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Preparation method of manganous-manganic oxide and manganous-manganic oxide

A technology of trimanganese tetraoxide and manganese dioxide, which is applied in the direction of manganese oxide/manganese hydroxide, etc., can solve the problems of losing application value and the particle size distribution of manganese dioxide tail powder not meeting the requirements, so as to improve the appearance and improve the Efficiency, the effect of increasing the packing density

Active Publication Date: 2012-11-07
SHENZHEN MODERN SKY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, lithium manganese oxide for power batteries is mainly prepared by solid-phase synthesis after the block EMD powder making process. In the block EMD powder making process, more manganese dioxide ultrafine powder will be produced. This part of the small particle manganese dioxide tail powder Because the particle size distribution does not meet the requirements, it loses its due application value

Method used

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  • Preparation method of manganous-manganic oxide and manganous-manganic oxide
  • Preparation method of manganous-manganic oxide and manganous-manganic oxide
  • Preparation method of manganous-manganic oxide and manganous-manganic oxide

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Embodiment 1

[0075] 1) pickling

[0076] Add deionized water to 200 kg of electrolytic manganese dioxide (EMD) tail powder according to the material-to-water ratio of 1:5 to make manganese dioxide slurry. Among them, the MnO of electrolytic manganese dioxide (EMD) tail powder 2 The content is about 91wt%, D 50 The particle size is 1.0 μm, and the Fe content is 100 ppm. Adjust the pH value of the slurry to 2.3 with sulfuric acid, stir the slurry at 65°C for 2 hours, press filter and separate, and the obtained solid phase (manganese dioxide) is washed before proceeding to the next step.

[0077] 2) The first step redox

[0078] Press MnO 2 :MnSO 4 = 1:1.5 molar ratio, that is, the manganese dioxide after pickling is added to 3120L of manganese sulfate solution with a concentration of 150g / L, and the container is replaced with nitrogen, and the solution is heated to 58°C under stirring; then, NH 3 Maintain the pH value of the solution at 7.7, and keep stirring for 1 hour after the pH va...

Embodiment 2

[0083] 1) pickling

[0084] Add deionized water to 200 kg of electrolytic manganese dioxide (EMD) tail powder according to the material-to-water ratio of 1:5 to make manganese dioxide slurry. Among them, the MnO of electrolytic manganese dioxide (EMD) tail powder 2 The content is about 91wt%, D 50 The particle size is 0.5 micron, and the mass content of Fe is 80ppm. Adjust the pH value of the slurry to 2.2 with sulfuric acid, stir the slurry at 62°C for 2 hours, press filter and separate, and the obtained solid phase (manganese dioxide) is washed and then enters the next step.

[0085] 2) The first step redox

[0086] Press MnO 2 :MnSO 4 =1:1.5 molar ratio, add manganese dioxide after pickling to 3120L of manganese sulfate solution with a concentration of 150g / L, replace with nitrogen and seal the container, stir the solution to heat up to 56°C; then, feed NH 3 The pH value of the solution was maintained at 7.6, and after the pH value of the solution was stabilized, the ...

Embodiment 3

[0090] 1) pickling

[0091] Add deionized water to 200 kg of electrolytic manganese dioxide (EMD) tail powder according to the material-to-water ratio of 1:5 to make manganese dioxide slurry. Among them, the MnO of electrolytic manganese dioxide (EMD) tail powder 2 The content is about 91wt%, D 50 The particle size is 1.8 microns, and the mass content of Fe is 150 ppm. Adjust the pH value of the slurry to 2.4 with sulfuric acid, stir the slurry at 68° C. for 2 hours, press filter and separate, and the obtained solid phase (manganese dioxide) is washed and then enters the next step.

[0092] 2) The first step redox

[0093] Press MnO 2 :MnSO 4 =1:1.5 molar ratio, add manganese dioxide after pickling to 2790L of manganese sulfate solution with a concentration of 170g / L, replace with nitrogen and seal the container, stir the solution to heat up to 58°C; then, pass in NH 3 The pH value of the solution was maintained at 7.8, and after the pH value of the solution was stabilized...

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Abstract

The invention provides a preparation method of manganous-manganic oxide and the manganous-manganic oxide. The preparation method comprises the following steps of adjusting the pH value of manganese dioxide powder slurry to be 2.0-2.5, stirring the slurry at the temperature of 60-70 DEG C and conducting solid-liquid separation; adding manganese dioxide after scouring in manganese sulfate solution with the concentration of 100-200g / L; warming the solution at nitrogen atmosphere to the temperature in the scope of 55-60DEG C; leading in NH3 holding solution with the pH value in the scope of 7.5-8.0, and maintaining, stirring and reacting for 0.8-1.2 hours after the pH value of the holding solution is stable; replacing nitrogen atmosphere by using oxygen atmosphere, leading in NH3 holding solution with the pH value in the scope of 7.0-7.5, adding 250-350g / L of MnSO4 solution, reacting until concentration of Mn+ is smaller than 500ppm, stopping the reaction, conducting solid-liquid separation, washing solid phase, and drying to obtain globular Mn3O4 products. The preparation method can use electrolytic manganese dioxide (EMD) tail powder to serve as raw materials, obtained manganous-manganic oxide products are approximately spherical and high in purity, and requirements for lithium-ion secondary battery are met.

Description

technical field [0001] The invention relates to the preparation of a manganese-based basic material for a lithium-ion secondary battery, in particular to a method for preparing spherical trimanganese tetraoxide. Background technique [0002] At present, lithium manganese oxide for power batteries is mainly prepared by solid-phase synthesis after the block EMD powder making process. In the block EMD powder making process, more manganese dioxide ultrafine powder will be produced. This part of the small particle manganese dioxide tail powder Because the particle size distribution does not meet the requirements, it loses its due application value. [0003] In the preparation of manganese-based positive electrode materials for lithium-ion secondary batteries, trimanganese tetraoxide has become a promising manganese-based material due to its excellent physical and chemical properties. EMD tail powder is used to prepare spherical lithium-ion secondary batteries through various step...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/02
Inventor 吴筱菁
Owner SHENZHEN MODERN SKY TECH CO LTD
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