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A preparation method for high-purity manganese source applied to lithium battery cathode material

A positive electrode material and manganese source technology, which is applied in the field of high-purity manganese source preparation, can solve the problems of limited raw material sources, unsatisfactory economic and social benefits, and the inability to obtain high value-added utilization of manganese-containing waste liquid. The effect of high product purity and high product added value

Active Publication Date: 2017-11-17
HUBEI HAOYUAN MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The existing production process of manganese sources (such as high-purity manganese chloride, high-purity manganese sulfate, etc.) used in lithium battery positive electrode materials is to use high-purity manganese carbonate or high-purity metal manganese to add acid and dissolve, then remove calcium magnesium, heavy metals, iron, etc. and organic impurities, the source of raw materials is limited; low-grade manganese ore with abundant domestic reserves and manganese-containing waste liquid in chemical production cannot be utilized with high added value; resulting in unsatisfactory economic and social benefits

Method used

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  • A preparation method for high-purity manganese source applied to lithium battery cathode material

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Effect test

Embodiment 1

[0030] A preparation method for high-purity manganese source applied to lithium battery cathode material

[0031] 1) Manganese source preparation: adjust the concentration of manganese sulfate solution to 30 ° Be';

[0032] 2) Manganese source impurity removal: In the manganese sulfate solution of step 1), add hydrogen peroxide to remove iron impurities in the solution, react for 50 minutes, filter to obtain filtrate 1, add sulfide salt to remove heavy metal ions in the filtrate 1, and adjust the pH value 4.5, the filtered filtrate 2 is for standby; this step is in the high temperature stage, pay attention to the position of the liquid level, and keep it not lower than the original liquid level when pressing the filter;

[0033] 3) prepare the mass fraction of 15% ammonia water, measure the manganese ion concentration of the filtrate, pass nitrogen protection in the reaction kettle, inject the filtrate 2 obtained in step 2) into the reaction kettle, drip the ammonia water into...

Embodiment 2

[0046] A preparation method for high-purity manganese source applied to lithium battery cathode material

[0047] 1) Manganese source preparation: adjust the concentration of manganese sulfate solution to 32°Be';

[0048] 2) Manganese source impurity removal: In the manganese sulfate solution of step 1), add hydrogen peroxide to remove iron impurities in the solution, react for 30 minutes, filter to obtain filtrate 1, add sulfide to the filtrate 1 to remove heavy metal ions, and adjust the pH value 5.0, the filtered filtrate 2 is set aside; this step is in the high temperature stage, pay attention to the position of the liquid level. When pressing the filter, it must be kept not lower than the original liquid level;

[0049] 3) prepare the mass fraction of 15% ammonia water, measure the manganese ion concentration of the filtrate, pass nitrogen protection in the reaction kettle, inject the filtrate 2 obtained in step 2) into the reaction kettle, drip the ammonia water into th...

Embodiment 3

[0062] A preparation method for high-purity manganese source applied to lithium battery cathode material

[0063] 1) Manganese source preparation: adjust the concentration of manganese sulfate solution to 35 ° Be';

[0064] 2) Manganese source impurity removal: In the manganese sulfate solution of step 1), add hydrogen peroxide to remove iron impurities in the solution, react for 40 minutes, filter to obtain filtrate 1, add sulfide salt to remove heavy metal ions in the filtrate 1, and adjust the pH value It is 4.8, and the filtered filtrate 2 is set aside; this step is at a high temperature stage, pay attention to the position of the liquid level. When pressing the filter, it must be kept not lower than the original liquid level;

[0065] 3) prepare the mass fraction of 15% ammonia water, measure the manganese ion concentration of the filtrate, pass nitrogen protection in the reaction kettle, inject the filtrate 2 obtained in step 2) into the reaction kettle, drip the ammoni...

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Abstract

The invention relates to the technical field applied to lithium battery anode materials (lithium manganate, nickel, cobalt and lithium manganate tri-element material and manganese, iron and lithium phosphate), in particular to a preparation method of a high-purity manganese source (manganese hydroxide) applied to lithium battery anode materials. The preparation method includes: adjusting concentration of a manganese sulfate solution to 30-35 Be';adding hydrogen peroxide into the manganese sulfate solution to remove iron impurity in the solution, adding sulfurizing salt to remove heavy metal ions, and adjusting pH value to 4.5-5.0 to obtain filtered filtrate; feeding nitrogen into a reaction kettle for protection, injecting the obtained filtrate into the reaction kettle, dropping ammonia into the reaction kettle at constant speed, holding temperature for reaction after dropping of ammonia is completed, washing precipitate, and drying to obtain a finished product. By using the preparation method, the defect that an existing process utilizing high-purity manganese carbonate or high-purity metal manganese and adding acid for dissolving at home and abroad is limited by high-purity raw materials is overcome, and the product is shallow peach hexagonal crystals, is high in purity and little in impurity and meets using requirements on the lithium battery anode materials.

Description

technical field [0001] The invention relates to the technical field of lithium battery cathode materials (lithium manganese oxide, nickel cobalt lithium manganate ternary material, manganese iron lithium phosphate, etc.), in particular to a method for preparing a high-purity manganese source applied to lithium battery cathode materials. Background technique [0002] The existing production process of manganese sources (such as high-purity manganese chloride, high-purity manganese sulfate, etc.) used in lithium battery positive electrode materials is to use high-purity manganese carbonate or high-purity metal manganese to add acid and dissolve, then remove calcium magnesium, heavy metals, iron, etc. and organic impurities, and the source of raw materials is limited; low-grade manganese ore with abundant domestic reserves and manganese-containing waste liquid in chemical production cannot be utilized with high added value; resulting in unsatisfactory economic and social benefit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G45/12H01M4/505
CPCC01G45/12C01G45/1207H01M4/505Y02E60/10
Inventor 杨晓平
Owner HUBEI HAOYUAN MATERIAL TECH
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