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Method for removing calcium and magnesium ions in high-purity manganese sulfate production

A technology of calcium and magnesium ions and manganese sulfate, applied in the direction of manganese sulfate, etc., can solve problems such as excess solubility, and achieve the effects of simple steps, good removal effect, and easy operation.

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

AI Technical Summary

Problems solved by technology

However, in production, the concentration of manganese sulfate often reaches 500-600g / L, and the ionic strength of the solution is very high, so that the solubility of calcium fluoride and manganese fluoride far exceeds their solubility product.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Get feed grade manganese sulfate 3kg (Ca, Mg concentration are respectively 135ppm and 406ppm), be dissolved in 5L water, add the sodium bicarbonate of sufficient amount (total addition is 1.7kg) under the non-stop stirring condition, the pH value of solution is with drop The method of adding 20g / L sodium hydroxide solution is controlled to below 8.6. After the manganese ion concentration in the solution is less than 0.2g / L, filter it. Collect the crude manganese carbonate filter cake (theoretical dry weight of manganese carbonate obtained is 2.14kg).

[0032] The obtained crude manganese carbonate filter cake was added into 10.7kg of high-purity water (liquid-solid ratio 5:1), and stirred to uniformly suspend the manganese carbonate. Weigh 117g of sodium carbonate in advance and dissolve it in 1000mL of ultrapure water, add the sodium carbonate solution into the manganese carbonate slurry under constant stirring, and continue stirring for 2 hours. Then carbon dioxide...

Embodiment 2

[0035] Guizhou Neng Mine manganese sulfate feed solution 5L (manganese sulfate concentration 368g / L, Ca, Mg concentration are 180ppm and 250ppm respectively, solution acidity pH value 3.2), add enough sodium bicarbonate (a total amount is 1200g ), the pH value of the solution is controlled to below 8.6 by adding dropwise the sodium hydroxide solution of 20g / L. After the manganese ion concentration in the solution is less than 0.2g / L, filter it. Collect the crude manganese carbonate filter cake (theoretical dry weight of manganese carbonate obtained is 1.31kg).

[0036] The obtained crude manganese carbonate filter cake is transferred to 10.5kg of high-purity water (liquid-solid ratio 8:1), stirred, and the manganese carbonate is evenly suspended. Take by weighing 122g sodium carbonate in advance and be dissolved in 1000mL ultrapure water, sodium carbonate solution is added in the manganese carbonate slurry under the condition of constant stirring, after stirring, the molar co...

Embodiment 3

[0039] Guizhou Neng Mine manganese sulfate feed liquid 5L (manganese sulfate concentration 368g / L, Ca, Mg concentration are 180ppm and 250ppm respectively, solution acidity pH value 3.2), add a sufficient amount of sodium hydroxide (total addition is 950g), until slurry pH>12. After the manganese ion concentration in the solution is less than 0.1g / L, filter it. Collect the crude manganese hydroxide filter cake (theoretical dry weight of manganese hydroxide obtained is 1.02kg).

[0040] The obtained thick manganese hydroxide filter cake is transferred to 5.5kg of high-purity water (liquid-solid ratio 5:1), stirred, and the manganese hydroxide is evenly suspended. Weigh 70g of sodium carbonate in advance and dissolve it in 1000mL of ultrapure water, add the sodium carbonate solution into the manganese hydroxide slurry under constant stirring, after stirring evenly, the molar concentration of sodium carbonate in the slurry is about 0.1mol / L , continue to stir for 2h. Then carb...

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PUM

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Abstract

The invention relates to the technical field of lithium battery positive electrode materials, and provides a method for removing calcium and magnesium ions in high-purity manganese sulfate production.The method provided by the invention comprises the following steps: firstly, adding soluble carbonate to convert a high-purity manganese sulfate precursor (crude manganese carbonate and / or crude manganese hydroxide) into manganese carbonate, simultaneously converting calcium and magnesium ions in the manganese carbonate into calcium carbonate and magnesium carbonate, and then introducing carbon dioxide to convert the calcium carbonate and the magnesium carbonate into calcium bicarbonate and magnesium bicarbonate; calcium bicarbonate and magnesium bicarbonate are easily dissolved in water andcan be separated from manganese carbonate through solid-liquid separation, so that calcium and magnesium ions are removed. The method provided by the invention is simple in steps, easy to operate, lowin cost and good in calcium and magnesium ion removal effect.

Description

technical field [0001] The invention relates to the technical field of positive electrode materials for lithium batteries, in particular to a method for removing calcium and magnesium ions in the production of high-purity manganese sulfate. Background technique [0002] High-purity manganese sulfate is called battery-grade manganese sulfate, which 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 10ppm. The existing calcium and magnesium removal process generally uses manganese fluoride, because manganese fluoride has a relatively large solubility in the solution, and the fluoride ions dissolved in the solution, and the calcium and magnesium ions in the solution form calcium fluoride and magnesium fluoride precipitation , so that the concentration of cal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/10
CPCC01G45/10
Inventor 王毅李亚艾云艳王邦达贾美然
Owner TSINGHUA UNIV
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