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Method for preparing cell-grade high-purity manganese sulfate by low-grade manganese ore high-pressure crystallization

A low-grade manganese ore and high-pressure crystallization technology, applied in the direction of manganese sulfate, etc., can solve the problems of large equipment corrosion, high energy consumption, and large sulfuric acid consumption, and achieve high profits, increase production, and reduce environmental pollution.

Inactive Publication Date: 2014-01-08
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the methods for producing manganese sulfate crystals are as follows: 1. Atmospheric pressure evaporation method, the solvent is continuously evaporated by heating the solution to achieve concentrated crystalline manganese sulfate, but this method is carried out under normal pressure, and a large amount of water needs to be evaporated, consuming a large amount of energy ; 2, concentrated sulfuric acid salting out method, in the presence of sulfuric acid, the solubility of manganese sulfate significantly decreased, mainly due to SO 4 2- The same ion effect will lead to the precipitation of manganese sulfate crystals in the solid phase, but the disadvantage of this method is that it consumes a large amount of sulfuric acid, and the corrosion of the equipment is great.
These methods generally need to use high-grade manganese ore as raw material, but as the high-grade manganese ore is exhausted, these methods for preparing manganese sulfate in the face of low-grade manganese ore are not effective, have many disadvantages, and greatly increase the cost.

Method used

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  • Method for preparing cell-grade high-purity manganese sulfate by low-grade manganese ore high-pressure crystallization
  • Method for preparing cell-grade high-purity manganese sulfate by low-grade manganese ore high-pressure crystallization
  • Method for preparing cell-grade high-purity manganese sulfate by low-grade manganese ore high-pressure crystallization

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030]The low-grade pyrolusite and pyrite are respectively ball-milled into powders with a particle size of 0.01mm. Grinding is one of the most important links in the leaching process. If the particle size is too small, the cost of grinding will increase. The leaching rate of manganese is greatly reduced, which directly affects the final production cost; the manganese sulfate solution with a concentration of 60g / L is mixed with pyrolusite powder to obtain preliminary pulp, and 100kg of preliminary pulp and 10kg of 0.01mm particle size are obtained. Pyrite powder and 20kg of concentrated sulfuric acid are prepared according to the mass ratio of the initial pulp: concentrated sulfuric acid: pyrite = 1:0.2:0.1. The temperature is heated to 75°C and kept at this temperature for 180min of manganese leaching. Such ratio, manganese leaching time and heating temperature can obtain good leaching results; The pH value of the mixed pulp is 6.5, so that the ferric ions in the pulp are pre...

Embodiment 2

[0034] The low-grade pyrolusite and pyrite were ball-milled into powders with a particle size of 0.03 mm, respectively, and a manganese sulfate solution with a concentration of 70 g / L was mixed with the pyrolusite powders to obtain a preliminary pulp. 0.03mm pyrite powder and 25kg of concentrated sulfuric acid are prepared according to the mass ratio of the initial pulp: concentrated sulfuric acid:pyrite=1:0.25:0.13 ratio, put the prepared material into the manganese soaking bucket with stirring, The temperature in the barrel was heated to 80°C and kept at this temperature for 180 min of manganese leaching, and the neutralizing agent manganese carbonate ore powder was added to the pulp to adjust the pH value. The pH value of the neutralized pulp was 6.1, so that the ferric ions in the pulp were Precipitate in the form of ferric hydroxide, so as to achieve the purpose of removing iron, add barium sulfide to the neutralized manganese sulfate-containing ore slurry, and perform pre...

Embodiment 3

[0038] The low-grade pyrolusite and pyrite were ball-milled into powders with a particle size of 0.05mm, and a manganese sulfate solution with a concentration of 80g / L was mixed with the pyrolusite powders to obtain a preliminary pulp. 0.05mm pyrite powder and 30kg concentrated sulfuric acid are prepared according to the mass ratio of the initial pulp: concentrated sulfuric acid:pyrite=1:0.3:0.15 ratio, put the prepared material into the manganese leaching bucket with stirring, The temperature in the barrel was heated to 85°C and kept at this temperature for 180min of manganese leaching, and the neutralizing agent manganese carbonate ore powder was added to the pulp to adjust the pH value. The pH value of the neutralized pulp was 5.8, so that the ferric ions in the pulp were Precipitate in the form of ferric hydroxide, so as to achieve the purpose of removing iron, add barium sulfide to the neutralized manganese sulfate-containing ore slurry, and perform pressure filtration aft...

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Abstract

The invention discloses a method for preparing cell-grade high-purity manganese sulfate by low-grade manganese ore high-pressure crystallization. The method comprises the following steps of grinding low-grade pyrolusite and pyrite into powder particles, preparing a manganese sulfate solution, mixing the manganese sulfate solution and the pyrolusite powder particles to obtain preliminary pulp, mixing the preliminary pulp, concentrated sulfuric acid and the pyrite powder particles according to a certain ratio, carrying out heating, stirring and manganese impregnation on the mixture, adding a neutralizer into the mixture to adjust a pH value, adding barium sulphide and sodium dimethyldithiocarbamate into the mixture to remove impurities so that a pure manganese sulfate solution is obtained, carrying out heating pressurization stirring on the pure manganese sulfate solution, discharging a supernatant to obtain a manganese sulfate crystal-containing solution, carrying out standing precipitation of the manganese sulfate crystal-containing solution at a normal temperature, carrying out filtration to obtain a high-concentration manganese sulfate solution, adding the high-concentration manganese sulfate solution into a high-pressure autoclave, carrying out crystallization at a high temperature under high pressure, discharging a supernatant after crystallization to obtain manganese sulfate crystal-containing magma, separating the manganese sulfate crystal-containing magma to obtain high-purity manganese sulfate crystals, and drying and crushing the high-purity manganese sulfate crystals to obtain the cell-grade high-purity manganese sulfate.

Description

technical field [0001] The invention relates to a method for preparing battery-grade manganese sulfate, in particular to using low-grade manganese ore to prepare battery-grade high-purity manganese sulfate by a high-pressure crystallization method. Background technique [0002] Compared with ordinary manganese sulfate, high-purity manganese sulfate is a high-value-added manganese deep-processing product with higher technical content and very strict production process control. Its uses are mainly in three fields: industrial field, food and medicine industry and energy field. High-purity manganese sulfate is mainly used as a raw material for nickel-cobalt lithium manganate and lithium manganese oxide in large quantities, except for the general industrial field, food and medicine industry, and nickel-cobalt lithium manganese oxide and manganese as the positive electrode material of power battery. Lithium oxide has been widely used in the production of power batteries for automo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/10
Inventor 袁明亮李康刘金华
Owner CENT SOUTH UNIV
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