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A kind of preparation method of high-purity ultrafine spherical cobalt carbonate

A cobalt carbonate and spherical technology, which is applied in the field of preparation of high-purity ultrafine spherical cobalt carbonate, can solve the problems that it is difficult to produce ultrafine spherical cobalt carbonate, increase particle and particle agglomeration, and uneven distribution of product particles, so as to avoid local concentration The effects of excessively high, reduced dosage, and simple and easy-to-control production methods

Active Publication Date: 2015-08-05
YUCHEN ADVANCED ENERGY MATERIALS & TECH WUXI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional production of cobalt carbonate adopts a batch-type discontinuous production process. The precipitant is directly added to the cobalt-containing solution for precipitation reaction. The chance of agglomeration between particles, and the phenomenon of peritectic and alkali-coated segregation will eventually result in uneven particle size distribution and various shapes (dendritic, flake, rod, etc.), which are not conducive to product stability.
The traditional process requires complex processes such as washing, centrifugal filtration, sediment drying, crushing, and screening, and the control of flow, temperature difference, and pH value is unstable and inaccurate, resulting in uneven distribution of product particles and poor consistency, which is not conducive to product quality. stable, it is difficult to produce ultrafine spherical cobalt carbonate
Basic cobalt carbonate prepared in the patent "spherical agglomerated basic cobalt (II) carbonate (II) and cobalt hydroxide (II) and its production method and application" published in 1998 by German Stark company (patent number: 96195592) The sphericity is higher, but cobalt carbonate is a spherical particle formed by the aggregation of fine particles, not a real spherical cobalt carbonate; mentioned in the domestic patent "spherical cobalt carbonate production method" (patent number: 200810143011.X) Preparation method, although the physical appearance and physical indicators of the prepared cobalt carbonate are acceptable, but the reaction temperature is low in the preparation process, and involves aging growth time of up to 18 hours, which is not conducive to the improvement of production efficiency

Method used

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  • A kind of preparation method of high-purity ultrafine spherical cobalt carbonate
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  • A kind of preparation method of high-purity ultrafine spherical cobalt carbonate

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Effect test

Embodiment 1

[0037] (1) Take 100g of high-purity cobalt metal sheet as a raw material, dissolve and purify it with nitric acid, then extract and remove impurities with p204 and p507 solutions to obtain a cobalt nitrate solution with a concentration of 100g / L; add 10g of ammonia water to the above cobalt nitrate solution The complexing agent is stirred and fully mixed to obtain a complexed cobalt salt solution; the pH value of the above-mentioned complexed cobalt salt solution is adjusted to 4.0 with nitric acid solution;

[0038] (2) Take 50g of ammonium carbonate and 50g of urea. Prepare a precipitant solution with a concentration of 100g / L; add 0.05g of dispersant PVP to the above precipitant solution, dissolve and stir evenly;

[0039] (3) Take 0.5L of the above-mentioned complexed cobalt salt solution and 0.75L of the precipitating agent solution, and add them to the reactor by the co-current feeding method according to the volume ratio of 1:1.5. 7.9, the stirring speed is 120rpm;

...

Embodiment 2

[0042] (1) Take 100g of high-purity cobalt metal sheet as raw material, dissolve and purify it with hydrochloric acid, then extract and remove impurities with p204 and p507 solutions to obtain a cobalt chloride solution with a concentration of 150g / L; add 0.5g complexing agent citric acid is prepared complexed cobalt salt solution, stirs and fully mixes, and the pH value of complexed cobalt salt solution is adjusted to 2.0 with hydrochloric acid;

[0043] (2) Take 150g of ammonium bicarbonate and 50g of urea to prepare a precipitant solution with a concentration of 200g / L;

[0044] Add 20g of dispersant ethanol to the above precipitant solution, dissolve and stir evenly;

[0045] (3) Take 0.1L of the above-mentioned complexed cobalt salt solution and 0.35L of the precipitating agent solution, and add them to the reactor with the co-current feeding method according to the volume ratio of 1:3.5, and control the synthesis reaction temperature to 50°C, and the reaction pH to be 8....

Embodiment 3

[0048] (1) Take 100g of high-purity cobalt metal sheet as a raw material, dissolve and purify it with nitric acid, then extract and remove impurities with p204 and p507 solutions to obtain a cobalt nitrate solution with a concentration of 60g / L; add 2.5g of cobalt nitrate to the above cobalt nitrate solution Polyacrylamide complexing agent and 2.5g ethylenediamine complexing agent, generate complexed cobalt salt solution, stir and fully mix; Regulate complexed cobalt salt solution pH value 2.0 with hydrochloric acid;

[0049] (2) Take 50g of ammonium bicarbonate and 50g of urea to prepare a precipitant solution with a concentration of 100g / L;

[0050] Add 0.1g dispersant PAA, 0.1g dispersant butanol and 0.1g dispersant acetone to the precipitant solution, stir and mix evenly;

[0051] (3) Take 0.1L of the above-mentioned complexed cobalt salt solution and 0.5L of the precipitating agent solution, and add them to the reactor by the co-current feeding method according to the volum...

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Abstract

The invention discloses a preparation method of high-purity superfine spherical cobalt carbonate, and belongs to the field of preparation of metal powder materials. The preparation method is as follows: metal cobalt is used as a raw material to prepare a cobalt salt solution, a complexing agent is used for prepare a complexed cobalt salt solution from the cobalt salt solution, a mixture of an ammonium salt and urea is prepared in to a precipitant solution, a dispersant is added into the precipitant solution, the complexed cobalt salt solution and the precipitant are added agent according to a certain volume ratio by a parallel flow feeding method into a reactor for reaction, the reaction temperature is controlled at 50-80 DEG C, the pH value is controlled to 7.8-8.3, and the stirring speed is 60-200rpm, and finally the superfine spherical cobalt carbonate is obtained by washing, filtering and drying of prepared cobalt carbonate. The preparation method has the advantages of simple production process, easy control, short production cycle, high efficiency and continuous production, a prepared cobalt carbonate product has the advantages of good mobility, uniform particle size distribution, spherical microtopography, high chemical purity and good chemical properties.

Description

technical field [0001] The invention belongs to the field of metal powder material preparation, and in particular relates to a preparation method of high-purity ultrafine spherical cobalt carbonate. Background technique [0002] In the field of diamond tools and hard alloy materials, the quality of cobalt powder has a great influence on the performance of the alloy. In order to meet the requirements of high-end hard alloy and cobalt powder for diamond tools, high-quality ultra-fine cobalt powder is being paid more and more attention. The method of preparing cobalt powder with cobalt oxalate has been reported, but due to the genetic characteristics of cobalt oxalate raw material, the cobalt powder prepared with cobalt oxalate has a coarse powder particle size, and the powder shape is mostly poor dendritic or needle-like, and the shape The appearance is difficult to control, so its application is limited. Further improving the particle size and shape of cobalt powder, produci...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G51/06
Inventor 何爱山
Owner YUCHEN ADVANCED ENERGY MATERIALS & TECH WUXI
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