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Preparation method of lithium hexafluorophosphate of lithium ion battery electrolyte

A lithium hexafluorophosphate and lithium fluoride technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of lithium hexafluorophosphate products containing, low product purity, imperfect control, etc., and achieve good economic value and social value, The effect of simple process and low production cost

Inactive Publication Date: 2012-06-27
DONGGUAN DONGJUN NEW ENERGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above preparation method of lithium hexafluorophosphate, because the raw material phosphorus pentachloride, anhydrous hydrogen fluoride, lithium fluoride pre-treatment and the control of important process parameters in the preparation process are not perfect, resulting in impurity such as moisture, free acid in the lithium hexafluorophosphate product, product purity is not good high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A preparation method of lithium hexafluorophosphate, it comprises the following steps:

[0023] Step A. Preparation of high-purity hydrogen fluoride: Put 150kg of anhydrous hydrogen fluoride into a 316L stainless steel 1# reactor for distillation and refining. The distillation temperature is controlled at 25°C, and the condensation temperature is not higher than 19°C to obtain high-purity hydrogen fluoride liquid;

[0024] Step B, preparation of high-purity phosphorus pentafluoride: Add 20 kg of high-purity hydrogen fluoride liquid prepared in step A to 2# reactor of 316L stainless steel with 40 kg of phosphorus pentachloride for reaction, and the temperature is controlled at 0°C -19°C, the pressure is controlled at 0.15Mpa, and the reaction produces a mixed gas of phosphorus pentafluoride and hydrogen chloride;

[0025] Step C, preparation of lithium fluoride solution: Add 100 kg of the high-purity hydrogen fluoride liquid prepared in step A into a PTFE-lined 3# reacto...

Embodiment 2

[0031] Step A. Preparation of high-purity hydrogen fluoride: Put 150kg of anhydrous hydrogen fluoride into a 316L stainless steel 1# reactor for distillation and refining. The distillation temperature is controlled at 20°C-28°C, and the condensation temperature is not higher than 19°C to obtain high-purity hydrogen fluoride liquid;

[0032] Step B, preparation of high-purity phosphorus pentafluoride: 18 kg of high-purity hydrogen fluoride liquid prepared in step A is added to 316L stainless steel 2# reactor with 36 kg of phosphorus pentachloride for reaction, and the temperature is controlled at 9 ° C. The pressure is controlled at 0.1-0.2Mpa, and the reaction generates a mixed gas of phosphorus pentafluoride and hydrogen chloride;

[0033] Step C, preparation of lithium fluoride solution: 105 kg of the mother liquor crystallized in Example 1 was added to a PTFE-lined 3# reactor with 4.5 kg of lithium fluoride added, the temperature was controlled at 0°C, stirred and dissolved...

Embodiment 3

[0039] A preparation method of lithium hexafluorophosphate, it comprises the following steps:

[0040] Step A. Preparation of high-purity hydrogen fluoride: Put 150kg of anhydrous hydrogen fluoride into a 316L stainless steel 1# reactor for distillation and refining. The distillation temperature is controlled at 25°C, and the condensation temperature is not higher than 19°C to obtain high-purity hydrogen fluoride liquid;

[0041] Step B, preparation of high-purity phosphorus pentafluoride: Add 19 kg of high-purity hydrogen fluoride liquid prepared in step A to 316L stainless steel 2# reactor with 38 kg of phosphorus pentachloride for reaction, and the temperature is controlled at 12°C , the pressure is controlled at 0.1Mpa, and the reaction generates a mixed gas of phosphorus pentafluoride and hydrogen chloride;

[0042] Step C, preparation of lithium fluoride solution: Add 98kg of the high-purity hydrogen fluoride liquid prepared in step A to the PTFE-lined 3# reactor with 4....

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Abstract

The invention relates to the technical field of lithium batteries, in particular to a preparation method of lithium hexafluorophosphate of lithium ion battery electrolyte. The preparation method is characterized in that hydrogen fluoride, phosphorus pentachloride and lithium fluoride, which are adopted as raw materials, are refined and react under the conditions of proper temperature, pressure and time, and then high-purity lithium hexafluorophosphate is prepared by adopting the technical route of low-temperature crystallization and vacuum drying. The raw materials used in the method are cheap and easy to obtain; the production cost is low; the technological process is simple; the operation is convenient to control; excellent economical and social values in extensive use of energy-saving environment-friendly new energies are achieved; moisture, free acid and other impurities in a product are effectively reduced, so that the product yield is high, and the product quality is high; and the purity of the lithium hexafluorophosphate product reaches 99.95 percent, so as to satisfy the production requirements of the lithium ion batteries.

Description

technical field [0001] The invention relates to the technical field of lithium batteries, in particular to a preparation method of lithium hexafluorophosphate electrolyte solution for lithium ion batteries. Background technique [0002] Lithium hexafluorophosphate is an important electrolyte salt for the electrolyte of lithium-ion batteries. As an electrolyte material for lithium batteries, it must meet the following properties, namely, high electrical conductivity, good chemical and electrochemical stability, wide usable temperature range, good safety, and low price. Higher physical properties are required, otherwise, the internal resistance of the battery will increase, the battery capacity will decay rapidly, the cycle life will be shortened, and even the safety of the battery will be affected. The standards of the Ministry of Chemical Industry of my country are: the moisture content of the product is less than 20ppm; the free acid is less than 150ppm; the insoluble matte...

Claims

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Application Information

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IPC IPC(8): C01B25/455
Inventor 王克俊刘永鸿
Owner DONGGUAN DONGJUN NEW ENERGY TECH
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