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Method for purifying manganese sulfate solution

A technology of manganese sulfate solution and purification method, which is applied in the field of purification of manganese-containing solution, and can solve the problems of high energy consumption, inability to effectively remove impurities and equipment costs, etc.

Inactive Publication Date: 2021-06-11
CHINA ENFI ENGINEERING CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The main purpose of the present invention is to provide a kind of purification method of manganese sulfate solution, to solve the problems in the prior art that the purification method of manganese sulfate solution consumes a lot of energy, cannot effectively remove impurities and has high equipment costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Get the manganese sulfate solution to be purified of 1L, wherein, the manganese sulfate solution to be purified comprises: the Mn of 60g / L 2+ , 0.4g / L of Ca 2+ , 12g / L of Mg 2+ , 1.5g / L Cu 2+ , 0.6g / L of Zn 2+ , 0.6g / L of Cd 2+ , 0.5g / L of Fe 3+ , 0.5g / L of Al 3+ , 5g / L of K + , 5g / L Na + and 0.1g / L of F - . Sodium hydroxide was added to adjust the pH of the manganese sulfate solution to be purified to 5.

[0044] The volume ratio of P204 extractant to sulfonated kerosene was selected as 1:3, and the saponification rate was controlled at 35% by using sodium hydroxide solution to obtain a saponified organic phase.

[0045] Add 0.064 mol of sodium sulfide to the manganese sulfate solution to be purified, stir to carry out the heavy metal removal reaction for 4 hours, and then separate the solid and liquid to obtain the first intermediate liquid. 1.17 mol of sodium fluoride was added to the first intermediate liquid, and the temperature was 70° C., and the decal...

Embodiment 2

[0048] Get the manganese sulfate solution to be purified of 1L, wherein, the manganese sulfate solution to be purified comprises: the Mn of 20g / L 2+ , 0.1g / L of Ca 2+ , 0.1g / L Mg 2+ , 0.1g / L of Cu 2+ , 0.01g / L Zn 2+ , 0.01g / L of Cd 2+ , 0.01g / L Fe 3+ , 0.01g / L of Al 3+ , 0.1g / L of K + , 0.1g / L Na + and 5g / L of F -. Sodium hydroxide was added to adjust the pH of the manganese sulfate solution to be purified to 4.

[0049] Select the volume ratio of P204 extractant to sulfonated kerosene as 3:7, and use sodium hydroxide solution to control its saponification rate at 50%, to obtain a saponified organic phase.

[0050] Add 0.0028 mol of ammonium sulfide to the manganese sulfate solution to be purified, stir for 2 hours to remove heavy metals, and then separate the solid and liquid to obtain the first intermediate liquid. Add 0.1185 mol of ammonium fluoride to the first intermediate liquid, perform a decalcification reaction at 80°C for 2 hours, and then separate the sol...

Embodiment 3

[0053] Get the manganese sulfate solution to be purified of 1L, wherein, the manganese sulfate solution to be purified comprises: the Mn of 100g / L 2+ , 0.6g / L of Ca 2+ , 24g / L of Mg 2+ , 3g / L Cu 2+ , 1g / L of Zn 2+ , 1g / L of Cd 2+ , 1g / L of Fe 3+ , 1g / L of Al 3+ , 10g / L of K + , 10g / L of Na + and 0.1g / L of F - . Add sodium hydroxide to adjust the pH of the manganese sulfate solution to be purified to 6.

[0054] The volume ratio of P204 extractant to sulfonated kerosene was selected as 1:9, and the saponification rate was controlled at 30% by using sodium hydroxide solution to obtain a saponified organic phase.

[0055] Add 0.143 mol of sodium sulfide to the manganese sulfate solution to be purified, stir to carry out the heavy metal removal reaction for 6 hours, and then separate the solid and liquid to obtain the first intermediate liquid. 2.24 mol of sodium fluoride was added to the first intermediate liquid, the temperature was 70° C., and the decalcification rea...

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Abstract

The invention provides a method for purifying a manganese sulfate solution. The purification method comprises the steps of S1, removing heavy metals from a manganese sulfate solution to be purified by using a sulfide, and carrying out first solid-liquid separation to obtain a first intermediate liquid; S2, removing calcium from the first intermediate liquid by using fluoride, and carrying out second solid-liquid separation to obtain a second intermediate liquid; S3, removing fluorine from the second intermediate liquid by using magnesium sulfate or magnesium chloride, and performing third solid-liquid separation to obtain a third intermediate liquid; S4, extracting the third intermediate liquid by adopting a saponified organic phase to obtain a manganese-rich organic phase; S5, washing the manganese-rich organic phase with first sulfuric acid to obtain a purified manganese-rich organic phase; and S6, conducting reverse extraction on the purified manganese-rich organic phase through second sulfuric acid, and obtaining a high-purity manganese sulfate solution and a regenerated organic phase. Manganese ions and magnesium ions in the third intermediate liquid arepurified by adopting the extraction-washing-reverse extraction process to obtain the high-purity manganese sulfate solution.

Description

technical field [0001] The invention relates to the technical field of purification of manganese-containing solutions, in particular to a method for purifying manganese sulfate solutions. Background technique [0002] The ternary nickel-cobalt-manganese cathode material is a very important cathode material. It has important advantages such as better performance than lithium cobalt oxide, much lower cost than lithium cobalt oxide, and much higher energy density than lithium iron phosphate. Mainstream cathode material for power batteries. With the development of ternary battery materials, the demand for battery grade manganese sulfate is increasing. However, since the manganese sulfate used in battery production has very strict requirements on impurities such as calcium, magnesium, copper, zinc, cadmium, and fluorine, the manganese sulfate solution needs to be purified before synthesizing the ternary material precursor. [0003] For example, the Chinese patent application wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G45/10
CPCC01G45/10C01G45/003C01P2006/80
Inventor 王恒利张阳郑明臻崔宏志戴江洪李俊殷书岩王宏岩
Owner CHINA ENFI ENGINEERING CORPORATION
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