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Preparation method of high-purity manganese sulfate

A manganese sulfate, high-purity technology, applied in manganese sulfate and other directions, can solve the problems of high production cost of high-purity manganese sulfate, complicated preparation process, and increased operating cost.

Active Publication Date: 2020-11-10
TSINGHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of these processes is that it is difficult to meet the requirements for manganese fluoride to remove calcium and magnesium, and the introduction of fluoride ions
Because the existence of fluoride ions will affect the stability of lithium batteries, it is necessary to use activated alumina to absorb and remove fluorine before evaporation and concentration, the process is complicated and the operating cost is increased.
Various unfavorable factors lead to the high production cost of high-purity manganese sulfate at present, and the preparation process is relatively complicated

Method used

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preparation example Construction

[0019] The invention provides a kind of preparation method of high-purity manganese sulfate, comprises the following steps:

[0020] (1) removing heavy metal ions in the thick manganese salt solution to obtain a liquid phase product;

[0021] (2) Mix the liquid-phase product and bicarbonate to carry out precipitation of calcium, magnesium and manganese ions, and carry out solid-liquid separation after the concentration of manganese ions in the system≤0.2g / L to obtain crude manganese carbonate solid; the calcium, magnesium and manganese ions The pH value of the system during the precipitation process is ≤8.6;

[0022] (3) After the thick manganese carbonate solid is dispersed in water, carbon dioxide is introduced into the dispersion, and the refined manganese carbonate solid is obtained after solid-liquid separation;

[0023] (4) Wash the refined manganese carbonate solid and dissolve it in dilute sulfuric acid, then concentrate and crystallize to obtain high-purity manganese...

Embodiment 1

[0037] With feed grade manganese sulfate (Ca, Mg concentration is respectively 135ppm and 406ppm) as raw material, the concentration of each impurity in feed grade manganese sulfate is shown in Table 1.

[0038] Table 1. Concentration of each impurity element in feed grade manganese sulfate

[0039] Impurity elements calcium magnesium cobalt chromium copper iron Potassium sodium nickel lead silicon cadmium zinc Concentration (ppm) 1337 4058 326 32 0.0 269 8 585 617 43 155 3 2569

[0040] Dissolve 5 kg of feed grade manganese sulfate in 10 L of water, add solid sodium bicarbonate to adjust the pH of the solution to 5, and let it stand for 24 hours. Then restart stirring, add 100 grams of formane, stir for 2h, then filter. The filtrate is transferred to another 20L plastic barrel, and a sufficient amount of sodium bicarbonate solid (total amount is 2.8kg) is added under constant stirring condition, and the pH value of the...

Embodiment 2

[0046] Take 5L of manganese sulfate feed solution from Guizhou Neng Mine (see Table 3 for the concentration of impurity elements, and the concentration of manganese sulfate is 368g / L), add solid sodium bicarbonate under constant stirring, adjust the pH value of the solution to 7, let stand for 24h, filter . The filtrate was transferred to another 10L container, and 120g of sodium forma solid was added under continuous stirring, and after stirring for 2 hours, it was left to stand for 24 hours and filtered. Under constant stirring condition, add sodium bicarbonate solid (total addition is 1450g) in filtrate, the pH value of solution is controlled to below 8.6 with the mode of the sodium hydroxide solution of 100g / L. Wait for the manganese ion concentration in the solution to be less than 0.2g / L, leave standstill, treat that after most of the manganese carbonate precipitation settles to the bottom of the container, dump and discard the last clear liquid, filter, and collect the ...

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Abstract

The invention relates to the technical field of lithium battery cathode materials, and provides a preparation method of high-purity manganese sulfate, which comprises the following steps: removing heavy metal ions in a crude manganese salt solution, and mixing the obtained liquid-phase product with bicarbonate to precipitate calcium, magnesium and manganese ions, thereby obtaining a crude manganese carbonate solid; dispersing the crude manganese carbonate solid in water, and introducing carbon dioxide into the dispersion liquid to obtain a refined manganese carbonate solid; dissolving the refined manganese carbonate solid in dilute sulfuric acid, and then concentrating and crystallizing to obtain high-purity manganese sulfate. According to the method, manganese salt is converted into manganese carbonate by controlling reaction conditions, calcium carbonate and magnesium carbonate precipitated along with manganese carbonate are converted into soluble bicarbonate by introducing carbon dioxide, then calcium and magnesium ions are removed, and high-purity manganese sulfate can be conveniently obtained through sulfuric acid redissolution and crystallization. The method provided by the invention is simple in steps and low in cost, and the content of impurity ions in the obtained high-purity manganese sulfate is extremely low.

Description

technical field [0001] The invention relates to the technical field of lithium battery cathode materials, in particular to a preparation method of high-purity manganese sulfate. Background technique [0002] High-purity manganese sulfate, also known as battery-grade manganese sulfate, is one of the raw materials required for the production of ternary lithium batteries. In order to ensure the quality of lithium batteries, the purity requirements for manganese sulfate are very high. For example, the requirements for calcium and magnesium are not more than 50ppm, the concentration of other impurity metals (iron, lead, zinc, copper, etc.) shall not exceed 10ppm. The existing production process of high-purity manganese sulfate generally uses manganese fluoride to remove calcium and magnesium, sodium sulfide or sodium thiomer to remove heavy metals, and then evaporates and concentrates to obtain high-purity manganese sulfate products. The disadvantage of these processes is that i...

Claims

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Application Information

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IPC IPC(8): C01G45/10
CPCC01G45/10
Inventor 王毅李亚贾美然王邦达
Owner TSINGHUA UNIV
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