to increase. The application shows that lithium-ion battery is an ideal small green power source. [0003] Lithium hexafluorophosphate, as an important electrolyte salt of lithium-ion battery electrolyte, requires high purity (usually not less than 99.5%), and the content of impurities such as water, alkali metals, heavy metals and other ...

Claims

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Application Information

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IPC IPC(8): C01B25/455
Inventor 堀尾博英
Owner MORITA NEW ENERGY MATERIALS ZHANGJIAGANG CO LTD
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