A method for preparing ternary positive electrode material using manganese-cobalt-nickel waste residue

A cathode material, manganese-cobalt-nickel technology, which is applied in the field of preparation of ternary cathode materials, can solve problems such as optimization of precursors of non-ternary cathode materials, performance optimization of non-ternary cathode materials, complex multi-stage extraction and impurity removal process, etc., to achieve The process is simple and feasible, the production cost is reduced, and the ion conductivity is improved

Active Publication Date: 2022-07-08
GUANGXI NORMAL UNIV OF SCI & TECH
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Problems solved by technology

The shortcoming of this invention is that the precursor of the prepared ternary positive electrode material has not been further optimized.
The disadvantage of this invention is that the complex multi-stage extraction and impurity removal process is used for the leachate, and the components that are beneficial to the modification of the positive electrode material are not utilized.
The disadvantage of this invention is that the performance of the prepared ternary cathode material is not optimized
The disadvantage of this invention is that only the cobalt-nickel oxide precursor is obtained, and the manganese oxide precursor needs to be additionally introduced to prepare the ternary positive electrode material, and the sintering effect of the cobalt-nickel oxide precursor and the manganese oxide precursor does not directly generate magnesium Ion-doped manganese-cobalt-nickel ternary cathode material precursor is good

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  • A method for preparing ternary positive electrode material using manganese-cobalt-nickel waste residue

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preparation example Construction

[0048] (6) Preparation of ternary cathode material: Mix magnesium ion-doped manganese-cobalt-nickel ternary cathode material precursor and lithium hydroxide in a certain mass ratio, and then sinter at high temperature to obtain Li(N i0.6 Co 0.2 Mn 0.2 ) 0.99 Mg 0.01 O 2 Ternary positive electrode material; step (6), the sintering temperature is 650-900° C., the sintering time is 10h, and the amount of lithium hydroxide is 1%-10% of the theoretical excess mass of lithium hydroxide.

[0049] (7) Surface modification: disperse the ternary positive electrode material in water, and use the manganese-rich cobalt-nickel-magnesium solution and ammonium fluoride after decalcification in step (3) as modifiers to disperse the ternary positive electrode material in a certain mass ratio. The material is subjected to surface modification, and the finished product is obtained after post-treatment after the modification; the amount of modifier added is 1-5% of the mass of the ternary posi...

Embodiment 1

[0053] 10g of manganese-cobalt-nickel waste residue was crushed and sieved to 200 mesh, mixed evenly, 90g / L of dilute sulfuric acid was added at a liquid-solid ratio of 10:1, 0.1Mpa of oxygen was introduced, heated to 90°C for leaching, mechanical stirring, and leaching for 180min. Measure the end point pH=3.0, filter, take the filtrate and adjust pH=0.5 with dilute sulfuric acid, mix with volume fraction 30% P204+70% sulfonated kerosene according to the ratio O / A=1:1, and then add sodium hydroxide for saponification, The saponification rate of the extractant is 20%, the extraction is performed for 10 minutes, and then the liquid is separated in a separating funnel to obtain a manganese-rich, cobalt-rich, nickel-magnesium solution after decalcification. Manganese solution, adjust the molar ratio of nickel, cobalt, manganese and magnesium ions in the solution to 0.6:0.2:0.2:0.01, and add 1mol / L sodium hydroxide solution and 10% ammonia solution by volume at the same time to main...

Embodiment 2

[0055] 10g of manganese-cobalt-nickel waste residue was crushed and sieved to 200 mesh, mixed evenly, 100g / L of dilute sulfuric acid was added at a liquid-solid ratio of 9:1, 0.2Mpa of oxygen was introduced, heated to 80°C for leaching, mechanically stirred, and leached for 180min. Measure the end point pH=3.0, filter, take the filtrate and adjust pH=0.5 with dilute sulfuric acid, mix with volume fraction 30% P204+70% sulfonated kerosene according to the ratio O / A=1:1, add sodium hydroxide for saponification, wherein The saponification rate of the extractant is 20%, extraction is performed for 10 minutes, and then the liquid is separated in a separating funnel to obtain a manganese-cobalt-nickel-magnesium solution rich in manganese, cobalt, nickel, and magnesium after decalcification. , adjust the molar ratio of nickel, cobalt, manganese, and magnesium in the solution to 0.5:0.3:0.2:0.02, add 2mol / L sodium hydroxide solution and 15% ammonia solution by volume at the same time, ...

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Abstract

The invention discloses a method for preparing a ternary positive electrode material by utilizing manganese-cobalt-nickel waste residue, which is carried out according to the following steps: (1) crushing and sieving; (2) oxidative leaching; (3) calcium removal; (4) optimization of manganese-cobalt-nickel Magnesium ratio; (5) Preparation of magnesium ion-doped manganese-cobalt-nickel ternary cathode material precursor; (6) Preparation of ternary cathode material; (7) Surface modification: The ternary cathode material is dispersed in water, According to a certain mass ratio, the manganese-rich cobalt-nickel-magnesium solution and ammonium fluoride after decalcification in step (3) are used as modifiers to modify the surface of the ternary cathode material. The method is simple and feasible, can realize leaching of manganese-cobalt-nickel-magnesium waste residue, filter and remove impurities from the filtrate, directly prepare magnesium ion-doped manganese-cobalt-nickel ternary positive electrode material precursor, and prepare ternary positive electrode material, which can not only realize The comprehensive utilization of waste residue can also improve the ionic conductivity of the product, inhibit the increase of electrochemical impedance, and improve the cycle performance.

Description

technical field [0001] The invention belongs to the field of hydrometallurgy and clean metallurgy, and particularly relates to a method for preparing a ternary positive electrode material by utilizing manganese-cobalt-nickel waste residue. Background technique [0002] Manganese, cobalt and nickel are important industrial raw materials. Electrolysis is a common method for producing manganese. The basic steps are: leaching manganese ore to obtain manganese-containing leachate, then neutralizing and removing iron, removing heavy metals by vulcanizing agent, and finally electrolyzing to obtain electrolytic manganese, In the removal of heavy metals by the vulcanizing agent, a large amount of manganese, cobalt, and nickel will also be precipitated in the form of cobalt sulfide, resulting in the loss of valuable metals, manganese, cobalt, and nickel. Therefore, comprehensive utilization of manganese, cobalt, nickel and cobalt is of great significance. [0003] With the rapid growt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/62H01M4/505H01M4/525H01M10/0525
CPCH01M4/505H01M4/525H01M4/628H01M4/626H01M10/0525H01M2004/028Y02W30/84
Inventor 谢雨寻曾军叶有明谢雪珍廖政达蒋才云蓝峻峰吴元花
Owner GUANGXI NORMAL UNIV OF SCI & TECH
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