CN111266602A - Preparation method of superfine cobalt-nickel powder for hard alloy - Google Patents
Preparation method of superfine cobalt-nickel powder for hard alloy Download PDFInfo
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Abstract
The invention discloses a preparation method of superfine cobalt-nickel powder for hard alloy, which comprises the steps of mixing a cobalt chloride solution and a nickel chloride solution into a base solution according to a proportion, adding the base solution into a reaction kettle, then adding a sodium carbonate solution into the reaction kettle in a spraying mode, stirring for 3-4 hours at 40-80 ℃ to obtain a cobalt-nickel mixed solution, then carrying out filter pressing treatment and washing slurrying to obtain cobalt-nickel mixed slurry, and finally carrying out high-temperature reduction to directly obtain the superfine cobalt-nickel powder; therefore, the method can avoid the problem of powder agglomeration when the cobalt powder is prepared simply, and meanwhile, the directly prepared superfine cobalt-nickel powder has uniform particle size distribution and smaller particle size, can be directly used for preparing hard alloy, avoids the problem of hard alloy tool defects caused by uneven mixing, and prolongs the service life of the hard alloy.
Description
Technical Field
The invention belongs to the technical field of preparation of cobalt-nickel composite powder, and particularly relates to a preparation method of superfine cobalt-nickel powder for hard alloy.
Background
In the fields of diamond tools and cemented carbide materials, cobalt-nickel alloy powders are widely used due to their excellent bonding and strength properties.
In the process of simply preparing the cobalt powder, the cobalt powder is easy to agglomerate, so that the hole defect is caused in the process of preparing the hard alloy, the service life of the hard alloy is influenced,
when the mixed pressed film of the hard alloy cobalt powder, the nickel powder, the WC and the like is adopted, because the mixing of various powders is not uniform, the defects exist in the process of preparing the hard alloy easily, and the performance and the service life of the hard alloy are influenced
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of superfine cobalt-nickel powder for hard alloy.
The invention provides a preparation method of superfine cobalt-nickel powder for hard alloy, which is implemented by the following steps:
step 1, mixing a cobalt chloride solution and a nickel chloride solution in proportion to obtain a base solution, adding the base solution into a reaction kettle, then adding a sodium carbonate solution into the reaction kettle in a spraying manner, and stirring for 3-4 hours at 40-80 ℃ to obtain a cobalt-nickel mixed solution;
step 2, performing filter pressing treatment on the cobalt-nickel composite solution obtained in the step 1, washing the cobalt-nickel composite solution subjected to filter pressing treatment by using pure water, and slurrying the washed cobalt-nickel composite solution to obtain cobalt-nickel mixed slurry;
step 3, placing the cobalt-nickel mixed slurry obtained in the step 2 into a high-pressure reaction kettle, and performing high-temperature reduction by using hydrogen to obtain a reduced cobalt-nickel mixed solution;
and 4, sequentially carrying out solid-liquid separation, washing and drying on the reduced cobalt-nickel mixed solution obtained in the step 3 to obtain superfine cobalt-nickel powder.
In the scheme, the metal molar ratio of the cobalt chloride solution to the nickel chloride solution in the step 1 is 1: 1.5-1: 3.
In the scheme, the concentration of the cobalt chloride solution in the step 1 is 60-80 g/L.
In the scheme, the concentration of the nickel chloride solution in the step 1 is 120-140 g/L.
In the scheme, the concentration of the sodium carbonate solution in the step 1 is 120-150 g/L.
In the scheme, the mass ratio of the sodium carbonate solution added in the step 1 to the base solution is 1: 1.3-1.5.
In the scheme, the temperature of the pure water in the step 2 is 60-85 ℃.
In the scheme, the reaction temperature of the high-temperature reduction in the step 3 is 300-420 ℃, and the reaction time is 5-10 hours.
In the scheme, pure water at 25-40 ℃ is adopted for washing in the step 4.
In the scheme, the drying temperature in the step 4 is 40-80 ℃.
