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Preparation method of manganous-manganic oxide

A technology of manganese tetroxide and manganese powder, applied in manganese oxide/manganese hydroxide and other directions, can solve the problems of slow manganese hydrolysis, influence of purity, chlorine and sulfur residues, etc., to accelerate the hydrolysis reaction, accelerate the complexation, shorten the effect of time

Inactive Publication Date: 2013-04-24
JISHOU UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In fact, the addition of ammonium oxalate will form manganese oxalate precipitate with manganese ions, and the predetermined manganese hydroxide cannot be obtained, and the weak complexing ability of ammonium formate and ammonium acetate to manganese ions makes the hydrolysis rate of manganese slower
[0008] Chinese patent CN1252385A proposes to prepare trimanganese tetraoxide by a two-step method. In the first step, the metal manganese powder is completely generated into manganese hydroxide or basic manganese salt under the action of a catalyst, and in the second step, it is oxidized into trimanganese tetraoxide. ; Because the catalyst used in the embodiment is traditional catalyst ammonium sulfate, ammonium chloride, usually the catalyst concentration used is not less than 15g / L, the product still has chlorine and sulfur residues after washing, and the purity is affected
In addition to the Cl that will be brought by this method - In addition to residues, another biggest problem is that the specific surface area of ​​the produced manganese tetraoxide is relatively small, generally only 5-10m 2 / g, it is of practical significance to study the use of more suitable catalysts to prepare high-purity, high-specific surface area trimanganese tetroxide

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

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Example 1: The first step reaction conditions: take manganese powder with particle size less than 50 μm, ammonium lactate concentration 10g / L, temperature 40°C, stirring speed 300rpm / min, react for 5h, all manganese hydroxides are generated; the second step Reaction conditions: At a temperature of 60°C, a sufficient amount of air is introduced to oxidize, the stirring speed is 300rpm / min, and the reaction is completed in 4 hours. After washing and drying, trimanganese tetraoxide is obtained. The product index is: the manganese content is 71.6%, Na 2 O0.0045%, CaO0.0025%, MgO0.0045%, S0.007%, the specific surface area measured by BET method is 25.4m 2 / g; after adding 10-20% of the amount of ammonium ortholactate to the above-mentioned filtrate, it can be recycled.

Embodiment 2

[0034] Example 2: The first step reaction conditions: take manganese powder with a particle size of less than 50 μm, the concentration of ammonium succinate is 20g / L, the temperature is 50°C, the stirring speed is 400rpm / min, and the reaction is 6h, all of which are precursors of trimanganese tetraoxide body; the second step reaction conditions: at a temperature of 50°C, pass in a sufficient amount of air to oxidize, the air is dispersed into small bubbles through the air distributor, the stirring speed is 400rpm / min, the reaction is completed for 6h, and the trimanganese tetraoxide is obtained after washing and drying , its product index is: manganese content is 71.8%, Na 2 O0.0048%, CaO0.0035%, MgO0.0044%, S0.006%, the specific surface area measured by BET method is 26.5m 2 / g; the above-mentioned filtrate is recycled after adding 10-20% of the amount of ammonium orthosuccinate.

Embodiment 3

[0035] Example 3: Take manganese powder with a particle size of less than 50 μm, ammonium lactate concentration 20g / L, temperature 30°C, stirring speed 300rpm / min, react for 3h, and all produce trimanganese tetraoxide precursors; the second step reaction conditions: at temperature At 70°C, a sufficient amount of air is introduced to oxidize, the air is diffused into small bubbles through the air distributor, the stirring speed is 500rpm / min, and the reaction is completed in 4.5h. After washing and drying, trimanganese tetraoxide is obtained. The product index is: the manganese content is 71.9%, Na 2 00.0040%, CaO0.0046%, MgO0.0033%, S0.006%, the specific surface area measured by BET method is 24.8m 2 / g; after adding 10-20% of the amount of ammonium ortholactate to the above-mentioned filtrate, it can be recycled.

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Abstract

The invention discloses a preparation method of manganous-manganic oxide. Manganese metal powder is manufactured into manganous-manganic oxide with high purity and high specific surface area by using a two-step method in the presence of an organic acid catalyst or an organic acid amine salt catalyst. In the first step, the manganese powder is added into a solution containing the catalyst and hydrolyzed and reacted for a period of time, and all manganese powder is completely converted into hydroxide of the manganese; and in the second step, a suspension containing the hydroxide of the manganese is oxidized by air, filtered and dried by airflow so as to obtain solid powder of the manganous-manganic oxide, and a filter liquor is continuously used after being supplemented with a little amount of lost catalysts. The catalyst is characterized by being the organic acid or the amine salt of the organic acid; through adoption of the catalyst, the reaction speed can be increased, impurities in a product are reduced, the purity of the product is improved, the specific surface area of the product is increased and the manganous-manganic oxide with high purity and high specific surface area can be obtained.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a preparation method of manganese tetraoxide. The invention relates to a catalyst used in the production of manganese manganese tetraoxide with high purity and high specific surface area by a two-step method of hydrolysis and oxidation of metal manganese powder. Background technique [0002] As an important industrial raw material, electronic grade trimanganese tetraoxide is mainly used in the preparation of manganese zinc ferrite and Li-Mn-O batteries, and their performance is affected by the purity and specific surface area of ​​trimanganese tetraoxide used. In the national standard GB / T21836-2008, there are specific regulations on the use of manganese tetraoxide for soft magnetic bodies. There is no clear regulation on the trimanganese tetraoxide used in the preparation of Li-Mn-O batteries, but experiments have confirmed that the Li-Mn-O battery positive electro...

Claims

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Application Information

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IPC IPC(8): C01G45/02
Inventor 陈上吴显明李长安刘伟刘建本
Owner JISHOU UNIVERSITY
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