CN113894287A - Preparation method of large FSSS spherical cobalt powder - Google Patents
Preparation method of large FSSS spherical cobalt powder Download PDFInfo
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- CN113894287A CN113894287A CN202111021008.2A CN202111021008A CN113894287A CN 113894287 A CN113894287 A CN 113894287A CN 202111021008 A CN202111021008 A CN 202111021008A CN 113894287 A CN113894287 A CN 113894287A
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
Abstract
The invention discloses a preparation method of large FSSS spherical cobalt powder, which comprises the following steps: the first step is as follows: preparing cobalt chloride solution and ammonium bicarbonate solution with different concentrations; the second step is that: synthesizing cobalt carbonate through a reaction kettle; the third step: washing the cobalt carbonate by a filter press, and controlling the concentration of chloride ions in the cobalt carbonate; the fourth step: directly drying wet cobalt carbonate by a flash evaporation machine; the fifth step: and reducing the screened dry material cobalt carbonate into cobalt powder at high temperature by a reducing furnace. The cobalt powder prepared by the method has the advantages of uniform particle size distribution, no sintering agglomeration, spherical shape and the like, and is easy to industrialize.
Description
Technical Field
The invention relates to the field of hard alloy materials, in particular to a preparation method of large FSSS spherical cobalt powder with uniformly distributed particles.
Background
At present, the cobalt powder is widely applied to the industrial fields of aviation, aerospace, electrical appliances, mechanical manufacturing and the like. Cobalt-based alloy or cobalt-containing alloy materials have good toughness and strong hardness, and are mostly applied to the fields of hard alloys and diamonds because cobalt is used as a good adhesive. Cobalt is also an important component of permanent magnetic alloys, an indispensable material in modern electronic and electromechanical industries, used to manufacture various components of acoustic, optical, electrical and magnetic devices.
The important precursor for preparing the cobalt powder by the prior art is mostly cobalt carbonate (1-2 μm) with small FSSS (Fischer-Tropsch type particle size), the cobalt carbonate (3-5 μm) for producing the large FSSS needs to continuously react for a longer time, the requirement on flow control precision is strict, traditional cobalt carbonate manufacturers mostly prepare the cobalt powder by a single reaction kettle, the cobalt powder does not have the requirement on continuous reaction, the requirement on input equipment is over high and is abandoned, and the cobalt powder with the large FSSS gradually becomes a high-end product along with the continuous development of the society, so the capability of producing the cobalt powder with the large FSSS needs to be improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of large FSSS spherical cobalt powder with uniformly distributed particles.
The invention is realized by the following technical scheme.
A preparation method of large FSSS spherical cobalt powder is characterized by comprising the following steps:
(1) preparing a cobalt chloride solution and an ammonium bicarbonate solution;
(2) adding the base solution into the reaction kettle, stirring, and controlling the pH value of the base solution to be 7.5-8.5;
(3) adding a cobalt chloride solution and an ammonium bicarbonate solution into a reaction kettle simultaneously to carry out a synthesis reaction, maintaining the pH of slurry in the reaction kettle to be 7.0-7.3, controlling the growth speed of seed crystals synthesized by the reaction to be 0.25-0.45 mu m increased every 8 hours, carrying out continuous crystallization reaction in the simultaneous feeding process, and stopping the reaction when the granularity D50 of particles generated by the reaction is 12.0-14.0 mu m, thus obtaining a cobalt carbonate finished product;
(4) washing, drying and screening the finished cobalt carbonate product to obtain a cobalt carbonate dry material;
(5) the cobalt carbonate dry material is calcined, reduced, crushed and screened, and then is packaged to obtain cobalt powder.
Furthermore, the concentration of cobalt ions in the cobalt chloride solution in the step (1) is 120g/L-180g/L, and the concentration of the ammonium bicarbonate solution is 200g/L-280 g/L.
Further, the base solution in the step (2) is prepared by adding pure water and an ammonium bicarbonate solution into a reaction kettle in sequence, wherein the concentration of ammonium bicarbonate in the base solution is 2g/L-10g/L, and the ratio of the volume of the added pure water to the volume of the reaction kettle is 0.5-1.5; the temperature of the base solution is 40-60 ℃, and the stirring speed in the reaction kettle is 150-300 r/min.
