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Method for production of high purity manganese sulfate by using pyrolusite as raw material

A production method, the technology of manganese sulfate, applied in the direction of manganese sulfate, etc., can solve the problems of high impurity content, failure to meet the technical index requirements of high-purity manganese sulfate, low main content of the product, etc., and achieve simple operation, quality controllability and Highly reproducible, quality-assured results

Active Publication Date: 2013-04-03
DAXIN MANGANESE MINE BRANCH OF CITIC DAMENG MINING IND
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Problems solved by technology

[0004] However, domestic manganese sulfate production technology, whether it is wet method or fire method, the purification and impurity removal technology only stays in the simple treatment stage of oxidation-hydrolysis iron removal and sulfide removal of heavy metals, and the main content of the product is low (MnSO 4 ·H 2 O between 98% and 98.5%), high impurity content (calcium and magnesium content are above 1200ppm, potassium and sodium content are about 600ppm), far from meeting the above technical specifications of high-purity manganese sulfate

Method used

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  • Method for production of high purity manganese sulfate by using pyrolusite as raw material

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Effect test

Embodiment 1

[0018] a. Carbon fire method reduction-leaching of pyrolusite: mix pyrolusite powder and reduced coal powder in a mass ratio of 100:18, put them into a reduction furnace, roast at a temperature of 800-900°C, roast for 2 hours, and discharge the material for cooling Finally, after the reducing material and deionized water are slurried at a solid-to-liquid ratio of 1:4, sulfuric acid with a weight concentration of 98% is added. The amount of sulfuric acid added is 1.05 times the amount of acid required in theory, and the reaction time is stirred at 60°C for 2 hours. Then add iron and manganese powder, oxidize and remove iron for 1 hour, the amount of manganese powder added is 1.05 to 1.1 times the theoretical requirement, add ammonium sulfide, the amount of ammonium sulfide added is 1% of the dry weight of the reduced ore, react at room temperature for 60 minutes, filter ;

[0019] b. Remove calcium and magnesium impurities: add barium fluoride to the filtrate obtained in step ...

Embodiment 2

[0023] a. Carbon fire method reduction-leaching of pyrolusite: mix pyrolusite powder and reduced coal powder in a mass ratio of 100:18, put them into a reduction furnace, roast at a temperature of 800-900°C, roast for 2 hours, and discharge the material for cooling Finally, the reducing material and deionized water are slurried at a solid-to-liquid ratio of 1:4, and sulfuric acid with a weight concentration of 98% is added. The amount of sulfuric acid added is 1.07 times the amount of acid required in theory. , then add iron and manganese powder to oxidize and remove iron for 0.7h, the addition of manganese powder is 1.06 times of the theoretical requirement, add manganese sulfide, the addition of manganese sulfide is 1% of the dry weight of reduced ore, react at room temperature for 40min, and filter;

[0024] b. Remove calcium and magnesium impurities: add manganese fluoride to the filtrate obtained in step a, the amount added is 5 times the theoretical molar mass, react at ...

Embodiment 3

[0028] a. Carbon fire method reduction-leaching of pyrolusite: mix pyrolusite powder and reduced coal powder in a mass ratio of 100:18, put them into a reduction furnace, roast at a temperature of 800-900°C, roast for 2 hours, and discharge the material for cooling Finally, after reducing the raw material and deionized water to slurry at a solid-to-liquid ratio of 1:4, add sulfuric acid with a weight concentration of 98%, the amount of sulfuric acid added is 1.08 times the amount of acid required in theory, and the reaction time is stirred at 80°C for 2 hours. Then add iron and manganese powder to oxidize and remove iron for 1 hour. The amount of manganese powder added is 1.1 times the theoretical requirement. Add hydrogen sulfide. The amount of hydrogen sulfide added is 1% of the dry weight of the reduced ore, react at room temperature for 45 minutes, and filter;

[0029] b. Remove calcium and magnesium impurities: add barium fluoride to the filtrate obtained in step a, the a...

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Abstract

The invention relates to a production method for high purity manganese sulfate. The production method is characterized in that pyrolusite is used as a raw material and is reduced by using a carbon fire method, then an acid is added for leaching, a vulcanizing agent is used to remove heavy metals consisting of cobalt and nickel, a fluoride is employed to remove calcium and magnesium, then filtering is carried out, ammonium bicarbonate or ammonium carbonate is added into a filtrate for deposition of manganese to realize separation of potassium and sodium, an obtained filtrate is used for recovery of the by-product ammonia sulfate for usage as an additive for metal manganese, the filter residue manganese carbonate is washed and then subjected to acid dissolution so as to obtain a manganese sulfate solution, and then crystallization is carried out to obtain a high purity manganese sulfate product, wherein mother liquor can be returned to a high purity system for reutilization. With the method provided by the invention, the high purity manganese sulfate product in which MnSO4 content is more than 99.8% and respective content of impurities consisting of Ca, Mg, K and Na is lower than 10 ppm is produced.

Description

technical field [0001] The invention relates to a production method of high-purity manganese sulfate, in particular to using pyrolusite as a raw material, adopting carbon fire reduction and acid leaching to produce manganese sulfate monohydrate with a content of more than 99.8% and impurities of calcium, magnesium, potassium and sodium less than 30ppm The method of the high-purity manganese sulfate product. Background technique [0002] Manganese sulfate is a traditional manganese salt product with a wide range of uses. At present, the domestic manganese sulfate production process mainly uses pyrolusite as raw material, and is divided into two reduction leaching technologies: carbon fire reduction and wet reduction (pyrite, ferrous sulfate or titanium white waste acid and other reducing agents) and acid leaching. Then carry out simple oxidation-hydrolysis iron removal, sulfuration removal of heavy metals, filtration, static precipitation, solution crystallization, centrifug...

Claims

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Application Information

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IPC IPC(8): C01G45/10
Inventor 罗昌璃梁敏刘春明刘栋柱江炤荣周明山方广盛韦旭甜龙海平
Owner DAXIN MANGANESE MINE BRANCH OF CITIC DAMENG MINING IND
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