CN103028735A - Preparation method of semi-micrometer cobalt powder - Google Patents
Preparation method of semi-micrometer cobalt powder Download PDFInfo
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- CN103028735A CN103028735A CN2011102967928A CN201110296792A CN103028735A CN 103028735 A CN103028735 A CN 103028735A CN 2011102967928 A CN2011102967928 A CN 2011102967928A CN 201110296792 A CN201110296792 A CN 201110296792A CN 103028735 A CN103028735 A CN 103028735A
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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
The present patent application relates to a kind of preparation method of half micron cobalt powder, belongs to the metal powder material preparing technical field.
Background technology
Cobalt powder is the irregular powder of grey, be dissolved in acid, be magnetic, easily oxidation in humid air, as metallurgic products such as carbide alloy, diamond tool, high temperature alloy, magnetic materials, and the chemicals such as chargeable battery, industrial blasting agent, rocket fuel and medicine.During general industry was used, common cobalt powder was divided into standard type cobalt powder, near-spherical cobalt powder and ultra-fine near-spherical cobalt powder.
Super-fine cobalt powder has special physical and chemical performance, have great skin effect and bulk effect, development along with science and technology, different applications improves constantly the requirement of dusty material performance, in the preparation such as ultra-fine cemented carbide, require the cobalt powder Fisher particle size less than 0.8 um, just can obtain better serviceability.The preparation method of super-fine cobalt powder is a lot, common are gas phase reduction process, hydrothermal reduction method, liquid phase reduction etc., but exists the shortcomings such as equipment requirement is higher, cost is higher, product purity is not high.Disclose a kind of process of producing spherical submicron metal with hydro-thermal treatment such as Chinese patent CN101428348A, the cobalt powder purity of its preparation can only reach 2N5(namely 99.5%), and need under HTHP, react, higher to equipment requirement; Chinese patent CN101100001A discloses a kind of super-fine cobalt powder and manufacturing process thereof, need to be in high energy ball mill ball milling 20～50 hours, production efficiency is low, energy consumption is large; Chinese patent CN101780545A discloses low-oxygen content submicron cobalt powder and cobalt oxalate presoma and manufacture method, and its reaction process is gentle, and cobalt oxalate presoma particle diameter is thin and even, but exists the difficulty of filtration, washing.
Summary of the invention
The present patent application namely is the above-mentioned shortcoming that exists in the super-fine cobalt powder preparation at present, and a kind of with low cost, method simple practical is provided, and the high preparation method of product purity.
The present patent application adopts cobalt chloride and carbonic hydroammonium reaction to produce the cobalt carbonate precipitation, then react with oxalic acid solution, directly use Frequency Conversion Technique of Centrifugal Spraying Drying Equipment dry broken product behind the reaction terminating, airflow crash, it is carefully even to obtain particle diameter, granule-morphology is class spherical cobalt oxalate and cobalt carbonate mixing precursor powder, precursor powder is in superfines hydrogen reduction furnace reduction, after reduction is come out of the stove, in nitrogen or carbon dioxide atmosphere, preserved 12～24 hours, broken in the nitrogen atmosphere downstream, and adding paraffin, the oleic acid parcel prevents the cobalt powder oxidation, is convenient to store and use.
Specifically, the present patent application provides a kind of preparation method of half micron cobalt powder, and described method comprises following step:
1) cobalt chloride and carbonic hydroammonium or ammonium carbonate, sodium carbonate are reacted 30～50 ℃ of reaction temperatures, pH value 6.5～7.2;
2) solution that obtains after will reacting filters, and obtains the cobalt carbonate precipitation, then washs and pulp with 70～90 ℃ pure water;
3) with concentration be the oxalic acid solution of 100～300 g/L, add in the above-mentioned cobalt carbonate slurry by the flow of 20～100 L/min and to react, mixing speed 100～800 r/min, 0～40 ℃ of reaction temperature, after oxalic acid solution adds, reacted 1～5 hour, and after pH value reaches 6～7, filtered or centrifugal spray drying;
4) behind the above-mentioned dry materials, adopt airflow crash, obtain the cobalt precursor powder that cobalt oxalate and cobalt carbonate mix;
5) above-mentioned cobalt precursor powder is reduced in hydrogen reduction furnace, in nitrogen or carbon dioxide atmosphere, preserve after reduction is come out of the stove and carried out passivation in 12～24 hours, the super-fine cobalt powder surface energy is discharged fully, improve its oxidation resistance, then through airflow crash, add paraffin or oleic acid parcel, vacuum packet is dressed up product.
