Preparation method for ultrapure ultrafine cobalt carbonate

A technology of cobalt carbonate and carbonate, applied in directions such as cobalt carbonate, can solve the problems of high processing cost, difficult to wash, difficult to handle impurities, etc., and achieve the effect of simple process and low production cost

Inactive Publication Date: 2017-02-15
JINGMEN GEM NEW MATERIAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the small particle size and large specific surface area of ​​cobalt carbonate, it is difficult to filter, wash and dry after synthesis, so it is often difficult to balance the ultra-pure and ultra-fine properties of cobalt carbonate
For example, in the invention with the publication number CN103922426A, add ammonium bicarbonate with 4-6 times the amount of cobalt chloride to precipitate cobalt, wash after aging for 12 hours, and the Cl can only be guaranteed to be less than 500ppm; for example, the invention with the publication number CN102115214A prepares a D50 of about 5 μm cobalt carbonate, but this method adds a variety of surfactants and complexing agents, the impurities in the product are difficult to handle, and the follow-up processing cost is bound to be high; the publication number is CN102910686A In the invention, a low-temperature (0-30° C.) synthesis method is adopted , prepared cobalt carbonate with a D50 of 1.6-2.4 μm, but in this method, the interception effect of D50<1.5 μm particles is limited during micropore filtration, and the product yield is low, and it is difficult to effectively remove it by rinsing in micropores Cl ion

Method used

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  • Preparation method for ultrapure ultrafine cobalt carbonate
  • Preparation method for ultrapure ultrafine cobalt carbonate
  • Preparation method for ultrapure ultrafine cobalt carbonate

Examples

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preparation example Construction

[0066] Please refer to figure 1 , figure 1 It is a schematic flow sheet of an ultra-pure ultra-fine cobalt carbonate preparation method in an embodiment of the present invention, comprising the following steps:

[0067] S01. Add the reaction bottom liquid in the reaction kettle, add the carbonate solution or bicarbonate solution and the cobalt salt solution to the reaction bottom liquid, and react under stirring conditions, the carbonate or bicarbonate and the cobalt salt The molar ratio of cobalt ions is 3.0-6.0:1, the pH of the reaction system is 6.8-8.2, the reaction temperature is 25-80°C, and the reaction time is 0.5-3h to obtain a slurry containing cobalt carbonate;

[0068] S02, performing solid-liquid separation on the slurry containing cobalt carbonate to obtain a filter cake, slurrying the filter cake to obtain a slurried material, washing the slurried material with water at a constant temperature, and performing solid-liquid separation after washing to obtain Coba...

Embodiment 1

[0074] A preparation method of ultrapure ultrafine cobalt carbonate, comprising the following steps:

[0075] (1), add the ammonium bicarbonate solution (reaction bottom liquid) that concentration is 40g / L to stirring paddle place in synthetic reactor, after raising reactor temperature to 35 ℃, start stirring paddle, control rotating speed is 250rpm, simultaneously Cobalt chloride solution and ammonium bicarbonate solution are added in parallel, wherein the flow rate of cobalt chloride solution is 400L / h, the pH is adjusted by the ammonium bicarbonate flow rate, the reaction pH is controlled between 6.8-7.8, and the reaction temperature is 35°C. Stop feeding after reacting 2h, obtain the slurry that contains cobalt carbonate; The mol ratio of cobalt ion in ammonium bicarbonate and cobalt chloride is 4.5:1;

[0076] (2) The slurry containing cobalt carbonate is transported to the plate and frame filter press for solid-liquid separation, and the pressure is 22Mpa to obtain mothe...

Embodiment 2

[0083] A preparation method of ultrapure ultrafine cobalt carbonate, comprising the following steps:

[0084] (1) Add pure water (reaction bottom liquid) to the stirring paddle in the synthesis reactor, raise the temperature of the reactor to 50°C, start the stirring paddle, control the speed at 500rpm, and simultaneously add cobalt chloride solution and carbonic acid Ammonium solution, wherein the flow rate of the cobalt chloride solution is 300L / h, the pH is adjusted by the ammonium carbonate flow rate, the reaction pH is controlled between 7.3-8.2, and the reaction temperature is 50°C. Stop feeding after reacting 1h, obtain the slurry that contains cobalt carbonate; The mol ratio of cobalt ion in ammonium carbonate and cobalt chloride is 6.0:1;

[0085] (2) The slurry containing cobalt carbonate is transported to the microporous filter for solid-liquid separation, the pressure is 0.2Mpa, mother liquor and filter cake are obtained, the mother liquor enters the recovery syste...

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Abstract

The invention provides a preparation method for ultrapure ultrafine cobalt carbonate. The preparation method comprises the following steps: (1) adding a base reaction solution into a reaction vessel, adding a carbonate solution or bicarbonate solution and a cobalt salt solution into the base reaction solution, and carrying out a reaction under stirring so as to obtain slurry containing cobalt carbonate, wherein a mol ratio of carbonate or bicarbonate to cobalt ions in the cobalt salt is (3.0-6.0): 1, the pH value of a reaction system is 6.8 to 8.2, reaction temperature is 25 to 80 DEG C and reaction time is 0.5 to 3 h; (2) subjecting the slurry containing cobalt carbonate to solid-liquid separation so as to obtain a filter cake, conveying the filter cake to a slurrying tank for slurrying so as to obtain a slurried material, conveying the slurried material to a washing tank for washing at a constant temperature and carrying out solid-liquid separation after completion of washing so as to obtain a cobalt carbonate precipitate; and (3) drying, crushing and sieving the cobalt carbonate precipitate so as to obtain ultrapure ultrafine cobalt carbonate. The preparation method provided by the invention is low in cost, simple in process flow and easy to operate.

Description

technical field [0001] The invention belongs to the technical field of metal particle preparation, and in particular relates to a method for preparing ultra-pure and ultra-fine cobalt carbonate. Background technique [0002] Cobalt carbonate is one of the precursors for preparing cobalt powder, and its physical and chemical properties directly affect the application of cobalt powder. In order to obtain cobalt powder with good performance, there are generally strict restrictions on the content of impurities in cobalt carbonate. For example, the requirements for the content of impurities in battery-grade cobalt carbonate are: Cl content is less than 0.01%, Na content is less than 0.01%, and Ca content is less than 0.01%. , Mg content is less than 0.01%, Fe content is less than 0.005%. However, due to the small particle size and large specific surface area of ​​cobalt carbonate, it is difficult to filter, wash and dry after synthesis, so it is often difficult to balance the ul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/06
Inventor 许开华张云河
Owner JINGMEN GEM NEW MATERIAL
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