Further, the feeding flow rate of the cobalt chloride solution added into the reaction kettle in the step (3) is 500L/h-800L/h, and the feeding flow rate of the ammonium bicarbonate solution added into the reaction kettle is 1500L/h-2500L/h.
Further, the continuous crystallization reaction process in the step (3): the method is characterized in that partial cobalt carbonate slurry synthesized by a cobalt chloride solution and an ammonium bicarbonate solution overflows to a thickener through an overflow port of a reaction kettle, the mother liquor and the thick slurry are obtained through concentration of the thickener, and the thick slurry returns to the reaction kettle for multiple cyclic crystallization reactions.
Furthermore, the stirring mechanism of the reaction kettle adopts three layers of stirring blades, and the volume of the reaction kettle is 16m3。
Further, the cobalt carbonate finished product in the step (4) is washed by a filter press, and the washing process adopts a pure water washing mode, wherein the temperature of the pure water is 70-90 ℃, and the chloride ion content in the washed cobalt carbonate finished product is 0-0.005%.
Further, in the step (4), the wet cobalt carbonate material obtained by washing is dried at the temperature of 150-200 ℃ through a flash evaporation machine, and is sieved by a 200-mesh airflow sieve to obtain a dry cobalt carbonate material.
Further, in the step (5), introducing hydrogen into the cobalt carbonate dry material through a reduction furnace at the temperature of 550-650 ℃ for reduction to obtain cobalt powder, crushing the cobalt powder through an airflow crusher, and sieving and packaging the crushed cobalt powder through a 200-mesh sieving machine.
The preparation method has the beneficial technical effects that the cobalt powder prepared by the method has uniform particle size distribution, no sintering agglomeration, spherical morphology, Fisher particle size of 3-5.5 mu m and the like, and is easy to industrialize.
Drawings
FIG. 1 is an electron micrograph of cobalt powder obtained in example 1;
FIG. 2 is an electron micrograph of cobalt powder obtained in example 2;
FIG. 3 is an electron micrograph of cobalt powder obtained in example 3.
FIG. 4 is an electron micrograph of cobalt powder obtained in the comparative example.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The method comprises the following steps: the first step is as follows: preparing cobalt chloride solution and ammonium bicarbonate solution with different concentrations; the second step is that: synthesizing cobalt carbonate through a reaction kettle; the third step: washing the cobalt carbonate by a filter press, and controlling the concentration of chloride ions in the cobalt carbonate; the fourth step: directly drying wet cobalt carbonate by a flash evaporation machine; the fifth step: and reducing the screened dry material cobalt carbonate into cobalt powder at high temperature by a reducing furnace.
Example 1
A preparation method of large FSSS spherical cobalt powder comprises the following steps:
(1) preparing a cobalt chloride solution with the cobalt ion concentration of 120g/L and an ammonium bicarbonate solution with the concentration of 280 g/L;
(2) the volume of the stirring blade adopting three layers is 16m3Sequentially adding base liquid prepared from pure water and ammonium bicarbonate solution into the reaction kettle, stirring, and controlling the pH of the base liquid to be 7.5; the concentration of ammonium bicarbonate in the base solution is 2g/L, and the ratio of the volume of the added pure water to the volume of the reaction kettle is 1.5; the temperature of the base solution is 60 ℃, and the stirring speed in the reaction kettle is 300 r/min;
(3) adding a cobalt chloride solution and an ammonium bicarbonate solution into a reaction kettle at the same time at feeding flow rates of 800L/h and 1500L/h respectively to perform a synthesis reaction, maintaining the pH of slurry in the reaction kettle to be 7.0-7.1, controlling the growth speed of seed crystals synthesized by the reaction to be 0.25 mu m increased every 8 hours, and performing continuous crystallization reaction in the simultaneous feeding process: the method comprises the following steps of (1) enabling a part of synthesized cobalt carbonate slurry overflowing through an overflow port (30 cm away from a kettle port) of a reaction kettle to enter a thickener to be concentrated to obtain mother liquor and thick slurry, continuously returning the thick slurry into the reaction kettle to carry out multiple circulating crystallization reactions, discharging the mother liquor, and stopping the reaction when the particle size D50 generated by the reaction grows to 12.0 mu m to obtain a cobalt carbonate finished product;
(4) washing the cobalt carbonate finished product by using a filter press, wherein the washing process adopts a pure water washing mode, the temperature of the pure water is 70 ℃, and the chloride ion content in the washed cobalt carbonate finished product is 0.004%; drying the washed wet cobalt carbonate material at 200 ℃ by a flash evaporation machine, and screening by using a 200-mesh airflow screen to obtain a dry cobalt carbonate material;
(5) introducing hydrogen into the cobalt carbonate dry material through a reducing furnace at the temperature of 650 ℃ for reduction to obtain cobalt powder, crushing the cobalt powder through an airflow crusher, and sieving and packaging the crushed cobalt powder through a 200-mesh sieving machine, wherein the Fisher particle size of the cobalt powder is 3.8 mu m.
