Method for producing high-purity cobalt chloride by utilizing cobalt carbonate defective products

A technology of cobalt chloride and cobalt carbonate, which is applied in chemical instruments and methods, cobalt halides, cobalt compounds, etc., can solve the problems of being unable to be directly acid-soluble and having no cost advantage, and achieves low production cost, high cobalt recovery rate, The effect of simple process

Active Publication Date: 2018-07-27
XIAMEN TUNGSTEN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, in the production process of lithium cobalt oxide cathode materials, the precursors are commonly mixed according to different models. For the unqualified materials caused by physical factors such as morphology and particle size in the production process, no other substances are introduced except for the doping elements. impurities, but this type of waste has not been effectively separated according to different types of impurities during the production process, so that the elements entrained by different additives are mixed and cannot be used directly in acid solution
If this type of material is treated with conventional waste: acid dissolution-impurity removal-extraction, there is no cost advantage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1: Utilize cobalt carbonate residual product to produce high-purity cobalt chloride

[0041] Weigh the residual cobalt carbonate and add water to the stirred reactor for slurrying. A 160 g / l hydrochloric acid solution was added to a final pH=1.5.

[0042] Cobalt carbonate was added to the resulting solution to reverse the pH to 3.5, and a cobalt chloride solution was obtained after pressure filtration.

[0043] Pour the above cobalt chloride solution into a heated and stirred reactor, raise the temperature to 85°C, and slowly add 40g / l sodium hydroxide solution to adjust the pH to 4.5-5.0 under the condition of sufficient stirring.

[0044] When the pH is completely stable at 4.5-5.0, slowly add ammonium fluoride with an excess coefficient of 1.1, and keep stirring for one hour. Co 2+ ≥100g / l, Fe 3+ ≤0.5ug / ml, Cu 2+ ≤0.5ug / ml, Al 3+ ≤0.5ug / ml, Mg 2+ The high-purity cobalt chloride solution of ≤5ug / ml can reach the battery grade standard, and the yield ...

Embodiment 2

[0045] Embodiment 2: Utilize cobalt carbonate residual product to produce high-purity cobalt chloride

[0046] Weigh the residual cobalt carbonate and add water to the stirred reactor for slurrying. And control the speed to add 175g / l hydrochloric acid solution to the final pH=1.

[0047] Add cobalt carbonate to the solution in step (1) to adjust the pH to 4.0, and press filter to obtain a cobalt chloride solution.

[0048] Put the above cobalt chloride solution into a heated and stirred reactor, raise the temperature to 80°C, and slowly add 40g / l sodium hydroxide solution to adjust the pH to 4.7 under the condition of sufficient stirring.

[0049] When the pH is completely stable above 4.5, slowly add ammonium fluoride with an excess coefficient of 1.2, and keep stirring for one and a half hours. After filtering to get Co 2+ ≥100g / l, Fe 3+ ≤0.5ug / ml, Cu 2+ ≤0.5ug / ml, Al 3+ ≤0.5ug / ml, Mg 2+ The high-purity cobalt chloride solution of ≤5ug / ml can reach the battery grade ...

Embodiment 3

[0050] Embodiment 3: Utilize cobalt carbonate residual product to produce high-purity cobalt chloride

[0051] Weigh the residual cobalt carbonate and add water to the stirred reactor for slurrying. And control the speed to add 190g / l hydrochloric acid solution to the final pH=2.

[0052] Add cobalt carbonate to the solution in step (1) to adjust the pH to 3.0, and obtain a cobalt chloride solution after pressure filtration.

[0053]Pour the above cobalt chloride solution into a heated and stirred reactor, raise the temperature to 90°C, and slowly add 40g / l sodium hydroxide solution to adjust the pH to 5 under the condition of sufficient stirring.

[0054] When the pH is completely stable above 4.5, slowly add ammonium fluoride with an excess coefficient of 1.5, and keep stirring for two hours. After filtering to get Co 2+ ≥100g / l, Fe 3+ ≤0.5ug / ml, Cu 2+ ≤0.5ug / ml, Al 3+ ≤0.5ug / ml, Mg 2+ The high-purity cobalt chloride solution of ≤5ug / ml can reach the battery grade sta...

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PUM

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Abstract

The invention discloses a method for producing high-purity cobalt chloride by utilizing cobalt carbonate defective products. The method comprises the following steps: adding defective cobalt carbonateand water into a reaction kettle and pulping; then adding acid to regulate the pH (Potential of Hydrogen) to sufficiently dissolve the cobalt carbonate; then adding the cobalt carbonate to inverselyregulate the pH; after carrying out filter pressing, obtaining a first cobalt chloride solution; adding the cobalt chloride solution into the reaction kettle capable of being heated and being stirredand improving the temperature to 80 to 90 DEG C; under the condition of sufficiently stirring, slowly adding a sodium hydroxide solution to adjust the pH to ensure that the solution contains enough hydroxyl ions and aluminum ions are sufficiently hydrolyzed; when the pH is completely stable, slowly adding an excessive amount of ammonium fluoride to ensure that magnesium ion sediment is completelyremoved; carrying out heat insulation and stirring; after filtrating, obtaining a high-purity cobalt chloride solution. The method disclosed by the invention has a simple technology and low productioncost; the recovery rate of cobalt reaches 99 percent or more and reaches battery-grade standards.

Description

technical field [0001] The invention relates to the technical field of recycling waste battery materials, in particular to a method for producing high-purity cobalt chloride by using defective cobalt carbonate products. Background technique [0002] Lithium-ion battery is a rechargeable battery with good electrochemical performance, high energy, safety and pollution-free. Its development speed is extremely fast and it has been widely used in all walks of life. Valuable metal recycling has also received great attention. [0003] At present, in the production process of lithium cobalt oxide cathode materials, the precursors are commonly mixed according to different models. For the unqualified materials caused by physical factors such as morphology and particle size in the production process, no other substances are introduced except for the doping elements. Impurities, but this type of waste has not been effectively separated according to different types of impurities during ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/08
CPCC01G51/085C01P2006/80
Inventor 张伟刘华旭祝小明
Owner XIAMEN TUNGSTEN
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