Compared with the prior art, the method controls the cobalt-nickel ratio of the superfine cobalt-nickel powder by controlling the ratio of the cobalt chloride solution to the nickel chloride solution, and adopts a spraying mode to add sodium carbonate, and finally, the superfine cobalt-nickel powder is directly obtained by a high-pressure reduction method, so that the problem of powder agglomeration when the cobalt powder is simply prepared can be avoided, and meanwhile, the directly prepared superfine cobalt-nickel powder has uniform particle size distribution and smaller particle size, can be directly used for preparing the hard alloy, avoids the problem of defects of the hard alloy tool caused by uneven mixing, and prolongs the service life of the hard alloy.
Drawings
Fig. 1 is a scanning electron microscope image of the ultrafine cobalt nickel powder prepared by the method for preparing the ultrafine cobalt nickel powder for cemented carbide according to embodiment 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of superfine cobalt-nickel powder for hard alloy, which is implemented by the following steps:
step 1, mixing a cobalt chloride solution with the concentration of 60-80 g/L and a nickel chloride solution with the concentration of 120-140 g/L according to the metal molar ratio of 1: 1.5-1: 3 to form a base solution, adding the base solution into a reaction kettle, wherein the adding amount of the base solution is 2-3 m3Then, adding a sodium carbonate solution with the concentration of 120-150 g/L into the reaction kettle in a spraying mode, wherein the mass ratio of the added sodium carbonate solution to the base solution is 1: 1.3-1.5, keeping the temperature of the reaction kettle at 40-80 ℃, and stirring for 3-4 hours to obtain a cobalt-nickel mixed solution;
step 2, transferring the cobalt-nickel composite solution obtained in the step 1 into a filter press to remove mother liquor, washing for 3-5 times by adopting pure water at the temperature of 60-85 ℃, and transferring the washed feed liquid to a slurrying barrel to perform slurrying treatment to obtain cobalt-nickel mixed slurry;
step 3, placing the cobalt-nickel mixed slurry obtained in the step 2 in a high-pressure reaction kettle, introducing inert gas into the high-pressure reaction kettle, introducing hydrogen in a reducing atmosphere, carrying out high-temperature reduction reaction at 300-420 ℃ in the hydrogen atmosphere, keeping the pressure in the reaction kettle at 5-8 atmospheric pressures, and reacting for 5-10 hours under the pressure to obtain a reduced cobalt-nickel mixed solution;
and 4, carrying out solid-liquid separation on the reduced cobalt-nickel mixed solution obtained in the step 3, washing filter residues obtained after separation for 3-5 times by adopting pure water at the temperature of 25-40 ℃, and drying at the temperature of 40-80 ℃ after washing to obtain superfine cobalt-nickel powder.
According to the invention, the cobalt-nickel ratio of the superfine cobalt-nickel powder is controlled by controlling the proportion of the cobalt chloride solution and the nickel chloride solution, the sodium carbonate is added in a spraying manner, and finally, the superfine cobalt-nickel powder is directly obtained by a high-pressure reduction method, so that the problem of powder agglomeration when the cobalt powder is simply prepared can be avoided, and meanwhile, the directly prepared superfine cobalt-nickel powder has uniform particle size distribution, smaller particle size, D103.5 mu m, D507.2 mu m and D9018.5 mu m, can be directly used for preparing hard alloy, the problem of defects of hard alloy tools caused by uneven mixing is avoided, and the service life of the hard alloy is prolonged.
Example 1
The embodiment 1 of the invention provides a preparation method of superfine cobalt-nickel powder for hard alloy, which is implemented by the following steps:
step 1, mixing a cobalt chloride solution with the concentration of 60-80 g/L and a nickel chloride solution with the concentration of 120-140 g/L according to the metal molar ratio of 1:1.5 to form a base solution, adding the base solution into a reaction kettle, wherein the adding amount of the base solution is 2-3 m3Then, adding a sodium carbonate solution with the concentration of 120-150 g/L into the reaction kettle in a spraying mode, wherein the mass ratio of the added sodium carbonate solution to the base solution is 1:1.5, and stirring the reaction kettle for 4 hours at the temperature of 40 ℃ to obtain a cobalt-nickel mixed solution;
step 2, transferring the cobalt-nickel composite solution obtained in the step 1 into a filter press to remove mother liquor, washing for 3-5 times by adopting pure water at 72 ℃, transferring the washed feed liquid to a slurrying barrel to perform slurrying treatment, and obtaining cobalt-nickel mixed slurry;
step 3, placing the cobalt-nickel mixed slurry obtained in the step 2 in a high-pressure reaction kettle, introducing inert gas into the high-pressure reaction kettle, introducing hydrogen in a reducing atmosphere, carrying out high-temperature reduction reaction at 380 ℃ in the hydrogen atmosphere, keeping the pressure in the reaction kettle at 5-8 atmospheric pressures, and reacting for 8 hours under the pressure to obtain a reduced cobalt-nickel mixed solution;
and 4, carrying out solid-liquid separation on the reduced cobalt-nickel mixed solution obtained in the step 3, washing filter residues obtained after separation for 3-5 times by adopting pure water at 30 ℃, and drying at 60 ℃ after washing to obtain superfine cobalt-nickel powder.