Further, in above-mentioned step 1, the concentration of cobalt chloride is 80～120 g/l, and the concentration of carbonic hydroammonium or ammonium carbonate, sodium carbonate is 150～250 g/l.
Preferably, in above-mentioned step 3, the temperature that oxalic acid solution and cobalt carbonate slurry react is 15～30 ℃.
Further, in above-mentioned step 3, the mol ratio of described cobalt carbonate and oxalic acid is 1:0.1～0.99.
Preferably, in above-mentioned step 3, described oxalic acid adopts technical grade or food-grade oxalic acid, dissolves with pure water.
The cobalt precursor powder that in above-mentioned steps 4, obtains, wherein, the D50 particle diameter is 0.6～1.5 um, and FSSS particle diameter (being Fisher particle size) is 0.5～0.8 um, and particle diameter is about half micron, and apparent density is 0.15～0.25 g/cm
3, cobalt content is 32～45% wt.
Further, in above-mentioned steps 5, the temperature that the cobalt precursor powder reduces in hydrogen reduction furnace is at 360～450 ℃, and the recovery time is 2～10 hours.
In above-mentioned steps 5, described hydrogen reduction furnace is conventional cobalt powder tubular electric resistance reduction furnace, its bringing-up section and cooling section Length Ratio are 1:1～2, strengthen its cooling effect, its cooling section has 2 above gas feeds at least simultaneously, can lead to the gases such as nitrogen or carbon dioxide, be adsorbed on the cobalt powder surface, improve the cobalt powder oxidation resistance.
By half micron cobalt powder that said method obtains, its Fei Shi particle diameter is 0.4～0.8 um, oxygen content 0.4～0.8%, and carbon content 0.01～0.05% is shaped as the class sphere.
The described method of the present patent application has following characteristics and advantage:
1. the described method of the present patent application is at room temperature reacted, and is easy to suitability for industrialized production;
2. this thinking adopts cobalt carbonate to wash in advance, and the pure oxalic acid of top grade is raw material, guarantees under the prerequisite of product purity, has saved the washing of cobalt oxalate mix products and dehydration procedure, has solved the difficult problem that the cobalt oxalate mixture filters and washs;
3. the described method of the present patent application adopts centrifugal spray or expansion drying mode, has improved the dispersiveness of powder;
4. processing is cooled off, wrapped up to the described method of the present patent application under nitrogen atmosphere, improves the antioxygenic property of cobalt powder.
Description of drawings
Fig. 1 is the preparation method's of the described half micron cobalt powder of the present patent application FB(flow block);
Fig. 2 is the scanning electron microscope (SEM) photograph that the present patent application embodiment three produces cobalt powder.
The specific embodiment
Preparation method to the described half micron cobalt powder of the present patent application is described below in conjunction with accompanying drawing and concrete example; purpose is better to understand the technology contents of the present patent application for the public; rather than to the restriction of described technology contents; in fact; in the principle identical or approximate with the present patent application, the change that processing step, condition, related reagent in the described method are carried out, or replace; reach identical purpose or effect, all within the present patent application technical scheme required for protection.
