Preparation method of small-particle size spherical cobalt carbonate

A technology of cobalt carbonate and small particle size, applied in the direction of cobalt carbonate, etc., can solve the problem of small particle size spherical cobalt carbonate not forming a sphere, etc., and achieve the effect of easy promotion and low process cost.

Active Publication Date: 2017-05-10
JINGMEN GEM NEW MATERIAL
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  • Abstract
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  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a method for preparing spherical cobalt carbonate with small particle size, which solves the problem of non-balling of spherical cobalt carbonate with small particle size prepared by existing methods under mild and industrializable conditions by controlling the pH value in the process

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  • Preparation method of small-particle size spherical cobalt carbonate
  • Preparation method of small-particle size spherical cobalt carbonate
  • Preparation method of small-particle size spherical cobalt carbonate

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[0026] The embodiment of the present invention provides a method for preparing spherical cobalt carbonate with small particle size, which specifically includes the following steps:

[0027] Step 1, cobalt salt and ammonium bicarbonate solution are added to the reactor to react, and the pH value of the reaction process is controlled so that the pH value of the system is adjusted to 7.0 ± 0.1 after half an hour; the cobalt salt is cobalt chloride, cobalt sulfate, acetic acid A kind of cobalt, the concentration of cobalt salt is 60-160g / l, the flow rate is 1-5L / h; adjust according to the flow rate of ammonium bicarbonate; the concentration of ammonium bicarbonate is 120-240g / l;

[0028] Step 2, continue to add cobalt salt and ammonium bicarbonate solution in parallel, keep the pH value of step 1 unchanged, and precipitate after 2 hours of reaction; the reaction temperature is 35-65°C, and the stirring rate is 50-220r / min;

[0029] Step 3, performing solid-liquid separation and dr...

Embodiment 1

[0032] Concentration is the cobalt chloride of 120g / l and the ammonium bicarbonate mixing reaction that concentration is 220g / l, and wherein the flow of cobalt chloride is 2.5L / h, and the flow of regulating ammonium bicarbonate in the reaction process makes the mixed solution after half an hour The pH value is 7.015, keep the pH value unchanged and continue to show, stir at 40°C at a speed of 150r / min, react for 2 hours and then precipitate, then separate the solid-liquid and dry the precipitated solution to obtain a small particle size Spherical cobalt carbonate, such as figure 1 and figure 2 shown. Among them, the laser particle size analyzer test D 10 18.572 μm, D 50 34.967μm, D 90 It is 50.655μm, and the size of the secondary particle electron microscope is between 3-5μm, which may be caused by the agglomeration of small spherical particles during the laser particle size test.

Embodiment 2

[0034] Mix the cobalt chloride with a concentration of 60g / l and the ammonium bicarbonate with a concentration of 120g / l, wherein the flow rate of cobalt chloride is 1L / h, adjust the flow rate of ammonium bicarbonate during the reaction so that the pH value of the mixed solution after half an hour It is 7.002, keep the pH value unchanged and continue the reaction, stir at 35°C at a speed of 220r / min, precipitate after 2 hours of reaction, and then separate solid-liquid and dry the precipitated solution to obtain spherical carbonic acid with small particle size Cobalt, such as image 3 and Figure 4 shown. Among them, the laser particle size analyzer test D 10 9.582 μm, D 50 23.616 μm, D 90 It is 44.681μm, and the size of the secondary particle electron microscope is between 3-5μm, which may be caused by the agglomeration of small spherical particles during the laser particle size test.

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Abstract

The invention discloses a preparation method of small-particle size spherical cobalt carbonate. The preparation method comprises the following specific steps: 1, converging cobalt salt and an ammonium bicarbonate solution, adding into a reaction kettle for reacting, controlling the pH value in the reaction process so as to adjust the pH value of a system after half an hour to 7.0+/-0.1; 2, further converging and adding the cobalt salt and an ammonium bicarbonate solution, keeping the pH in the step 1, continuing reacting for 2h, and precipitating; 3, performing solid-liquid separation and drying the solution after precipitation in the step 2 to obtain the small-particle size spherical cobalt carbonate. By the preparation method, through process control over the pH value, nucleation among cobalt carbonate particles and the uniformity of a growth condition are maintained, so that the isotropy of precipitates and the solution are achieved, and thus on the basis of the nucleation, the spherical cobalt carbonate is formed through outward, uniform and spherical growth. In addition, the preparation method is low in process cost and easy to popularize.

Description

technical field [0001] The invention belongs to the technical field of metal powder material preparation technology, and in particular relates to a preparation method of small-diameter spherical cobalt carbonate. Background technique [0002] As an important chemical raw material and material precursor, cobalt carbonate is widely used in colorants in the ceramic industry, beneficiation agents in the mining industry, catalysts in the organic industry, hard alloys, and battery material precursors. In terms of material application, such as cobalt powder precursors for cemented carbide and cobalt tetroxide precursors, there are requirements for the particle size, morphology and various physical indicators of cobalt carbonate. The development trend in both fields is a big one under spherical conditions. Two types of particles with a small particle size correspond to the precursors of spherical large particles of about 20 microns and spherical small particles of 2-5 microns. No, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/06
CPCC01G51/06C01P2004/03C01P2004/32C01P2004/61
Inventor 郭苗苗许开华张云河刘文泽
Owner JINGMEN GEM NEW MATERIAL
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