As shown in fig. 1, it can be seen that the cobalt-nickel powder is uniformly mixed, the particle size D100 is not greater than 20um, and the average particle size distribution is about 7 μm.
Example 2
The embodiment 2 of the invention provides a preparation method of superfine cobalt-nickel powder for hard alloy, which is implemented by the following steps:
step 1, mixing a cobalt chloride solution with the concentration of 60-80 g/L and a nickel chloride solution with the concentration of 120-140 g/L according to the metal molar ratio of 1:1.4 to form a base solution, adding the base solution into a reaction kettle, wherein the adding amount of the base solution is 2-3 m3Then, adding a sodium carbonate solution with the concentration of 120-150 g/L into the reaction kettle in a spraying mode, wherein the mass ratio of the added sodium carbonate solution to the base solution is 1:1.4, and keeping the temperature of the reaction kettle at 60 ℃ and stirring for 3.8 hours to obtain a cobalt-nickel mixed solution;
step 2, transferring the cobalt-nickel composite solution obtained in the step 1 into a filter press to remove mother liquor, washing for 3-5 times by adopting pure water at 72 ℃, transferring the washed feed liquid to a slurrying barrel to perform slurrying treatment, and obtaining cobalt-nickel mixed slurry;
step 3, placing the cobalt-nickel mixed slurry obtained in the step 2 in a high-pressure reaction kettle, introducing inert gas into the high-pressure reaction kettle, introducing hydrogen in a reducing atmosphere, carrying out high-temperature reduction reaction at 380 ℃ in the hydrogen atmosphere, keeping the pressure in the reaction kettle at 5-8 atmospheric pressures, and reacting for 8 hours under the pressure to obtain a reduced cobalt-nickel mixed solution;
and 4, carrying out solid-liquid separation on the reduced cobalt-nickel mixed solution obtained in the step 3, washing filter residues obtained after separation for 3-5 times by adopting pure water at 30 ℃, and drying at 60 ℃ after washing to obtain superfine cobalt-nickel powder.
The cobalt-nickel powder of the superfine cobalt-nickel powder for the hard alloy provided by the embodiment 2 of the invention is uniformly mixed, the particle size D100 is not more than 20um, and the average particle size distribution is about 7 mu m.
Example 3
Embodiment 3 of the present invention provides a method for preparing ultrafine cobalt nickel powder for cemented carbide, which is implemented by the following steps:
step 1, mixing a cobalt chloride solution with the concentration of 60-80 g/L and a nickel chloride solution with the concentration of 120-140 g/L according to the metal molar ratio of 1:1:3 to form a base solution, adding the base solution into a reaction kettle, wherein the adding amount of the base solution is 2-3 m3Then spraying into the reaction kettleAdding a sodium carbonate solution with the concentration of 120-150 g/L, wherein the mass ratio of the added sodium carbonate solution to the base solution is 1:1.3, keeping the temperature of the reaction kettle at 80 ℃, and stirring for 3 hours to obtain a cobalt-nickel mixed solution;
step 2, transferring the cobalt-nickel composite solution obtained in the step 1 into a filter press to remove mother liquor, washing for 3-5 times by adopting pure water at 72 ℃, transferring the washed feed liquid to a slurrying barrel to perform slurrying treatment, and obtaining cobalt-nickel mixed slurry;
step 3, placing the cobalt-nickel mixed slurry obtained in the step 2 in a high-pressure reaction kettle, introducing inert gas into the high-pressure reaction kettle, introducing hydrogen in a reducing atmosphere, carrying out high-temperature reduction reaction at 380 ℃ in the hydrogen atmosphere, keeping the pressure in the reaction kettle at 5-8 atmospheric pressures, and reacting for 8 hours under the pressure to obtain a reduced cobalt-nickel mixed solution;
and 4, carrying out solid-liquid separation on the reduced cobalt-nickel mixed solution obtained in the step 3, washing filter residues obtained after separation for 3-5 times by adopting pure water at 30 ℃, and drying at 60 ℃ after washing to obtain superfine cobalt-nickel powder.