Example 2
A preparation method of large FSSS spherical cobalt powder comprises the following steps:
(1) preparing a cobalt chloride solution with the cobalt ion concentration of 150g/L and preparing an ammonium bicarbonate solution with the concentration of 200 g/L;
(2) the volume of the stirring blade adopting three layers is 16m3Sequentially adding base liquid prepared from pure water and ammonium bicarbonate solution into the reaction kettle, stirring, and controlling the pH of the base liquid to be 8.0; the concentration of ammonium bicarbonate in the base solution is 6g/L, and the ratio of the volume of the added pure water to the volume of the reaction kettle is 1.0; the temperature of the base solution is 45 ℃, and the stirring speed in the reaction kettle is 250 r/min;
(3) adding a cobalt chloride solution and an ammonium bicarbonate solution into a reaction kettle at the same time at feeding flow rates of 520L/h and 2000L/h respectively to perform a synthesis reaction, maintaining the pH of slurry in the reaction kettle to be 7.1-7.2, controlling the growth rate of seed crystals synthesized by the reaction to be 0.35 mu m increased every 8 hours, and performing continuous crystallization reaction in the simultaneous feeding process: the method comprises the following steps of (1) enabling a part of synthesized cobalt carbonate slurry overflowing through an overflow port (30 cm away from a kettle port) of a reaction kettle to enter a thickener to be concentrated to obtain mother liquor and thick slurry, continuously returning the thick slurry into the reaction kettle to carry out multiple circulating crystallization reactions, discharging the mother liquor, and stopping the reaction when the particle size D50 generated by the reaction grows to 13.0 mu m to obtain a cobalt carbonate finished product;
(4) washing the cobalt carbonate finished product by a filter press, wherein the washing process adopts a pure water washing mode, the temperature of the pure water is 90 ℃, and chloride ions in the washed cobalt carbonate finished product are 0.0045%; drying the washed wet cobalt carbonate material at 180 ℃ by a flash evaporation machine, and screening by using a 200-mesh airflow screen to obtain a dry cobalt carbonate material;
(5) introducing hydrogen into the cobalt carbonate dry material through a reducing furnace at the temperature of 600 ℃ for reduction to obtain cobalt powder, crushing the cobalt powder through an airflow crusher, and sieving and packaging the crushed cobalt powder through a 200-mesh sieving machine, wherein the Fisher particle size of the cobalt powder is 4.5 mu m.