Embodiment one
React as example take cobalt chloride and carbonic hydroammonium, describe, described method comprises the steps:
1. with concentration be the cobalt chloride of 80 g/L and carbonic hydroammonium that concentration is 150 g/L 45 ℃ of temperature, react under the condition of pH value 6.5;
2. the solution that will obtain after will reacting filters, and obtains cobalt carbonate precipitation, then washs and pulp with 70 ℃ pure water;
3. technical grade oxalic acid is dissolved with pure water, obtain the oxalic acid solution that concentration is 100 g/L, add in the above-mentioned cobalt carbonate slurry by the flow of 20 L/min and to react, the mol ratio of described cobalt carbonate and oxalic acid is 1:0.5, mixing speed 400 r/min, 20 ℃ of reaction temperatures, after oxalic acid solution adds, reacted 1 hour, and after pH value reaches 6～7, filtered;
4. behind the above-mentioned dry materials, adopt airflow crash, obtain the cobalt precursor powder that cobalt oxalate and cobalt carbonate mix;
5. above-mentioned cobalt precursor powder is reduced in hydrogen reduction furnace, temperature is 360 ℃, recovery time is 4 hours, in nitrogen atmosphere, preserve after reduction is come out of the stove and carried out passivation in 12 hours, the super-fine cobalt powder surface energy is discharged fully, improve its oxidation resistance, then through airflow crash, add the paraffin parcel, vacuum packet is dressed up product.
Embodiment two
React as example take cobalt chloride and ammonium carbonate, describe, described method comprises the steps:
1. the cobalt chloride and the 250 g/L ammonium carbonates that with concentration are 120 g/L react 50 ℃ of reaction temperatures, pH value 7.2;
2. the solution that will obtain after will reacting filters, and obtains cobalt carbonate precipitation, then washs and pulp with 90 ℃ pure water;
3. food-grade oxalic acid is carried out the oxalic acid solution that concentration of ordinary dissolution is 300 g/L with pure water, the mol ratio of described cobalt carbonate and oxalic acid is 1:0.99, add in the above-mentioned cobalt carbonate slurry by the flow of 100 L/min and to react, mixing speed 800 r/min, 40 ℃ of reaction temperatures after oxalic acid solution adds, were reacted 5 hours, after pH value reaches 6～7, carry out centrifugal spray drying;
4. behind the above-mentioned dry materials, adopt airflow crash, obtain the cobalt precursor powder that cobalt oxalate and cobalt carbonate mix;
5. above-mentioned cobalt precursor powder is reduced in hydrogen reduction furnace, the temperature of reduction is 450 ℃, recovery time is 10 hours, in nitrogen or carbon dioxide atmosphere, preserve after reduction is come out of the stove and carried out passivation in 24 hours, the super-fine cobalt powder surface energy is discharged fully, improve its oxidation resistance, then through airflow crash, add oleic acid and wrap up, vacuum packet is dressed up product.
?
Embodiment three
React as example take cobalt chloride and sodium carbonate, describe, described method comprises the steps:
1. be that the cobalt chloride of 100 g/L and sodium carbonate that concentration is 200 g/L react 40 ℃ of reaction temperatures, pH value 6.8 with concentration;
2. the solution that will obtain after will reacting filters, and obtains cobalt carbonate precipitation, then washs and pulp with 80 ℃ pure water;
3. technical grade oxalic acid is carried out the oxalic acid solution that concentration of ordinary dissolution is 200 g/L with pure water, the mol ratio of described cobalt carbonate and oxalic acid is 1:0.7, add in the above-mentioned cobalt carbonate slurry by the flow of 60 L/min and to react, mixing speed 700 r/min, 15 ℃ of reaction temperatures after oxalic acid solution adds, were reacted 3 hours, after pH value reaches 6～7, filter;
4. behind the above-mentioned dry materials, adopt airflow crash, obtain the cobalt precursor powder that cobalt oxalate and cobalt carbonate mix;
5. above-mentioned cobalt precursor powder is reduced in hydrogen reduction furnace, the temperature of reduction is 400 ℃, recovery time is 7 hours, in nitrogen, preserve after reduction is come out of the stove and carried out passivation in 18 hours, the super-fine cobalt powder surface energy is discharged fully, improve its oxidation resistance, then through airflow crash, add the paraffin parcel, vacuum packet is dressed up product.
