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Crystallization method of nickel sulfate, cobalt sulfate and manganese sulfate

A technology of nickel sulfate and cobalt sulfate, applied in nickel sulfate, manganese sulfate, cobalt sulfate and other directions, can solve the problems of long crystallization time, inability to effectively remove impurities, and high cost, so as to improve the crystallization efficiency and avoid fine crystallization operations. Effect

Pending Publication Date: 2021-06-04
SVOLT ENERGY TECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Battery-grade nickel sulfate, cobalt sulfate, and manganese sulfate have high production requirements. In order to save energy and reduce consumption, and finely control the entire crystallization process during the evaporation crystallization process, there are high requirements for equipment and personnel operations. In order to control the impurity content, often The recrystallization process is also required, which complicates the production process and increases the production cost
[0003] It is difficult to obtain high-quality manganese sulfate from ordinary manganese sulfate materials, because various impurities cannot be effectively removed, and the crystallization recovery rate is low. At present, the following methods are mainly used in the preparation process of high-purity manganese sulfate: a. High temperature crystallization production Nickel sulfate, cobalt, and manganese; b. Production of high-purity nickel sulfate, cobalt, and manganese through multiple recrystallizations; c. Production of nickel sulfate, cobalt, and manganese crystals by anti-solvent method
Among the above preparation methods, the high-temperature crystallization and recrystallization methods involve the introduction of high-priced evaporation crystallization equipment and refined crystallization operations. The crystallization time is long, the efficiency is low, the production process is complicated, and the production cost is high; although the anti-solvent method does not use evaporation Crystallization, but solvent distillation and recovery are required, and most of the solvents are flammable and explosive organic compounds with strong volatility and great safety hazards on site; although these processes have already achieved industrial mass production, the above-mentioned defects have always existed and need to be improved
[0006] The above scheme has the problem of low purity or high cost of crystallized nickel sulfate. Therefore, it is necessary to develop a cheap nickel sulfate crystallization method that can prepare high-purity nickel sulfate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The present embodiment provides a kind of crystallization method of nickel sulfate, and described method comprises the following steps:

[0036] (1) First raise the temperature of 200g / L nickel sulfate solution to 40°C, then add 300g / L sodium sulfate powder to it, and add 3% nickel sulfate seed crystals (the seed crystals include sodium sulfate and the Nickel sulfate powder containing nickel sulfate, and additionally add nickel sulfate crystals of 2% of the total amount of nickel sulfate in the nickel sulfate solution), control the time of adding sodium sulfate powder to 2h, and continue to stir and crystallize for 2h;

[0037] (2) Centrifuge the crystallized slurry to control the water content to <10wt%. After dehydration, add 0.5 times the volume of 200g / L nickel sulfate solution to wash the crystal by centrifugation, and then continue to maintain the centrifugal speed for 10 minutes. The filter residue is dried to collect the finished nickel sulfate;

[0038] (3) Co...

Embodiment 2

[0041] The present embodiment provides a kind of crystallization method of cobalt sulfate, and described method comprises the following steps:

[0042] (1) First heat the 350g / L cobalt sulfate solution to 45°C, then add 300g / L sodium sulfate powder to it, and add 4% cobalt sulfate seed crystals (the seed crystals include sodium sulfate and the containing cobalt sulfate powder, and additionally add cobalt sulfate crystals with 2% of the total amount of cobalt sulfate in the cobalt sulfate solution), control the time of adding sodium sulfate powder to 3h, and continue to stir and crystallize for 3h;

[0043] (2) Centrifuge the crystallized slurry to control the water content to <10wt%. After the dehydration is completed, add 0.5 times the volume of 350g / L cobalt sulfate solution to wash the crystal by centrifugation, and then continue to maintain the centrifugal speed for 10 minutes. The filter residue is dried to collect the finished cobalt sulfate;

[0044] (3) Cool the mothe...

Embodiment 3

[0047] The present embodiment provides a kind of crystallization method of manganese sulfate, and described method comprises the following steps:

[0048] (1) First raise the temperature of 520g / L manganese sulfate solution to 35°C, then add 300g / L sodium sulfate powder to it, and add 5% manganese sulfate seed crystals (the seed crystals include sodium sulfate and the Manganese sulfate powder containing manganese sulfate, and additionally add manganese sulfate crystals of 2% of the total amount of manganese sulfate in the manganese sulfate solution), control the time of adding sodium sulfate powder to 2h, and continue to stir and crystallize for 3h;

[0049] (2) Centrifuge the crystallized slurry to control water content < 10wt%. After dehydration, add 0.5 times the volume of 350g / L manganese sulfate solution to wash the crystal by centrifugation, and then continue to maintain the centrifugal speed for 10 minutes. The filter residue is dried to collect the finished manganese s...

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PUM

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Abstract

The invention provides a crystallization method of nickel sulfate, cobalt sulfate and manganese sulfate, which comprises the following steps: (1) heating a nickel sulfate solution, a cobalt sulfate solution or a manganese sulfate solution, and adding sodium sulfate and seed crystal for crystallization to obtain crystallized slurry; and (2) carrying out centrifugal dewatering treatment on the crystallized slurry obtained in the step (1) to obtain filter residues and mother liquor, washing and drying the filter residues to obtain a finished product, and carrying out sodium sulfate crystallization treatment on the mother liquor to obtain sodium sulfate. According to the process, sodium sulfate is adopted as a crystallization additive, crystallization of nickel sulfate, cobalt sulfate and manganese sulfate can be achieved under the medium-low temperature condition, introduction of high-temperature crystallization equipment and fine crystallization operation are avoided, and the additive is low in cost, safe and stable.

Description

technical field [0001] The invention belongs to the technical field of crystallization and relates to a crystallization method of nickel sulfate, cobalt and manganese. Background technique [0002] Nickel sulfate, cobalt sulfate, and manganese sulfate have always been the main raw materials for the synthesis of ternary precursor materials in the field of new energy batteries, and have been widely used in medicine, printing and dyeing, electroplating and other inorganic chemical industries. Battery-grade nickel sulfate, cobalt sulfate, and manganese sulfate have high production requirements. In order to save energy and reduce consumption, and finely control the entire crystallization process during the evaporation crystallization process, there are high requirements for equipment and personnel operations. In order to control the impurity content, often A recrystallization process is also required, which complicates the production process and increases the production cost. ...

Claims

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Application Information

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IPC IPC(8): C01G53/10C01G51/10C01G45/10
CPCC01G45/10C01G51/10C01G53/10C01P2006/80
Inventor 万江涛张宁张勇杰刘满库李子郯
Owner SVOLT ENERGY TECHNOLOGY CO LTD
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