Example 3
A preparation method of large FSSS spherical cobalt powder comprises the following steps:
(1) preparing a cobalt chloride solution with the cobalt ion concentration of 175g/L and preparing an ammonium bicarbonate solution with the concentration of 240 g/L;
(2) the volume of the stirring blade adopting three layers is 16m3Sequentially adding base liquid prepared from pure water and ammonium bicarbonate solution into the reaction kettle, stirring, and controlling the pH of the base liquid to be 8.5; the concentration of ammonium bicarbonate in the base solution is 10g/L, and the ratio of the volume of the added pure water to the volume of the reaction kettle is 0.5; the temperature of the base solution is 50 ℃, and the stirring speed in the reaction kettle is 170 r/min;
(3) adding a cobalt chloride solution and an ammonium bicarbonate solution into a reaction kettle at the same time at feeding flow rates of 650L/h and 2400L/h respectively to perform a synthesis reaction, maintaining the pH of slurry in the reaction kettle to be 7.1-7.3, controlling the growth rate of seed crystals synthesized by the reaction to be 0.45 mu m increased every 8 hours, and performing continuous crystallization reaction in the simultaneous feeding process: the method comprises the following steps of (1) enabling a part of synthesized cobalt carbonate slurry overflowing through an overflow port (30 cm away from a kettle port) of a reaction kettle to enter a thickener to be concentrated to obtain mother liquor and thick slurry, continuously returning the thick slurry into the reaction kettle to carry out multiple circulating crystallization reactions, discharging the mother liquor, and stopping the reaction when the particle size D50 generated by the reaction grows to 14.0 mu m to obtain a cobalt carbonate finished product;
(4) washing the cobalt carbonate finished product by a filter press, wherein the washing process adopts a pure water washing mode, the temperature of the pure water is 80 ℃, and chloride ions in the washed cobalt carbonate finished product are 0.003%; drying the washed wet cobalt carbonate material at 160 ℃ by a flash evaporation machine, and screening by using a 200-mesh airflow screen to obtain a dry cobalt carbonate material;
(5) introducing hydrogen into the cobalt carbonate dry material through a reducing furnace at the temperature of 550 ℃ for reduction to obtain cobalt powder, crushing the cobalt powder through an airflow crusher, and sieving and packaging the crushed cobalt powder through a 200-mesh sieving machine, wherein the Fisher particle size of the cobalt powder is 5.0 mu m.
Comparative example
A preparation method of large FSSS spherical cobalt powder comprises the following steps:
(1) preparing a cobalt chloride solution with the cobalt ion concentration of 175g/L and an ammonium bicarbonate solution with the concentration of 260 g/L;
(2) the volume of the stirring blade adopting three layers is 16m3Sequentially adding base liquid prepared from pure water and ammonium bicarbonate solution into the reaction kettle, stirring, and controlling the pH of the base liquid to be 8.8; the concentration of ammonium bicarbonate in the base solution is 20g/L, and the ratio of the volume of the added pure water to the volume of the reaction kettle is 0.5; the temperature of the base solution is 55 ℃, and the stirring speed in the reaction kettle is 170 r/min;
(3) adding a cobalt chloride solution and an ammonium bicarbonate solution into a reaction kettle at the same time at the feeding flow rates of 850L/h and 2600L/h respectively for a synthesis reaction, maintaining the pH of slurry in the reaction kettle to be 7.1-7.3, controlling the growth speed of seed crystals synthesized by the reaction to be 0.45 mu m increased every 8 hours, and stopping the reaction when the granularity D50 of particles generated by the reaction grows to 14.0 mu m to obtain a cobalt carbonate finished product;
(4) washing the cobalt carbonate finished product by a filter press, wherein the washing process adopts a pure water washing mode, the temperature of the pure water is 70 ℃, and the chloride ions in the washed cobalt carbonate finished product are 0.005%; drying the washed wet cobalt carbonate material at 200 ℃ by a flash evaporation machine, and screening by using a 200-mesh airflow screen to obtain a dry cobalt carbonate material;
(5) introducing hydrogen into the cobalt carbonate dry material through a reducing furnace at the temperature of 650 ℃ for reduction to obtain cobalt powder, crushing the cobalt powder through an airflow crusher, and sieving and packaging the crushed cobalt powder through a 200-mesh sieving machine, wherein the Fisher particle size of the cobalt powder is 3.0 mu m.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.
