Method for preparing high-purity manganese sulfate and high-purity manganese carbonate by reduction leaching of pyrolusite through scrap iron

A technology of pyrolusite and manganese sulfate, applied in manganese sulfate, chemical instruments and methods, ferric sulfate, etc., can solve the problems of large impurity content, high production cost, complicated process, etc., and achieves reduction of impurity ions, easy operation, and technological process simple effect

Inactive Publication Date: 2012-09-05
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Using pyrolusite as raw material to convert Mn 4+ reduced to Mn 2+ Prepare a manganese sulfate solution, which requires the manganese sulfate solution to be clear and transparent, with a rose red color, a concentration of more than 60g / L, and a pH value of 5-6, and then add a precipitant to produce manganese carbonate; the production of manganese carbonate with manganese salt solution is often industrial production The manganese-containing waste liquid or by-products produced in the process have a large amount of impurities and are not easy to purify; high-purity manganese carbonate can be obtained by using electrolytic manganese as raw material to produce manganese carbonate. After dissolving, the solution is clear and transparent and has a rose red color. Finally, a precipitant is added to produce high-purity manganese carbonate. This method contains the least impurities, but the process is complicated, the investment is large, and the production cost is high.

Method used

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  • Method for preparing high-purity manganese sulfate and high-purity manganese carbonate by reduction leaching of pyrolusite through scrap iron
  • Method for preparing high-purity manganese sulfate and high-purity manganese carbonate by reduction leaching of pyrolusite through scrap iron
  • Method for preparing high-purity manganese sulfate and high-purity manganese carbonate by reduction leaching of pyrolusite through scrap iron

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add pyrolusite and deionized water to the reaction kettle, slowly add 98% concentrated sulfuric acid under mechanical stirring, so that the liquid-solid mass ratio in the reaction kettle is 8:1, after mixing evenly, the temperature rises to 50°C and then adds iron Shavings, the initial concentration of sulfuric acid in the reactor is 1.0mol / L, the molar ratios of iron filings, sulfuric acid and manganese dioxide in pyrolusite are 0.6:1 and 2:1 respectively, and after 0.5h of reaction, the temperature is raised to 100°C to continue the reaction for 1h , under the constant condition of keeping the temperature in the reactor, add calcium carbonate to adjust the pH value of the solution to 5 so that the ferric iron in the solution is completely hydrolyzed to ferric hydroxide, obtain the filter residue and the initial filtrate of manganese sulfate through filtration, and add to the obtained sulfuric acid Barium sulfide was added to the primary manganese filtrate to make the N...

Embodiment 2

[0030] Add pyrolusite and deionized water to the reaction kettle, slowly add 98% concentrated sulfuric acid under mechanical stirring, so that the liquid-solid mass ratio in the reaction kettle is 5:1, after mixing evenly, the temperature rises to 30°C and iron filings are added , the initial concentration of sulfuric acid in the reactor is 1.5mol / L, and the mol ratios of iron filings, sulfuric acid and manganese dioxide in pyrolusite are respectively 1.3:1, 1.5:1, and the reaction is heated up to 80°C for 1h to continue the reaction for 0.5h. Under the condition of keeping the temperature in the reaction kettle constant, add calcium carbonate to adjust the pH value of the solution to 6 so that the ferric iron in the solution is completely hydrolyzed into ferric hydroxide, and the initial filtrate of manganese sulfate is obtained by filtration, and the obtained manganese sulfate initial Add sodium dimethyl dithiocarbamate (SDD) in the filtrate to make the Ni in the solution 2+...

Embodiment 3

[0032] Add pyrolusite and deionized water to the reaction kettle, slowly add 98% concentrated sulfuric acid under mechanical stirring, so that the liquid-solid mass ratio in the reaction kettle is 10:1, mix evenly and raise the temperature to 60°C and add iron filings , the initial concentration of sulfuric acid in the reactor was 2.0mol / L, and the molar ratios of iron filings, sulfuric acid and manganese dioxide in pyrolusite were 1.0:1 and 2.5:1 respectively. After 1 hour of reaction, the temperature was raised to 70°C to continue the reaction for 1.5 hours. Under the constant temperature condition in the reactor, add calcium carbonate to adjust the pH value of the solution to 5.5 and make the ferric iron in the solution be completely hydrolyzed to ferric hydroxide, obtain the first filtrate of manganese sulfate through filtration, and add the first filtrate to the manganese sulfate first filtrate of gained A mixture of barium sulfide and sodium dimethyldithiocarbamate (SDD) ...

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Abstract

The invention discloses a method for preparing high-purity manganese sulfate and high-purity manganese carbonate by reduction leaching of pyrolusite through scrap iron. The method comprises the following steps of: performing reduction leaching on the pyrolusite with the scrap iron in a sulfuric acid medium to obtain manganese, regulating the pH value to be 5-6 by using a neutralization method, hydrolyzing ferric iron in the solution into an iron hydroxide precipitate, and filtering to obtain primary filtrate of manganese sulfate and filter residue; adding a vulcanizing agent into the primary filtrate for vulcanization to remove heavy metal ions, adding a fluorinating agent for removing calcium, magnesium and other ions in the solution, standing the solution and removing sediments; and concentrating and crystallizing the purified solution to prepare the high-purity manganese sulfate, or adding ammonium carbonate to prepare high-purity manganese carbonate, concentrating the filtrate andrecovering the ammonium carbonate, wherein the filter residue in the first step is leached by solution of dilute sulfuric acid, and the filtrate after filtration is subjected to calcium removal, standing and concentration to form polyferric sulfate. The method is low in cost and investment, is suitable for comprehensive exploitation and utilization of different grades of pyrolusite, can effectively utilize natural resources and also can create obvious economic benefit.

Description

technical field [0001] The invention belongs to the field of metallurgy, and in particular relates to a method for leaching pyrolusite by using iron filings as a reducing agent, preparing high-purity manganese sulfate and high-purity manganese carbonate, and simultaneously recovering ammonium sulfate and polyferric sulfate. Background technique [0002] Manganese sulfate is one of the important basic manganese salts, and most manganese products are prepared through manganese sulfate or manganese sulfate solution. In the traditional production process, leaching rhodochrosite with sulfuric acid to prepare high-purity manganese sulfate and its manganese products has higher quality requirements for rhodochrosite, which is mainly because the impurity content is too high in the process of leaching rhodochrosite, especially magnesium. The content (calculated as MgO) is generally required to be less than 1%. For my country's manganese ore resources, there are not many high-grade rhod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G45/10C01G45/00C01G49/14C01C1/24
Inventor 易清风蔡振勇
Owner HUNAN UNIV OF SCI & TECH
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