Embodiment four
React as example take cobalt chloride and sodium carbonate, describe, described method comprises the steps:
1. be that the cobalt chloride of 90 g/L and sodium carbonate that concentration is 180 g/L react 35 ℃ of reaction temperatures, pH value 7.0 with concentration;
2. the solution that will obtain after will reacting filters, and obtains cobalt carbonate precipitation, then washs and pulp with 75 ℃ pure water;
3. food-grade oxalic acid is carried out the oxalic acid solution that concentration of ordinary dissolution is 160 g/L with pure water, the mol ratio of cobalt carbonate and oxalic acid is 1:0.30, add in the above-mentioned cobalt carbonate slurry by the flow of 80 L/min and to react, mixing speed 600 r/min, 30 ℃ of reaction temperatures after oxalic acid solution adds, were reacted 4 hours, after pH value reaches 6～7, filter or centrifugal spray drying;
4. behind the above-mentioned dry materials, adopt airflow crash, obtain the cobalt precursor powder that cobalt oxalate and cobalt carbonate mix;
5. above-mentioned cobalt precursor powder is reduced in hydrogen reduction furnace, the temperature of reduction is at 380 ℃, recovery time is 7 hours, in nitrogen or carbon dioxide atmosphere, preserve after reduction is come out of the stove and carried out passivation in 16 hours, the super-fine cobalt powder surface energy is discharged fully, improve its oxidation resistance, then through airflow crash, add the oleic acid parcel, vacuum packet is dressed up product.
The half micron cobalt powder that obtains by said method, its Fei Shi particle diameter is 0.4～0.8 um, oxygen content 0.4～0.8 %, carbon content 0.01～0.05 %, be shaped as the class sphere, have the advantage of super-fine cobalt powder and class ball cobalt powder concurrently, fine size, narrowly distributing, particle diameter is little and even, is widely used in hart metal product and the battery industries such as digital cuttings, bar, top hammer, drill bit.
Claims (9)
1. the preparation method of one and half microns cobalt powders, it is characterized in that: described method comprises following step:
1) cobalt chloride and carbonic hydroammonium or ammonium carbonate, sodium carbonate are reacted 30～50 ℃ of reaction temperatures, pH value 6.5～7.2;
2) solution that obtains after will reacting filters, and obtains the cobalt carbonate precipitation, then washs and pulp with 70～90 ℃ pure water;
3) with concentration be the oxalic acid solution of 100～300 g/L, add in the above-mentioned cobalt carbonate slurry by the flow of 20～100 L/min and to react, mixing speed 100～800 r/min, 0～40 ℃ of reaction temperature, after oxalic acid solution adds, reacted 1～5 hour, and after pH value reaches 6～7, filtered or centrifugal spray drying;
4) behind the above-mentioned dry materials, adopt airflow crash, obtain the cobalt precursor powder that cobalt oxalate and cobalt carbonate mix;
5) above-mentioned cobalt precursor powder is reduced in hydrogen reduction furnace, in nitrogen or carbon dioxide atmosphere, preserve after reduction is come out of the stove and carried out passivation in 12～24 hours, the super-fine cobalt powder surface energy is discharged fully, improve its oxidation resistance, then through airflow crash, add paraffin or oleic acid parcel, vacuum packet is dressed up product.
2. preparation method according to claim 1, it is characterized in that: in above-mentioned step 1), the concentration of cobalt chloride is 80～120 g/L, and the concentration of carbonic hydroammonium or ammonium carbonate, sodium carbonate is 150～250 g/L.
3. preparation method according to claim 1, it is characterized in that: in above-mentioned step 3), the temperature that oxalic acid solution and cobalt carbonate slurry react is 15～30 ℃.
