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Method for preparing trimanganese tetraoxide by using acid-soluble manganese ore based on sulfur and ammonia cycle

A manganese tetroxide, acid-soluble technology, applied in manganese oxide/manganese hydroxide and other directions, can solve the problems of heavy metal pollution of soil, lower price of ammonium sulfate, low utilization value, etc., to reduce the energy consumption of pyrolysis and comprehensive utilization. High rate and the effect of reducing purchases

Active Publication Date: 2019-07-23
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of preparing trimanganese tetroxide by manganese sulfate liquid phase oxidation, when ammonia water is used as a neutralizing agent, a large amount of ammonium sulfate solution will be produced. Since the solution contains a small amount of manganese, it is easy to use it as a nitrogen fertilizer. Cause heavy metal pollution in the soil, so it is difficult to follow-up use
And at present, due to the overcapacity of chemical fertilizers, the price of ammonium sulfate continues to decrease, and the economic benefits are low. Taking nitrogen fertilizer as the follow-up utilization object has little utilization value.

Method used

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  • Method for preparing trimanganese tetraoxide by using acid-soluble manganese ore based on sulfur and ammonia cycle
  • Method for preparing trimanganese tetraoxide by using acid-soluble manganese ore based on sulfur and ammonia cycle
  • Method for preparing trimanganese tetraoxide by using acid-soluble manganese ore based on sulfur and ammonia cycle

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Utilize manganese carbonate ore to prepare manganese tetroxide, and the specific process steps are as follows:

[0032] (1) leaching: utilize ammonium hydrogen sulfate solution as leaching agent to mix slurry with manganese carbonate ore, the mol ratio of manganese in ammonium hydrogen sulfate and manganese carbonate ore is 3:1, so that the manganese of manganese ore is converted into soluble manganese sulfate, and the obtained slurry is carried out Press filtration to obtain waste residue and a separation liquid containing manganese sulfate;

[0033] (2) Purification and impurity removal: air is introduced into the separation liquid obtained in step (1), so that Fe in the leaching liquid is 2+ oxidized to Fe 3+ , and adding ammonia water to adjust the pH to 5.5 to convert it into Fe(OH) 3 precipitation, while the Al in the leaching solution 3+ Converted to Al(OH) 3 Precipitation, solid-liquid separation to obtain Fe(OH) 3 , Al(OH) 3 Precipitation and separation l...

Embodiment 2

[0043] The manganese oxide ore after the reduction of pyrolusite is used to prepare manganese tetroxide, and the operation steps are as follows:

[0044] (1) Leaching: using ammonium hydrogen sulfate solution as a leaching agent to mix with the original manganese oxide ore, the molar ratio of ammonium hydrogen sulfate and manganese in the manganese ore is 2.5:1, so that the manganese in the manganese ore is converted into soluble manganese sulfate, and the The obtained slurry is centrifuged to obtain a waste residue and a separation liquid containing manganese sulfate.

[0045] (2) purifying and removing impurities: adding hydrogen peroxide to the separation liquid obtained in step (1) to make Fe in the leaching solution 2+ oxidized to Fe 3+ , and adding ammonia water to adjust the pH to 6.0 to convert it into Fe(OH) 3 precipitation, while the Al in the leaching solution 3+ Converted to Al(OH) 3 Precipitation, solid-liquid separation to obtain Fe(OH) 3 , Al(OH) 3 Precipi...

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Abstract

The invention provides a method for preparing trimanganese tetroxide by utilizing acid-soluble manganese ore and on basis of sulfur-ammonia circulation. The method comprises the following steps: (1) leaching; (2) purifying and removing impurities; (3) precipitating manganese, namely adding ammonia water and an oxidizing agent into the obtained manganese sulfate solution, and converting manganese hydroxide into trimanganese tetroxide; (4) carrying out solid-liquid separation; (5) evaporating and crystallizing; (6) drying; (7) carrying out pyrolysis on ammonium sulfate, namely carrying out pyrolysis on the obtained ammonium sulfate crystals, so that ammonium bisulfate crystals and ammonia gas are obtained; (8) recycling ammonium bisulfate, namely dissolving the obtained ammonium bisulfate crystals into water to obtain ammonium bisulfate solution, returning to the step (1) to be used as a leaching agent for leaching manganese in a manganese ore; and (9) recycling ammonia gas, namely absorbing the obtained ammonia gas with water and preparing into the ammonia water, and returning to the step (2) and / or the step (3) as a neutralizing agent. The method provided by the invention can realize recycling of ammonium sulfate produced in a trimanganese tetroxide preparation process by virtue of a manganese sulfate liquid-phase oxidation process and can be used for solving the problem that resource utilization of ammonium sulfate is difficult.

Description

technical field [0001] The invention belongs to the field of resource utilization for preparing manganese oxide from manganese ore, and particularly relates to a method for preparing manganese tetroxide by using acid-soluble manganese ore. Background technique [0002] Manganese tetroxide is an important magnetic material and a high-quality raw material for soft ferrite and lithium batteries for new energy vehicles. At present, there are two main production methods for manganese tetroxide: (1) manganese sulfate or manganese carbonate pyrolysis method; (2) electrolytic manganese or manganese sulfate solution liquid-phase oxidation method. Among them, the manganese sulfate liquid-phase oxidation method has the advantages of low cost and easy operation. Utilizing manganese sulfate liquid-phase oxidation to prepare manganese tetroxide includes the following three steps: (1) leaching manganese carbonate ore or pyrolusite reduced by roasting with a solution containing sulfuric ac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G45/02
CPCC01G45/02
Inventor 孙维义苏仕军丁桑岚
Owner SICHUAN UNIV
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