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Method and device for continuous preparation of lithium hexafluorophosphate

A lithium hexafluorophosphate and separation device technology, applied in lithium hexafluorophosphate, chemical instruments and methods, lithium compounds, etc., can solve problems such as high equipment requirements and difficult processes, and achieve large cryogenic loss, eliminate large power consumption, and large particles Effect

Active Publication Date: 2017-10-13
东营石大胜华新能源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Lithium hexafluorophosphate is a key raw material for lithium-ion battery electrolyte. Its production technology involves low temperature, high temperature, vacuum, corrosion resistance, safety and environmental protection, as disclosed in CN 106430255A, CN 105845931A, etc., and its equipment requirements are high and the process is difficult Big

Method used

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  • Method and device for continuous preparation of lithium hexafluorophosphate
  • Method and device for continuous preparation of lithium hexafluorophosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] A. Synthetic liquid heating up

[0062] Lithium hexafluorophosphate synthetic liquid (6000L / h, temperature 10°C, concentration 20%) from the liquid pump of the synthetic liquid storage tank enters the crystallizer together with the mother liquor (2000L / h, temperature 30°C, concentration 5%) The inlet of the circulation pump is pressurized to 0.15MPa by the external circulation pump and then enters the steam heater, and the mixed solution is heated to 45°C-50°C and enters the crystallizer (concentration is about 16%).

[0063] B. Stirring cycle inside the crystallizer

[0064] The mixed liquid entering the crystallizer, under the action of the magnetic stirrer, circulates along the circulation channel formed by the guide tube, and controls the negative pressure in the crystallizer to be between -15kPa~-25kPa, and the boiling liquid level is to produce supersaturation Area, with the help of evaporation, becomes a supersaturated solution and contacts the crystals in the c...

Embodiment 2

[0072] The specific process is the same as in Example 1, except for the following differences:

[0073] The feed temperature of the synthetic liquid in A is 5°C; the heating temperature of the synthetic liquid is 55°C;

[0074] The negative pressure in B is -25kPa;

[0075] The temperature of the refrigerant in C is -5°C; the refrigerant is 60wt% ethylene glycol aqueous solution;

[0076] The vacuum degree during condensation is -50kp;

[0077] The pressure at the time of separation in E is -10kPa.

[0078] The resulting high-quality lithium hexafluorophosphate has moisture ≤ 2.8ppm, acid ≤ 59ppm, insoluble matter ≤ 130ppm, and iron ≤ 2.4ppm.

Embodiment 3

[0080] The specific process is the same as in Example 1, except for the following differences:

[0081] The feed temperature of the synthetic liquid in A is 15°C; the heating temperature of the synthetic liquid is 40°C;

[0082] The negative pressure in B is -50kPa;

[0083] The temperature of the refrigerant in C is -20°C; the refrigerant is 15wt% ethylene glycol aqueous solution;

[0084] The vacuum degree during condensation is -40kPa;

[0085] The pressure at the time of separation in E is 0 kPa.

[0086] The resulting high-quality lithium hexafluorophosphate has moisture ≤ 3.4ppm, acid ≤ 65ppm, insoluble matter ≤ 146ppm, and iron ≤ 2ppm.

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Abstract

The invention relates to a device and method for continuous preparation of lithium hexafluorophosphate. The device comprises a continuous evaporation crystallizer, a condensation recoverer, a heater, an ex-situ circulation pump, a product crystal delivery pump and a separation apparatus. Specifically, the continuous evaporation crystallizer is internally equipped with a stirrer, and the lower part of the continuous evaporation crystallizer is equipped with an elutriating leg; the ex-situ circulation pump, the heater, and the continuous evaporation crystallizer are connected in order; the elutriating leg is connected to the product crystal delivery pump; the product crystal delivery pump is connected to the separation apparatus; and the condensation recoverer is connected to the upper part of the continuous evaporation crystallizer. The invention employs an effective evaporative crystallization method and the advanced DBT type continuous efficient evaporation crystallizer to make the crystalline particles of lithium hexafluorophosphate more uniform, and effectively lowers the product investment cost and energy consumption per ton, thus realizing continuous, efficient and large-scale production of lithium hexafluorophosphate.

Description

technical field [0001] The invention belongs to the technical field of power lithium ion battery manufacturing, in particular to a method and device for rapidly and efficiently preparing and purifying electrolyte salt 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. It is used in well-known products such as mobile phones, notebook computers, small cameras, and electric vehicles. With the industrialization of electric vehicles, the amount of use is bound to increase. The application shows that lithium-ion battery is an ideal small green power source. [0003] Electrolyte is one of the four key materials of lithium-ion batteries. It is called the "blood" of lithium-ion batteries. It plays the role of conducting electrons between the positive and negative electrodes. It enables...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/00H01M4/58H01M10/0525
CPCC01D15/005C01P2006/80C01P2006/82H01M4/5825H01M10/0525Y02E60/10
Inventor 贾风雷吕蕾陈效飞魏林埔马震袁磊谷洪闪季凯强
Owner 东营石大胜华新能源有限公司
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