The cobalt-nickel powder of the superfine cobalt-nickel powder for the hard alloy provided by the embodiment 3 of the invention is uniformly mixed, the particle size D100 is not more than 20um, and the average particle size distribution is about 7 mu m.
Example 4
Embodiment 4 of the present invention provides a method for preparing ultrafine cobalt nickel powder for cemented carbide, which is implemented by the following steps:
step 1, mixing a cobalt chloride solution with the concentration of 60-80 g/L and a nickel chloride solution with the concentration of 120-140 g/L according to the metal molar ratio of 1:1.4 to form a base solution, adding the base solution into a reaction kettle, wherein the adding amount of the base solution is 2-3 m3Then, adding a sodium carbonate solution with the concentration of 120-150 g/L into the reaction kettle in a spraying mode, wherein the mass ratio of the added sodium carbonate solution to the base solution is 1:1.4, and keeping the temperature of the reaction kettle at 64 ℃ and stirring for 3.5 hours to obtain a cobalt-nickel mixed solution;
step 2, transferring the cobalt-nickel composite solution obtained in the step 1 into a filter press to remove mother liquor, washing for 3-5 times by adopting pure water at 60 ℃, transferring the washed feed liquid to a slurrying barrel to perform slurrying treatment, and obtaining cobalt-nickel mixed slurry;
step 3, placing the cobalt-nickel mixed slurry obtained in the step 2 in a high-pressure reaction kettle, introducing inert gas into the high-pressure reaction kettle, introducing hydrogen in a reducing atmosphere, carrying out high-temperature reduction reaction at 360 ℃ in the hydrogen atmosphere, keeping the pressure in the reaction kettle at 5-8 atmospheric pressures, and reacting for 6 hours under the pressure to obtain a reduced cobalt-nickel mixed solution;
and 4, carrying out solid-liquid separation on the reduced cobalt-nickel mixed solution obtained in the step 3, washing filter residues obtained after separation for 3-5 times by adopting pure water at 25 ℃, and drying at 40 ℃ after washing to obtain superfine cobalt-nickel powder.
The cobalt-nickel powder of the superfine cobalt-nickel powder for the hard alloy provided by the embodiment 4 of the invention is uniformly mixed, the particle size D100 is not more than 20um, and the average particle size distribution is about 7 mu m.
Example 5
Embodiment 5 of the present invention provides a method for preparing ultrafine cobalt nickel powder for cemented carbide, which is implemented by the following steps:
step 1, mixing a cobalt chloride solution with the concentration of 60-80 g/L and a nickel chloride solution with the concentration of 120-140 g/L according to the metal molar ratio of 1:1.4 to form a base solution, adding the base solution into a reaction kettle, wherein the adding amount of the base solution is 2-3 m3Then, adding a sodium carbonate solution with the concentration of 120-150 g/L into the reaction kettle in a spraying mode, wherein the mass ratio of the added sodium carbonate solution to the base solution is 1:1.4, and keeping the temperature of the reaction kettle at 64 ℃ and stirring for 3.5 hours to obtain a cobalt-nickel mixed solution;
step 2, transferring the cobalt-nickel composite solution obtained in the step 1 into a filter press to remove mother liquor, washing for 3-5 times by adopting pure water at 72 ℃, transferring the washed feed liquid to a slurrying barrel to perform slurrying treatment, and obtaining cobalt-nickel mixed slurry;
step 3, placing the cobalt-nickel mixed slurry obtained in the step 2 in a high-pressure reaction kettle, introducing inert gas into the high-pressure reaction kettle, introducing hydrogen in a reducing atmosphere, carrying out high-temperature reduction reaction at 360 ℃ in the hydrogen atmosphere, keeping the pressure in the reaction kettle at 5-8 atmospheric pressures, and reacting for 6 hours under the pressure to obtain a reduced cobalt-nickel mixed solution;
and 4, carrying out solid-liquid separation on the reduced cobalt-nickel mixed solution obtained in the step 3, washing filter residues obtained after separation for 3-5 times by adopting pure water at 30 ℃, and drying at 62 ℃ after washing to obtain superfine cobalt-nickel powder.
