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A kind of high-density doped manganese tetraoxide and its preparation method

A manganese tetroxide, high-density technology, used in manganate/permanganate, electrical components, battery electrodes, etc., can solve the problems of complex production process, difficult to guarantee uniformity, low tap density, etc. Good doping uniformity, good particle morphology and stable doping effect

Active Publication Date: 2016-02-10
SINOSTEEL ANHUI TIANYUAN TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, if ordinary trimanganese tetroxide is to be used to prepare dynamic lithium manganate, there are still two deficiencies: first, ordinary trimanganese tetraoxide has small particle size, large specific surface area, and low tap density, resulting in the use of the prepared lithium manganese oxide. The lithium manganese oxide material has a large specific surface area and low compaction density, which is difficult to meet the requirements: second, the power type lithium manganate needs to use doping technology to overcome the Jahn-Teller effect, thereby improving the high temperature and cycle performance of the material, while Produced by ordinary manganese tetraoxide, the mixing of doping elements needs to be completed in the dry mixing process in the lithium manganate production process, and the uniformity is difficult to guarantee
This method can obtain spherical aluminum-doped trimanganese tetraoxide, but it needs to be rinsed with a large amount of deionized water to separate the sodium salt from the trimanganese tetraoxide, and the reaction produces a large amount of by-product sodium salt, which requires additional processes Recycling is carried out, so the production process is complicated by this method

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  • A kind of high-density doped manganese tetraoxide and its preparation method

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preparation example Construction

[0017] The method for preparing high-density doped trimanganese tetroxide of the present invention includes the following steps:

[0018] (1) Grinding: the metal manganese and doped oxide are massaged by Mn:M x O y =3: 0.01~0.3 is added to the mill, and the mixture is wet ground to a certain particle size;

[0019] (2) Reaction: Add the ground slurry to the reactor, then add ammonium salt as a catalyst according to 0.5%-10% of the total weight of the metal manganese, and pass in air or oxygen, and control the reaction temperature to 70℃±10℃ , Control the PH value of 6.5-7.0, and carry out the catalytic oxidation reaction;

[0020] (3) Washing: Use washing equipment to wash one or more times to remove impurity elements doped in trimanganese tetroxide;

[0021] (4) Drying: Use drying equipment to dry the trimanganese tetroxide after washing to obtain a trimanganese tetroxide product with high density and uniform doping.

[0022] Wherein, in step (1): the metal manganese is one or two of ...

Embodiment 1

[0028] (1) Grinding: The metal manganese sheet with a purity of 99.1% and aluminum oxide with a purity of 99.8% are combined according to the molar ratio Mn:Al 2 O 3 =3:0.07 for the ratio, the total weight is 1200Kg, add it to the ball mill, grind for 6h, control the slurry D50 (particle size) to 0.93um;

[0029] (2) Reaction: Add the ground slurry to the reactor, then add 50Kg of ammonium chloride, and start the air reaction. During the reaction, the pH value is controlled to be 6.6±0.1, and the reaction temperature is 75°C±3°C. When the reaction pH is less than or equal to 6.4, it is determined as the end point, and the reaction is 12 hours;

[0030] (3) Washing: Use a counter-current washing machine to wash the reacted slurry to control various impurities, especially Cl - , Controlled below 200ppm;

[0031] (4) Drying: Use spray drying equipment to dry the washed slurry. The inlet temperature is controlled to 300℃±5℃, the outlet temperature is controlled to 120℃±5℃, and the produc...

Embodiment 2

[0034] (1) Grinding, the metal manganese powder with purity of 99.1%, aluminum oxide with purity of 99.8% and magnesium oxide with purity of 99.6% are combined according to the molar ratio Mn:Al 2 O 3 :MgO=3:0.05:0.02, the total weight is 600Kg, add it to the ball mill, grind for 4h, control the slurry D50 (particle size) to 0.92um;

[0035] (2) For reaction, add the ground slurry to the reactor, then add 30Kg of ammonium chloride, and start the air reaction. During the reaction, the pH value is controlled to be 6.9±0.1, and the reaction temperature is 70°C±3°C. When the reaction pH is less than or equal to 6.4, it is determined as the end point, and the reaction is 10 hours;

[0036] (3) Washing, using a countercurrent washing machine to wash the reacted slurry to control various impurities, especially Cl - , Controlled below 200ppm;

[0037] (4) Drying, using spray drying equipment to dry the washed slurry, the inlet temperature is controlled to 300℃±5℃, the outlet temperature is c...

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Abstract

The invention discloses high-density doped trimanganese tetroxide. The chemical formula of the high-density doped trimanganese tetroxide is Mn3O4*zMxOy, wherein z is within the range of 0.01-0.3; and MxOy is one or several of MgO, Ni2O5, Co3O4, Cr2O3, Al2O3, ZrO2, V2O5 and TiO2, or rare earth oxide. The physical indexes of the high-density doped trimanganese tetroxide are as follows: D50 (particle size) is within the range of 3-25 microns; the tap density is within the range of 2.1-2.6 g / cm3; BET is within the range of 1 to 4 m<2> / g; and the particle morphology is a spherical shape. The invention further discloses a preparation method for the trimanganese tetroxide; the method enables manganese to be continuously agglomerated with doped oxide in the process of being converted to the trimanganese tetroxide; and the growth direction and the growth speed of agglomerates are controlled by using the pH value, the reaction temperature and the adding quantity of ammonium salt catalyst to obtain the doped trimanganese tetroxide with good doping uniformity, good particle morphology and high density.

Description

Technical field [0001] The invention relates to trimanganese tetroxide, a raw material for battery cathode material lithium manganate and a preparation method thereof. Background technique [0002] Lithium manganate is one of the more promising cathode materials for lithium-ion batteries. With the advancement of lithium manganate material technology, the consumption of lithium manganate is also increasing year by year. However, the manganese source selected for the traditional lithium manganate material is manganese dioxide, and its capacity performance and cycle performance limit the further expansion of the lithium manganate material. In recent years, with the deepening of research, lithium manganese oxide manufacturers have discovered that lithium manganese oxide materials prepared by using trimanganese tetroxide as a manganese source have better capacity and cycle performance. The main reason is that compared with manganese dioxide, the crystal form of trimanganese tetroxide...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/505C01G45/12
CPCY02E60/10
Inventor 杨洋马金保陈思学王志鹏王以存鲁俊
Owner SINOSTEEL ANHUI TIANYUAN TECH
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