4. preparation method according to claim 1, it is characterized in that: in above-mentioned step 3), the mol ratio of described cobalt carbonate and oxalic acid is 1:0.1～0.99.
5. preparation method according to claim 1 is characterized in that: in above-mentioned step 3), described oxalic acid adopts technical grade or food-grade oxalic acid, dissolves with pure water.
6. preparation method according to claim 1 is characterized in that: in above-mentioned steps 4) in the cobalt precursor powder that obtains, wherein, the D50 particle diameter is 0.6～1.5 μ m, namely Fisher particle size is 0.5～0.8 μ m, apparent density is 0.15～0.25 g/cm
3, cobalt content is 32～45% wt.
7. preparation method according to claim 1 is characterized in that: in above-mentioned steps 5) in, the temperature that the cobalt precursor powder reduces in hydrogen reduction furnace is at 360～450 ℃, and the recovery time is 2～10 hours.
8. preparation method according to claim 1, it is characterized in that: in above-mentioned steps 5) in, described hydrogen reduction furnace is conventional cobalt powder tubular electric resistance reduction furnace, its bringing-up section and cooling section Length Ratio are 1:1～2, strengthen its cooling effect, its cooling section has 2 above gas feeds at least simultaneously, can lead to the gases such as nitrogen or carbon dioxide, be adsorbed on the cobalt powder surface, improve the cobalt powder oxidation resistance.
9. preparation method according to claim 1 is characterized in that: the cobalt powder that step 5) obtains, and its Fei Shi particle diameter is 0.4～0.8 um, oxygen content 0.4～0.8 %, carbon content 0.01～0.05 % is shaped as the class sphere.
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| CN103624251A (en) * | 2013-12-02 | 2014-03-12 | 深圳市格林美高新技术股份有限公司 | Half-micron cobalt powder, preparation method thereof, cobalt hydroxide powder and preparation method thereof |
| CN103736987A (en) * | 2013-12-25 | 2014-04-23 | 抚顺龙诚新科技材料有限公司 | Method for performing direct passivation on micro-fine metal powder on hydrogen reduction production line |
| CN104117686A (en) * | 2014-08-01 | 2014-10-29 | 宁波雁门新能源有限公司 | Cobalt powder preparation method |
| CN104722766A (en) * | 2013-12-18 | 2015-06-24 | 深圳市格林美高新技术股份有限公司 | High-density cobalt powder and synthetic method thereof |
| CN104722778A (en) * | 2013-12-19 | 2015-06-24 | 荆门市格林美新材料有限公司 | Method of synthesizing low-oxygen superfine cobalt powder |
| CN105798318A (en) * | 2014-12-29 | 2016-07-27 | 荆门市格林美新材料有限公司 | Cobalt powder and preparation method thereof, cobalt oxalate precursor and preparation method thereof |
| CN106270554A (en) * | 2016-09-28 | 2017-01-04 | 广州凯耀资产管理有限公司 | A kind of preparation method of super-fine cobalt powder |
| CN107570723A (en) * | 2017-08-10 | 2018-01-12 | 湖南工业大学 | Method for producing superfine cobalt powder for hard alloy by fluidized reduction of cobalt carbonate and production system thereof |
| CN109128218A (en) * | 2017-06-16 | 2019-01-04 | 荆门市格林美新材料有限公司 | A kind of preparation method of the cobalt powder of doped lanthanum |
| CN109128208A (en) * | 2017-06-16 | 2019-01-04 | 荆门市格林美新材料有限公司 | A kind of preparation method of the cobalt powder of adulterated al |
| CN109128209A (en) * | 2017-06-16 | 2019-01-04 | 荆门市格林美新材料有限公司 | A kind of preparation method of chromium-doped cobalt powder |
