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Method for preparing spheroid manganous-manganic oxide from manganese sulfate solution

A technology of manganese sulfate solution and manganese tetraoxide, which is applied in the direction of manganese oxide/manganese hydroxide, can solve the problems of large specific surface area of ​​manganese tetraoxide, easy formation of basic manganese sulfate, irregular shape, etc., and achieve production The effect of low cost, low specific surface area and high tap density

Inactive Publication Date: 2020-02-07
DAXIN MANGANESE MINE BRANCH OF CITIC DAMENG MINING IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is low in cost and easy to operate, but the prepared trimanganese tetraoxide has large specific surface area, irregular shape, low tap density, and is easy to generate basic manganese sulfate, the reaction is difficult to control, and the reaction time is long

Method used

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  • Method for preparing spheroid manganous-manganic oxide from manganese sulfate solution
  • Method for preparing spheroid manganous-manganic oxide from manganese sulfate solution
  • Method for preparing spheroid manganous-manganic oxide from manganese sulfate solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Add 110g of electrolytic manganese metal flakes and 2000mL of pure water into the dissolution tank, add 110mL of industrial concentrated sulfuric acid with a mass percentage of 98% to the dissolution tank for reaction, and after the dissolution of the manganese flakes is completed, use manganese powder to adjust the pH value of the solution to 3.0 ~4.0, add 5mL hydrogen peroxide, stir for 30min, then add 0.5g ammonium sulfide, continue stirring for 30min, and finally filter to obtain manganese sulfate solution;

[0036] (2) Prepare 2000mL of 2.5mol / L ammonia water and 200mL of 15g / L cyclopentasiloxane solution with deionized water;

[0037] (3) Add deionized water into the reaction kettle as the bottom liquid, the volume of deionized water is just enough to submerge the stirring paddle, and the water bath is heated to 70°C; under the stirring condition, the stirring speed is 300r / min, and the above-mentioned The manganese sulfate solution, ammonia water and cyclopen...

Embodiment 2

[0041] (1) Add 220g of electrolytic manganese metal flakes and 2000mL of deionized water into the dissolving tank, add 220mL of industrial concentrated sulfuric acid with a mass percentage of 98% to the dissolving tank for reaction, and adjust the pH of the solution to 3.5-4.5, add 10mL hydrogen peroxide, stir for 30min, then add 1.0g ammonium sulfide, continue stirring for 30min, and finally filter to obtain manganese sulfate solution;

[0042] (2) Prepare 2000mL of 5.0mol / L ammonia water and 200mL of 20g / L cetyltrimethylammonium bromide solution with deionized water;

[0043] (3) Add deionized water into the reaction kettle as the bottom liquid. The volume of deionized water just submerges the stirring paddle, and the water bath is heated to 70°C; under stirring conditions, the stirring speed is 250r / min, and the above-mentioned The manganese sulfate solution that step obtains, ammoniacal liquor and cetyltrimethylammonium bromide solution are added in the reactor, and mangan...

Embodiment 3

[0047] (1) Add 275g of electrolytic manganese metal flakes and 2000mL of deionized water into the dissolving tank, add 272mL of industrial concentrated sulfuric acid with a mass percentage of 98% to the dissolving tank for reaction, and adjust the pH of the solution to 4.0~5.0, add 15mL hydrogen peroxide, stir for 30min, then add 1.5g sodium thiocarba, continue stirring for 30min, and finally filter to obtain manganese sulfate solution;

[0048] (2) Prepare 2000mL of 6mol / L ammonia water and 200mL of 5g / L ethyl acetate solution with deionized water;

[0049] (3) Add deionized water into the reaction kettle as the bottom liquid, the volume of deionized water is just enough to cover the stirring paddle, and the water bath is heated to 80°C; under the stirring condition, the stirring speed is 300r / min, and the above-mentioned The manganese sulfate solution that step obtains, ammoniacal liquor and ethyl acetate solution are added in the reactor, and manganese sulfate solution feed...

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Abstract

The invention discloses a method for preparing spheroid manganous-manganic oxide from a manganese sulfate solution. The method includes the following steps that an electrolytic manganese metal sheet is dissolved, impurity-removed and purified to obtain the manganese sulfate solution with low impurity content; the manganese sulfate solution, ammonia water and additives are added into a reaction kettle in a parallel flow mode, a sufficient amount of an oxidizer is added for one-step oxidation under the stirring condition, and the reaction temperature is 50-90 DEG C; and after addition of the manganese sulfate solution is completed, the ammonia water is continued to be added for 6-10 h to control the pH value of a reaction system to be 4.5-9.5, adding of the ammonia water is stopped and thenstirring is continued, heat preservation and aging are conducted for 4-20 h, then a product is filtered and washed, and the spheroid manganous-manganic oxide is obtained by drying at 120 DEG C. The prepared spheroid erical manganous-manganic oxide D50 is 4-20 [mu]m, the tap density is greater than or equal to 2.0 g / cm<3>, and the Mn content is greater than or equal to 70.5%. The method is simple in process flow and low in production cost, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to a method for preparing spherical manganese tetraoxide from manganese oxide and manganese sulfate solution, in particular to a method for preparing spherical manganese tetraoxide from manganese sulfate solution. Background technique [0002] Lithium-ion batteries have the characteristics of high output voltage, high energy density, long cycle life, and no memory effect, and are widely used in electronic equipment, electric vehicles, energy storage batteries and other fields. In recent years, with the development of green industries such as new energy vehicles, the market demand for cathode materials for power lithium-ion batteries has gradually increased. [0003] Lithium manganese oxide, as one of the most potential anode materials for power lithium-ion batteries, has significant advantages such as abundant storage, low price, high safety performance, and no pollution to the environment. At present, the production of lithium m...

Claims

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Application Information

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IPC IPC(8): C01G45/02
CPCC01G45/02C01P2002/72C01P2004/03C01P2004/32C01P2004/61C01P2004/62C01P2006/11C01P2006/80
Inventor 李春流农艳莉闫冠杰黎兆明李剑杨茂峰黄炳行詹海青明宪权李华成
Owner DAXIN MANGANESE MINE BRANCH OF CITIC DAMENG MINING IND
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