The cobalt-nickel powder of the superfine cobalt-nickel powder for the hard alloy provided by the embodiment 5 of the invention is uniformly mixed, the particle size D100 is not more than 20um, and the average particle size distribution is about 7 mu m.
Example 6
Embodiment 6 of the present invention provides a method for preparing ultrafine cobalt nickel powder for cemented carbide, which is implemented by the following steps:
step 1, mixing a cobalt chloride solution with the concentration of 60-80 g/L and a nickel chloride solution with the concentration of 120-140 g/L according to the metal molar ratio of 1:1.4 to form a base solution, adding the base solution into a reaction kettle, wherein the adding amount of the base solution is 2-3 m3Then, adding a sodium carbonate solution with the concentration of 120-150 g/L into the reaction kettle in a spraying mode, wherein the mass ratio of the added sodium carbonate solution to the base solution is 1:1.4, and keeping the temperature of the reaction kettle at 64 ℃ and stirring for 3.5 hours to obtain a cobalt-nickel mixed solution;
step 2, transferring the cobalt-nickel composite solution obtained in the step 1 into a filter press to remove mother liquor, washing for 3-5 times by pure water at 85 ℃, transferring the washed feed liquid to a slurrying barrel for slurrying treatment, and obtaining cobalt-nickel mixed slurry;
step 3, placing the cobalt-nickel mixed slurry obtained in the step 2 in a high-pressure reaction kettle, introducing inert gas into the high-pressure reaction kettle, introducing hydrogen in a reducing atmosphere, carrying out high-temperature reduction reaction at 360 ℃ in the hydrogen atmosphere, keeping the pressure in the reaction kettle at 5-8 atmospheric pressures, and reacting for 6 hours under the pressure to obtain a reduced cobalt-nickel mixed solution;
and 4, carrying out solid-liquid separation on the reduced cobalt-nickel mixed solution obtained in the step 3, washing filter residues obtained after separation for 3-5 times by adopting pure water at 40 ℃, and drying at 80 ℃ after washing to obtain superfine cobalt-nickel powder.
The cobalt-nickel powder of the superfine cobalt-nickel powder for the hard alloy provided by the embodiment 6 of the invention is uniformly mixed, the particle size D100 is not more than 20um, and the average particle size distribution is about 7 mu m.
Example 7
Embodiment 7 of the present invention provides a method for preparing ultrafine cobalt nickel powder for cemented carbide, which is implemented by the following steps:
step 1, mixing a cobalt chloride solution with the concentration of 60-80 g/L and a nickel chloride solution with the concentration of 120-140 g/L according to the metal molar ratio of 1:1.3 to form a base solution, adding the base solution into a reaction kettle, wherein the adding amount of the base solution is 2-3 m3Then, adding a sodium carbonate solution with the concentration of 120-150 g/L into the reaction kettle in a spraying mode, wherein the mass ratio of the added sodium carbonate solution to the base solution is 1:1.4, and keeping the temperature of the reaction kettle at 58 ℃ and stirring for 4 hours to obtain a cobalt-nickel mixed solution;
step 2, transferring the cobalt-nickel composite solution obtained in the step 1 into a filter press to remove mother liquor, washing for 3-5 times by adopting pure water at 72 ℃, transferring the washed feed liquid to a slurrying barrel to perform slurrying treatment, and obtaining cobalt-nickel mixed slurry;
step 3, placing the cobalt-nickel mixed slurry obtained in the step 2 in a high-pressure reaction kettle, introducing inert gas into the high-pressure reaction kettle, introducing hydrogen in a reducing atmosphere, carrying out high-temperature reduction reaction at 300 ℃ in the hydrogen atmosphere, keeping the pressure in the reaction kettle at 5-8 atmospheric pressures, and reacting for 10 hours under the pressure to obtain a reduced cobalt-nickel mixed solution;
and 4, carrying out solid-liquid separation on the reduced cobalt-nickel mixed solution obtained in the step 3, washing filter residues obtained after separation for 3-5 times by adopting pure water at 32 ℃, and drying at 60 ℃ after washing to obtain superfine cobalt-nickel powder.