| CN109692969A (en) * | 2019-03-04 | 2019-04-30 | 江苏萌达新材料科技有限公司 | A kind of preparation method of hypoxemia superfine spherical cobalt powder |
| CN112371990A (en) * | 2020-10-22 | 2021-02-19 | 宁波互邦新材料有限公司 | Preparation process of ammoniation-free metal cobalt powder |
| CN112974833A (en) * | 2021-02-02 | 2021-06-18 | 安徽寒锐新材料有限公司 | Cobalt powder and preparation method and preparation device thereof |
| CN113909485A (en) * | 2021-10-11 | 2022-01-11 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
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| CN103624251A (en) * | 2013-12-02 | 2014-03-12 | 深圳市格林美高新技术股份有限公司 | Half-micron cobalt powder, preparation method thereof, cobalt hydroxide powder and preparation method thereof |
| CN103624251B (en) * | 2013-12-02 | 2015-09-16 | 格林美股份有限公司 | A kind of half micron cobalt powder and preparation method thereof and cobalt hydroxide powder and preparation method thereof |
| CN104722766A (en) * | 2013-12-18 | 2015-06-24 | 深圳市格林美高新技术股份有限公司 | High-density cobalt powder and synthetic method thereof |
| CN104722778B (en) * | 2013-12-19 | 2017-07-25 | 荆门市格林美新材料有限公司 | A kind of synthetic method of hypoxemia super-fine cobalt powder |
| CN104722778A (en) * | 2013-12-19 | 2015-06-24 | 荆门市格林美新材料有限公司 | Method of synthesizing low-oxygen superfine cobalt powder |
| CN103736987A (en) * | 2013-12-25 | 2014-04-23 | 抚顺龙诚新科技材料有限公司 | Method for performing direct passivation on micro-fine metal powder on hydrogen reduction production line |
| CN104117686A (en) * | 2014-08-01 | 2014-10-29 | 宁波雁门新能源有限公司 | Cobalt powder preparation method |
| CN105798318A (en) * | 2014-12-29 | 2016-07-27 | 荆门市格林美新材料有限公司 | Cobalt powder and preparation method thereof, cobalt oxalate precursor and preparation method thereof |
| CN106270554A (en) * | 2016-09-28 | 2017-01-04 | 广州凯耀资产管理有限公司 | A kind of preparation method of super-fine cobalt powder |
| CN109128218A (en) * | 2017-06-16 | 2019-01-04 | 荆门市格林美新材料有限公司 | A kind of preparation method of the cobalt powder of doped lanthanum |
| CN109128208A (en) * | 2017-06-16 | 2019-01-04 | 荆门市格林美新材料有限公司 | A kind of preparation method of the cobalt powder of adulterated al |
| CN109128209A (en) * | 2017-06-16 | 2019-01-04 | 荆门市格林美新材料有限公司 | A kind of preparation method of chromium-doped cobalt powder |
| CN107570723A (en) * | 2017-08-10 | 2018-01-12 | 湖南工业大学 | Method for producing superfine cobalt powder for hard alloy by fluidized reduction of cobalt carbonate and production system thereof |
| CN107570723B (en) * | 2017-08-10 | 2019-12-03 | 湖南工业大学 | Method for producing superfine cobalt powder for hard alloy by fluidized reduction of cobalt carbonate and production system thereof |
| CN109692969A (en) * | 2019-03-04 | 2019-04-30 | 江苏萌达新材料科技有限公司 | A kind of preparation method of hypoxemia superfine spherical cobalt powder |
| CN112371990A (en) * | 2020-10-22 | 2021-02-19 | 宁波互邦新材料有限公司 | Preparation process of ammoniation-free metal cobalt powder |
| CN112974833A (en) * | 2021-02-02 | 2021-06-18 | 安徽寒锐新材料有限公司 | Cobalt powder and preparation method and preparation device thereof |
| CN113909485A (en) * | 2021-10-11 | 2022-01-11 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
| CN113909485B (en) * | 2021-10-11 | 2023-11-17 | 先导薄膜材料（广东）有限公司 | Preparation method of superfine cobalt powder |
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