Claims (9)
1. A preparation method of large FSSS spherical cobalt powder is characterized by comprising the following steps:
(1) preparing a cobalt chloride solution and an ammonium bicarbonate solution;
(2) adding the base solution into the reaction kettle, stirring, and controlling the pH value of the base solution to be 7.5-8.5;
(3) adding a cobalt chloride solution and an ammonium bicarbonate solution into a reaction kettle simultaneously to carry out a synthesis reaction, maintaining the pH of slurry in the reaction kettle to be 7.0-7.3, controlling the growth speed of seed crystals synthesized by the reaction to be 0.25-0.45 mu m increased every 8 hours, carrying out continuous crystallization reaction in the simultaneous feeding process, and stopping the reaction when the granularity D50 of particles generated by the reaction is 12.0-14.0 mu m, thus obtaining a cobalt carbonate finished product;
(4) washing, drying and screening the finished cobalt carbonate product to obtain a cobalt carbonate dry material;
(5) the cobalt carbonate dry material is calcined, reduced, crushed and screened, and then is packaged to obtain cobalt powder.
2. The preparation method of large FSSS spherical cobalt powder as claimed in claim 1, wherein the cobalt ion concentration in the cobalt chloride solution in step (1) is 120g/L-180g/L, and the ammonium bicarbonate solution concentration is 200g/L-280 g/L.
3. The preparation method of large FSSS spherical cobalt powder as claimed in claim 1, wherein the base solution in step (2) is prepared by sequentially adding pure water and ammonium bicarbonate solution into a reaction kettle, the concentration of ammonium bicarbonate in the base solution is 2g/L-10g/L, and the ratio of the volume of the added pure water to the volume of the reaction kettle is 0.5-1.5; the temperature of the base solution is 40-60 ℃, and the stirring speed in the reaction kettle is 150-300 r/min.
4. The method for preparing large FSSS spherical cobalt powder as claimed in claim 1, wherein the feed flow rate of the cobalt chloride solution into the reaction kettle in the step (3) is 500L/h-800L/h, and the feed flow rate of the ammonium bicarbonate solution into the reaction kettle is 1500L/h-2500L/h.
5. The method for preparing large FSSS spherical cobalt powder as claimed in claim 1, wherein the continuous crystallization reaction process in the step (3): the method is characterized in that partial cobalt carbonate slurry synthesized by a cobalt chloride solution and an ammonium bicarbonate solution overflows to a thickener through an overflow port of a reaction kettle, the mother liquor and the thick slurry are obtained through concentration of the thickener, and the thick slurry returns to the reaction kettle for multiple cyclic crystallization reactions.
6. The method for preparing large FSSS spherical cobalt powder as claimed in claim 1, wherein the stirring mechanism of the reaction kettle adopts three layers of stirring blades, and the volume of the reaction kettle is 16m3。
7. The preparation method of large FSSS spherical cobalt powder as claimed in claim 1, wherein the cobalt carbonate finished product in step (4) is washed by a filter press, the washing process is carried out by pure water, the temperature of the pure water is 70-90 ℃, and the chloride ion content in the washed cobalt carbonate finished product is 0-0.005%.
8. The method for preparing large FSSS spherical cobalt powder as claimed in claim 1, wherein the wet cobalt carbonate obtained by washing in step (4) is dried by flash evaporation at 150-200 ℃ and sieved by 200-mesh airflow sieve to obtain dry cobalt carbonate.
9. The preparation method of large FSSS spherical cobalt powder as claimed in claim 1, wherein in the step (5), the cobalt carbonate dry material is reduced by introducing hydrogen into a reduction furnace at a temperature of 550-650 ℃ to obtain cobalt powder, and the cobalt powder is crushed by a jet mill and then screened and packaged by a 200-mesh sieving machine.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114905048A (en) * | 2022-06-02 | 2022-08-16 | 兰州理工大学 | Preparation method of nano cobalt powder for additive manufacturing |
| CN115488346A (en) * | 2022-08-25 | 2022-12-20 | 荆门市格林美新材料有限公司 | Cobalt powder for tungsten-based high-density alloy, preparation method and application |
| CN115872456A (en) * | 2022-11-18 | 2023-03-31 | 贵州雅友新材料有限公司 | Preparation method and application of nano spherical cobalt carbonate |
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