The cobalt-nickel powder of the superfine cobalt-nickel powder for the hard alloy provided by the embodiment 7 of the invention is uniformly mixed, the particle size D100 is not more than 20um, and the average particle size distribution is about 7 mu m.
Example 8
Embodiment 8 of the present invention provides a method for preparing ultrafine cobalt nickel powder for cemented carbide, which is implemented by the following steps:
step 1, mixing a cobalt chloride solution with the concentration of 60-80 g/L and a nickel chloride solution with the concentration of 120-140 g/L according to the metal molar ratio of 1:1.3 to form a base solution, adding the base solution into a reaction kettle, wherein the adding amount of the base solution is 2-3 m3Then, adding a sodium carbonate solution with the concentration of 120-150 g/L into the reaction kettle in a spraying mode, wherein the mass ratio of the added sodium carbonate solution to the base solution is 1:1.4, and keeping the temperature of the reaction kettle at 58 ℃ and stirring for 4 hours to obtain a cobalt-nickel mixed solution;
step 2, transferring the cobalt-nickel composite solution obtained in the step 1 into a filter press to remove mother liquor, washing for 3-5 times by adopting pure water at 72 ℃, transferring the washed feed liquid to a slurrying barrel to perform slurrying treatment, and obtaining cobalt-nickel mixed slurry;
step 3, placing the cobalt-nickel mixed slurry obtained in the step 2 in a high-pressure reaction kettle, introducing inert gas into the high-pressure reaction kettle, introducing hydrogen in a reducing atmosphere, carrying out high-temperature reduction reaction at 380 ℃ in the hydrogen atmosphere, keeping the pressure in the reaction kettle at 5-8 atmospheric pressures, and reacting for 8 hours under the pressure to obtain a reduced cobalt-nickel mixed solution;
and 4, carrying out solid-liquid separation on the reduced cobalt-nickel mixed solution obtained in the step 3, washing filter residues obtained after separation for 3-5 times by adopting pure water at 32 ℃, and drying at 60 ℃ after washing to obtain superfine cobalt-nickel powder.
The cobalt-nickel powder of the superfine cobalt-nickel powder for the hard alloy provided by the embodiment 8 of the invention is uniformly mixed, the particle size D100 is not more than 20um, and the average particle size distribution is about 7 mu m.
Example 9
Embodiment 9 of the present invention provides a method for preparing ultrafine cobalt nickel powder for cemented carbide, which is implemented by the following steps:
step 1, mixing a cobalt chloride solution with the concentration of 60-80 g/L and a nickel chloride solution with the concentration of 120-140 g/L according to the metal molar ratio of 1:1.3 to form a base solution, adding the base solution into a reaction kettle, wherein the adding amount of the base solution is 2-3 m3Then, spraying is adoptedAdding a sodium carbonate solution with the concentration of 120-150 g/L into a reaction kettle in a mode that the mass ratio of the added sodium carbonate solution to the base solution is 1:1.4, and keeping the temperature of the reaction kettle at 58 ℃ and stirring for 4 hours to obtain a cobalt-nickel mixed solution;
step 2, transferring the cobalt-nickel composite solution obtained in the step 1 into a filter press to remove mother liquor, washing for 3-5 times by adopting pure water at 72 ℃, transferring the washed feed liquid to a slurrying barrel to perform slurrying treatment, and obtaining cobalt-nickel mixed slurry;
step 3, placing the cobalt-nickel mixed slurry obtained in the step 2 in a high-pressure reaction kettle, introducing inert gas into the high-pressure reaction kettle, introducing hydrogen in a reducing atmosphere, carrying out high-temperature reduction reaction at 420 ℃ in the hydrogen atmosphere, keeping the pressure in the reaction kettle at 5-8 atmospheric pressures, and reacting for 5 hours under the pressure to obtain a reduced cobalt-nickel mixed solution;
and 4, carrying out solid-liquid separation on the reduced cobalt-nickel mixed solution obtained in the step 3, washing filter residues obtained after separation for 3-5 times by adopting pure water at 32 ℃, and drying at 60 ℃ after washing to obtain superfine cobalt-nickel powder.
