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Preparation method of ultra-pure high-activity battery-grade lithium fluoride

A lithium fluoride, battery-grade technology, applied in the field of preparation of ultra-pure and high-activity battery-grade lithium fluoride, can solve the problems of insufficient material purity, unstable lithium fluoride activity, affecting the purity of LiPF6 materials, and achieve low energy consumption effect

Pending Publication Date: 2021-01-29
于兴江
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are still many uncertainties in the preparation process of high-purity lithium fluoride materials by traditional technology, and the purity of the prepared materials is not high enough. Especially the preparation method using HF as raw material also has the influence of LiF·HF compound, which affects the Purity of prepared LiPF6 materials
In addition, the activity of the prepared lithium fluoride is also unstable, so that in the subsequent synthesis of lithium hexafluorophosphate, partial coating will be formed, which directly affects the indicators of lithium hexafluorophosphate

Method used

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  • Preparation method of ultra-pure high-activity battery-grade lithium fluoride

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preparation example Construction

[0031] A method for preparing ultra-pure and highly active battery-grade lithium fluoride, the method comprising the following steps:

[0032] Step 1, using ultrapure water to prepare anhydrous hydrogen fluoride into aqueous hydrofluoric acid, and blending the aqueous hydrofluoric acid and crude lithium fluoride into lithium fluoride slurry;

[0033] Step 2. Under continuous stirring, the lithium fluoride slurry is continuously fed into a ball mill for ball milling. The temperature of the suspension in the ball mill is 50-100 degrees Celsius. After the materials in the ball mill are dissolved, filter the eluate , washing to obtain high-quality hydrogen fluoride microcrystals;

[0034] Step 3, adding the refined hydrogen fluoride microcrystals into anhydrous hydrogen fluoride, dissolving at 10-15 degrees Celsius for 10-30 minutes, and filtering to obtain a clear lithium hydrogen fluoride solution;

[0035] Step 4, cooling and crystallizing the lithium hydrogen fluoride solutio...

Embodiment 1

[0047] A method for preparing ultra-pure and highly active battery-grade lithium fluoride, the method comprising the following steps:

[0048] Step 1, using ultrapure water to deploy anhydrous hydrogen fluoride into hydrofluoric acid with water, and blend the hydrofluoric acid with water and crude lithium fluoride into lithium fluoride slurry; the mass percentage of hydrofluoric acid with water The concentration is 25%, and the ambient temperature is 0 degrees Celsius during deployment.

[0049] Step 2. Under continuous stirring, continuously send the lithium fluoride slurry into a ball mill for ball milling. The temperature of the suspension in the ball mill is 80 degrees Celsius. After the materials in the ball mill are dissolved, filter and wash the solution , to obtain high-quality hydrogen fluoride microcrystals; the mass concentration of the eluate from the ball mill is 120mg / L.

[0050] Step 3, adding the refined hydrogen fluoride microcrystals into anhydrous hydrogen ...

Embodiment 2

[0054] A method for preparing ultra-pure and highly active battery-grade lithium fluoride, the method comprising the following steps:

[0055] Step 1, using ultrapure water to deploy anhydrous hydrogen fluoride into hydrofluoric acid with water, and blend the hydrofluoric acid with water and crude lithium fluoride into lithium fluoride slurry; the mass percentage of hydrofluoric acid with water The concentration is 5%, and the ambient temperature is 10 degrees Celsius during deployment.

[0056] Step 2. Under continuous stirring, continuously send the lithium fluoride slurry into a ball mill for ball milling. The temperature of the suspension in the ball mill is 100 degrees Celsius. After the materials in the ball mill are dissolved, filter and wash the solution , to obtain high-quality hydrogen fluoride microcrystals; the mass concentration of the eluate from the ball mill is 80mg / L.

[0057] Step 3: Add the refined hydrogen fluoride microcrystals into anhydrous hydrogen flu...

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Abstract

The invention discloses a preparation method of ultra-pure high-activity battery-grade lithium fluoride. The preparation method comprises the following steps: 1, blending anhydrous hydrogen fluoride into anhydrous hydrofluoric acid by using ultrapure water, and blending the anhydrous hydrofluoric acid and crude lithium fluoride into lithium fluoride slurry; 2, under continuous stirring, continuously feeding the lithium fluoride slurry into a ball mill for ball milling; 3, adding the ball-milled lithium fluoride slurry into anhydrous hydrogen fluoride, and carrying out filtering to obtain a clear lithium hydrogen fluoride solution; 4, performing cooling and crystallizing to obtain crystal mush; and 5, carrying out vacuum drying after airflow drying to obtain the ultra-pure high-activity battery-grade lithium fluoride crystal. The invention provides a low-energy-consumption short-flow purification process, and a finally obtained lithium fluoride product is applicable to batteries.

Description

technical field [0001] The invention relates to the field of lithium fluoride preparation methods, in particular to a preparation method of ultra-pure high-activity battery-grade lithium fluoride. Background technique [0002] With the increasing demand for high-purity lithium fluoride in traditional application fields and the continuous emergence of some new application fields (such as applying it to the raw materials for the synthesis of lithium hexafluorophosphate, long-distance communication optical fiber materials, etc.), the preparation of high-purity lithium fluoride is becoming more and more important. People have paid more and more attention to it. In the late 1980s, reports on the preparation technology of high-purity lithium fluoride began to appear internationally. The methods introduced successively include direct preparation, ion exchange preparation, and extraction preparation. [0003] The direct preparation method is the main method for the early preparation...

Claims

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Application Information

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IPC IPC(8): C01D15/04
CPCC01D15/04C01P2006/80
Inventor 于兴江
Owner 于兴江
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