Method for preparing lithium manganate positive electrode material from pyrolusite

A cathode material and pyrolusite technology, which is applied in the field of pyrolusite to prepare lithium manganate cathode material, can solve the problems of single source of raw materials and low economic value, and achieve the effects of single source of raw materials, less impurity content and abundant raw materials

Active Publication Date: 2021-11-02
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Realize the integrated process from manganese minerals directly to lithium manganese oxide cathode materials to solve the defects of single source of raw materials and low economic value in the current preparation stage of lithium manganate

Method used

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  • Method for preparing lithium manganate positive electrode material from pyrolusite
  • Method for preparing lithium manganate positive electrode material from pyrolusite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] (1) Use a planetary ball mill to crush and grind pyrolusite at high speed to obtain manganese ore with a particle size of about 66um.

[0061] (2) 70g of pyrolusite and 537.4mL of 65% potassium hydroxide solution were placed in an autoclave reactor for pressurized alkaline leaching, stirred at a stirring speed of 500r / min, the leaching temperature was 260°C, and the oxygen pressure was controlled at 0.3Mpa. The leaching time is 150min;

[0062] After oxygenation, redox reaction occurs; take out the reacted slurry after depressurization, dissolve it at high temperature with 2mol / L potassium oxide solution, then slowly cool and crystallize. Filtration, the filter cake is potassium manganate coarse crystals.

[0063] (3) Dissolving, grinding, and filtering the coarse crystals of potassium manganate obtained in the step (2) and a certain amount of filtrate. Weigh the coarse crystals of potassium manganate and potassium manganate filtrate for grinding and dissolving. The g...

Embodiment 2

[0068] (1) Use a planetary ball mill to crush and grind pyrolusite at high speed to obtain manganese ore with a particle size of about 66um.

[0069] (2) 70g of pyrolusite and 537.4mL of 65% potassium hydroxide solution were placed in an autoclave reactor for high-pressure alkaline leaching, stirred at a stirring speed of 500r / min, the leaching temperature was 250°C, and the oxygen pressure was controlled at 0.5Mpa. The time is 180min.

[0070] After passing oxygen, redox reaction occurs; take out the reacted slurry after depressurization, dissolve it at high temperature with 2mol / L potassium oxide solution or electrolytic mother liquor, and then slowly cool and crystallize, and after reaching a certain degree of crystallization, put The crystallization liquid is filtered, and the filter cake is coarse crystals of potassium manganate.

[0071] (3) Dissolving, grinding, and filtering the coarse crystals of potassium manganate obtained in the step (2) and a certain amount of fi...

Embodiment 3X

[0075] Example 3 X-ray Diffraction

[0076] The lithium manganate cathode material obtained in Example 1 was subjected to X-ray diffraction, and the X-ray diffraction conditions were as follows: the model of the diffractometer was D / Max2500, the radiation source was Cu-Kα, the wavelength was 0.15406nm, and the scan rate was 5° min- 1 , the scanning range is from 5° to 90°, and the scanning diffraction pattern is as follows figure 2 shown.

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Abstract

The invention belongs to the technical field of manganese ore smelting and lithium ion batteries, and particularly relates to a method for preparing a lithium manganate positive electrode material from pyrolusite. The method comprises the following steps: (1) mixing pyrolusite with a potassium hydroxide solution, and carrying out pressurized oxidation leaching to obtain potassium manganate slurry; (2) performing high-temperature dissolution and low-temperature crystallization on the potassium manganate slurry and alkali liquor, and filtering to obtain potassium manganate coarse crystal and potassium manganate filtrate; (3) dissolving the potassium manganate coarse crystal and the potassium manganate filtrate, grinding, and filtering to obtain manganese-containing alkali liquor; and (4) carrying out constant-temperature hydrothermal reaction on the manganese-containing alkali liquor and a lithium source under the action of a reducing agent aniline to obtain a hydrothermal product, washing the hydrothermal product, drying, and calcining in a muffle furnace for a certain time to obtain the lithium manganate positive electrode material. The method has the advantages of being rich in raw materials, environmentally friendly, low in cost, short in process, capable of saving energy, reducing consumption and the like, maximum utilization of resources is achieved, and the method has great significance in achieving material metallurgy integration.

Description

technical field [0001] The invention belongs to the technical fields of manganese ore smelting and lithium ion batteries, and in particular relates to a method for preparing a lithium manganate cathode material from pyrolusite. Background technique [0002] In the experimental research, the raw materials for the traditional preparation of lithium manganese oxide cathode materials are all obtained from purchased manganese sources (manganese dioxide, manganese sulfate, manganese nitrate, etc.) by liquid phase method and solid phase method, and the consumables are large and expensive. In industrial production, the original source of lithium manganese oxide cathode material lithium-ion battery raw materials are smelted upstream manganese ore to obtain raw materials with high impurity content. Manganese source materials, but the process is cumbersome, energy-consuming and time-consuming, the factory investment is huge, and the economic benefits are not good. [0003] The existin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/12H01M4/505H01M10/0525
CPCC01G45/1221H01M4/505H01M10/0525C01P2002/72Y02E60/10Y02P20/10
Inventor 谢红艳罗凤兰金会心李文蕾李晨哲
Owner GUIZHOU UNIV
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