The cobalt-nickel powder of the superfine cobalt-nickel powder for the hard alloy provided by the embodiment 9 of the invention is uniformly mixed, the particle size D100 is not more than 20um, and the average particle size distribution is about 7 mu m.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention.
Claims (10)
1. A preparation method of superfine cobalt-nickel powder for hard alloy is characterized by comprising the following steps:
step 1, mixing a cobalt chloride solution and a nickel chloride solution in proportion to obtain a base solution, adding the base solution into a reaction kettle, then adding a sodium carbonate solution into the reaction kettle in a spraying manner, and stirring for 3-4 hours at 40-80 ℃ to obtain a cobalt-nickel mixed solution;
step 2, performing filter pressing treatment on the cobalt-nickel composite solution obtained in the step 1, washing the cobalt-nickel composite solution subjected to filter pressing treatment by using pure water, and slurrying the washed cobalt-nickel composite solution to obtain cobalt-nickel mixed slurry;
step 3, placing the cobalt-nickel mixed slurry obtained in the step 2 into a high-pressure reaction kettle, and performing high-temperature reduction by using hydrogen to obtain a reduced cobalt-nickel mixed solution;
and 4, sequentially carrying out solid-liquid separation, washing and drying on the reduced cobalt-nickel mixed solution obtained in the step 3 to obtain superfine cobalt-nickel powder.
2. The method for preparing the ultrafine cobalt nickel powder for the hard alloy according to claim 1, wherein the metal molar ratio of the cobalt chloride solution to the nickel chloride solution in the step 1 is 1:1.5 to 1: 3.
3. The method for preparing the ultrafine cobalt nickel powder for the hard alloy according to claim 2, wherein the concentration of the cobalt chloride solution in the step 1 is 60-80 g/L.
4. The method for preparing the ultrafine cobalt nickel powder for the hard alloy according to claim 3, wherein the concentration of the nickel chloride solution in the step 1 is 120-140 g/L.
5. The method for preparing the ultrafine cobalt nickel powder for the hard alloy according to claim 3, wherein the concentration of the sodium carbonate solution in the step 1 is 120-150 g/L.
6. The method for preparing the ultrafine cobalt nickel powder for the hard alloy according to claim 4, wherein the mass ratio of the sodium carbonate solution added in the step 1 to the base solution is 1: 1.3-1.5.
7. The method for preparing ultra-fine cobalt-nickel powder for cemented carbide as claimed in any one of claims 1 to 6, wherein the temperature of pure water in step 2 is 60 to 85 ℃.
8. The method for preparing the ultrafine cobalt nickel powder for the hard alloy according to claim 7, wherein the reaction temperature of the high-temperature reduction in the step 3 is 300-420 ℃ and the reaction time is 5-10 hours.
9. The method of claim 8, wherein the washing in step 4 is performed with pure water at 25-40 ℃.
10. The method for preparing ultra-fine cobalt-nickel powder for cemented carbide as claimed in claim 9, wherein the drying temperature in step 4 is 40-80 ℃.
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| CN1830606A (en) * | 2006-04-14 | 2006-09-13 | 北京科技大学 | Method of preparing ultrafine alloy powder by coprecipitation coreduction |
| CN101096053A (en) * | 2006-06-29 | 2008-01-02 | 王世荣 | Preparation method of ferro-cobalt ultra-fine powder |
| CN101428348A (en) * | 2008-07-29 | 2009-05-13 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112404447A (en) * | 2020-11-18 | 2021-02-26 | 云南电网有限责任公司电力科学研究院 | Preparation method and application of metallic nickel |
| CN112404447B (en) * | 2020-11-18 | 2023-07-07 | 云南电网有限责任公司电力科学研究院 | Preparation method and application of metallic nickel |
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