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High-purity battery-level manganese source and preparation method thereof

A technology of battery grade and manganese source, which is applied in the direction of battery electrodes, circuits, electrical components, etc., can solve the problems of poor operating environment, long cycle, low product purity, etc., and achieve the effect of easy operation

Active Publication Date: 2015-02-18
深圳市北宸创新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Manganese sulfide is a kind of manganese sulfide, which is widely used in the preparation of powder metallurgy, weak magnetic semiconductor materials and optical, electrical and magnetic materials. The traditional processes include high-temperature reduction method, solid-phase synthesis, hydrogen sulfide gas injection Products produced by the shower method have low purity, high energy consumption, long cycle time, and poor operating environment, making it difficult to achieve industrial mass production

Method used

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  • High-purity battery-level manganese source and preparation method thereof
  • High-purity battery-level manganese source and preparation method thereof
  • High-purity battery-level manganese source and preparation method thereof

Examples

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Effect test

Embodiment 1

[0035] (1) 3000KG of manganese carbonate ore powder with a total manganese content of 12%, add 1500KG 30% industrial hydrochloric acid and 500KG water for acid hydrolysis reaction, and the terminal pH value is controlled at 4.0;

[0036](2) plate and frame filtration, obtain manganese chloride acid solution;

[0037] (3) Add an appropriate amount of industrial grade sodium sulfide crystals, adjust the pH value to 5.5, and keep the temperature at 75°C, react for 120 minutes, and filter to obtain the primary manganese salt solution;

[0038] (4) prepare 25% sodium sulfide solution, stand-by;

[0039] (5) 1500KG of the primary manganese salt solution obtained in step (3) is pumped into the reactor, the stirring is started, and the temperature rises to 45° C.; the sodium sulfide solution prepared in step (4) is slowly added until the pH is stable at 8.5, and the If the manganese element is not detected, the manganese precipitation on the surface is complete; the temperature is ra...

Embodiment 2

[0050] (1) Electrolytic metal manganese 500KG, add 1800KG 50% dilute sulfuric acid to carry out acidolysis reaction, the terminal pH value is controlled at 3.0;

[0051] (2) plate and frame filtration, obtain manganese sulfate acid hydrolysis solution;

[0052] (3) prepare 25% sodium sulfide solution, stand-by;

[0053] (4) Add an appropriate amount of industrial-grade 25% sodium sulfide solution, adjust the pH value to 5.0, and keep the temperature at 68° C., react for 120 minutes, and filter to obtain the primary manganese salt solution;

[0054] (5) Pump 2200KG of the primary manganese salt solution obtained in step (3) into the reactor, start stirring, and the temperature rises to 50° C.; slowly add the sodium sulfide solution prepared in step (3) until the pH is stable at 7.0; Rise to 80°C and keep it, continue to react for 4 hours, press filter to obtain manganese sulfide filter cake;

[0055] (6) The filter cake is fully washed three times with pure water at 60° C. to...

Embodiment 3

[0065] (1) Industrial grade manganese sulfate 1500KG, add 1500KG pure water and heat up properly to fully dissolve;

[0066] (2) plate and frame filtration, obtain manganese sulfate solution;

[0067] (3) Add an appropriate amount of industrial grade sodium sulfide crystals, adjust the pH value to 5.3, and keep the temperature at 55°C, react for 120 minutes, and filter to obtain the primary manganese salt solution;

[0068] (4) prepare 25% sodium sulfide solution, stand-by;

[0069] (5) Pump 2500KG of the primary manganese salt solution obtained in step (3) into the reactor, start stirring, and the temperature rises to 55°C; slowly add the sodium sulfide solution prepared in step (4), until the pH is stable at 6.8; the temperature rises to Keep at 65°C, continue to react for 4 hours, press filter to obtain manganese sulfide filter cake;

[0070] (6) The filter cake is fully washed three times with pure water at 60°C to obtain a high-purity battery-grade manganese source-mang...

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Abstract

The invention provides a high-purity battery-level manganese source which is manganese sulfide and / or manganese oxide, wherein a manganese sulfide XRD crystal phase is a pure gamma-phase and / or pure beta-phase similar-fibrid or claviform sulfide, and the appearance is pink, brownish red or brick red. The preparation method of the high-purity battery-level manganese source comprises the following steps of preparing a divalent manganese salt solution to the concentration of 5-50 degrees Be'; adding sulphurizing salt, and filtering to prepare a primary manganese salt solution; further adding a sulfide solution, and regulating pH to prepare a manganese sulfide filter cake; carrying out reverse osmosis washing to obtain a manganese sulfide crystal; beating, then controlling the temperature of manganese sulfide slurry to 50-100 DEG C, stirring, adding an acid source to the manganese sulfide slurry to react for 2-6 hours, carrying out acidolysis to prepare a manganese salt solution, wherein the manganese sulfide inside a system needs to be excessive during the acidolysis, and the excessive mass fraction of the manganese sulfide is controlled at 1%-10%; regulating the pH to 5.5-6.0, reacting for 2-6 hours, and then carrying out pressure filtration to obtain a high-purity battery-level manganese salt product. The manganese sulfide can not only be directly applied, but also be used for synthesizing different kinds of high-end manganese salt or manganese oxide by taking the obtained manganese sulfide as the high-purity manganese source.

Description

technical field [0001] The invention relates to a method for preparing a high-purity battery-grade manganese source, in particular to a high-purity battery-grade manganese sulfide and a preparation method thereof. Background technique [0002] At present, lithium battery has become a popular emerging material in the world. As a high-voltage, low-cost manganese-lithium battery, it has attracted more and more attention and research, especially in the field of ternary lithium battery and lithium manganese oxide battery. The research and development of high-purity manganese sources has entered an unprecedented hot period; even the current lithium iron phosphate battery materials are being developed and improved by adding manganese to obtain high-voltage lithium manganese iron phosphate materials. The lithium battery materials mentioned above have extremely high requirements on the purity of the manganese source, and are also limited by extremely low cost. [0003] Manganese sul...

Claims

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Application Information

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IPC IPC(8): H01M4/50H01M4/58
CPCH01M4/502H01M4/5825Y02E60/10
Inventor 常开军
Owner 深圳市北宸创新材料科技有限公司
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