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Preparation method of semi-micrometer cobalt powder

A technology of cobalt powder and cobalt carbonate, which is applied in the field of preparation of half-micron cobalt powder, can solve the problems of difficult filtration and washing, high energy consumption and high cost, and achieve the effect of improving anti-oxidation performance and improving dispersibility

Active Publication Date: 2013-04-10
GEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are many preparation methods for ultra-fine cobalt powder, common ones are gas phase reduction method, hydrothermal reduction method, liquid phase reduction method, etc., but there are disadvantages such as high equipment requirements, high cost, and low product purity.
For example, Chinese patent CN101428348A discloses a process method for preparing spherical ultrafine metal powder by hydrothermal treatment. The cobalt powder prepared by it can only reach 2N5 (99.5%) in purity, and needs to be reacted under high temperature and high pressure, which requires high equipment requirements; Chinese patent CN101100001A discloses a superfine cobalt powder and its manufacturing process, which needs to be milled in a high-energy ball mill for 20 to 50 hours, with low production efficiency and high energy consumption; Chinese patent CN101780545A discloses low-oxygen submicron cobalt powder and its cobalt oxalate Precursor and manufacturing method, its reaction process is mild, the particle size of cobalt oxalate precursor is fine and uniform, but there are difficulties in filtration and washing

Method used

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Embodiment 1

[0029] Take cobalt chloride and ammonium bicarbonate reaction as example, illustrate, and described method comprises the following steps:

[0030] 1. React cobalt chloride with a concentration of 80 g / L and ammonium bicarbonate with a concentration of 150 g / L at a temperature of 45 °C and a pH value of 6.5;

[0031] 2. Filter the solution obtained after the reaction to obtain a precipitate of cobalt carbonate, which is then washed and slurried with pure water at 70 °C;

[0032] 3. Industrial grade oxalic acid is dissolved with pure water, and the oxalic acid solution that obtains concentration is 100 g / L, adds in the above-mentioned cobalt carbonate slurry by the flow rate of 20 L / min and reacts, and the mol ratio of described cobalt carbonate and oxalic acid is 1:0.5, stirring speed 400 r / min, reaction temperature 20 ℃, after adding the oxalic acid solution, react for 1 hour, and filter after the pH value reaches 6-7;

[0033] 4. After the above materials are dried, they are...

Embodiment 2

[0036] Take cobalt chloride and ammonium carbonate reaction as example, illustrate, and described method comprises the following steps:

[0037] 1. React cobalt chloride with a concentration of 120 g / L and 250 g / L ammonium carbonate at a reaction temperature of 50 °C and a pH value of 7.2;

[0038] 2. Filter the solution obtained after the reaction to obtain cobalt carbonate precipitate, and then wash and slurry with pure water at 90 °C;

[0039] 3. Dissolve food-grade oxalic acid in pure water into an oxalic acid solution with a concentration of 300 g / L, the molar ratio of cobalt carbonate to oxalic acid is 1:0.99, and add it into the above-mentioned cobalt carbonate slurry at a flow rate of 100 L / min. Reaction, the stirring speed is 800 r / min, the reaction temperature is 40 ℃, after adding the oxalic acid solution, react for 5 hours, and after the pH value reaches 6-7, carry out centrifugal spray drying;

[0040] 4. After the above materials are dried, they are crushed by a...

Embodiment 3

[0044] Take cobalt chloride and sodium carbonate reaction as example, illustrate, and described method comprises the following steps:

[0045] 1. React cobalt chloride with a concentration of 100 g / L and sodium carbonate with a concentration of 200 g / L, the reaction temperature is 40 °C, and the pH value is 6.8;

[0046] 2. Filter the solution obtained after the reaction to obtain cobalt carbonate precipitate, and then wash and slurry with 80 °C pure water;

[0047]3. Dissolve industrial-grade oxalic acid in pure water into an oxalic acid solution with a concentration of 200 g / L. The molar ratio of cobalt carbonate to oxalic acid is 1:0.7, and add it into the above-mentioned cobalt carbonate slurry at a flow rate of 60 L / min. Reaction, the stirring speed is 700 r / min, the reaction temperature is 15 ℃, after adding the oxalic acid solution, react for 3 hours, and filter after the pH value reaches 6-7;

[0048] 4. After the above materials are dried, they are crushed by air flo...

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Abstract

The invention provides a preparation method of semi-micrometer cobalt powder. The preparation method of the semi-micrometer cobalt powder is low in cost and simple and practical, and products by means of the preparation method are high in purity. The preparation method includes that cobalt carbonate sediments are produced through reaction of cobalt chloride and ammonium hydrogen carbonate, reaction of the cobalt carbonate sediments and oxalate solution is carried out, when the reaction is stopped, reaction products are directly crushed through drying and air flow by centrifugal spray drying equipment, and therefore precursor powder which is fine and even in particle size and sphere-like in particle shape and mixed by oxalate cobalt and cobalt carbonate. The precursor powder is reduced in a superfine powder hydrogen reduction furnace and then comes out of the furnace after reduction, and then the precursor powder is kept in nitrogen or carbon dioxide for 12-24 hours for passivating treatment. Afterwards, the precursor powder is crushed by the air flow, paraffin wax and oleic acid are added in the precursor powder, the precursor powder is packaged so as to prevent cobalt powder from oxidation, and finally superfine cobalt powder is obtained by vacuum package. The semi-micrometer cobalt powder obtained by means of the preparation method has the advantages of superfine cobalt powder and sphere-like cobalt powder, is fine in particle size, narrow in distribution, small and even in partical size and can be widely used in battery industries and hard alloy products like numerical blades, bar materials, holding-up hammers and drills.

Description

technical field [0001] The application of the present invention relates to a method for preparing half-micron cobalt powder, which belongs to the technical field of metal powder material preparation. Background technique [0002] Cobalt powder is gray irregular powder, soluble in acid, magnetic, easy to oxidize in humid air, used as metallurgical products such as cemented carbide, diamond tools, superalloys, magnetic materials, and rechargeable batteries, industrial blasting agents, Chemicals such as rocket fuel and medicine. In general industrial applications, common cobalt powder is divided into standard cobalt powder, spherical cobalt powder and ultrafine spherical cobalt powder. [0003] Ultrafine cobalt powder has special physical and chemical properties, and has great surface effect and volume effect. With the development of science and technology, the requirements for powder material performance in different application fields are constantly increasing, such as in th...

Claims

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Application Information

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IPC IPC(8): B22F9/22B22F1/00
Inventor 苏陶贵何显达杨柳郭苗苗周继锋王勤
Owner GEM CO LTD
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