CN102886525A - Cobalt powder with large grain size and preparation method thereof - Google Patents
Cobalt powder with large grain size and preparation method thereof Download PDFInfo
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- CN102886525A CN102886525A CN2011102127200A CN201110212720A CN102886525A CN 102886525 A CN102886525 A CN 102886525A CN 2011102127200 A CN2011102127200 A CN 2011102127200A CN 201110212720 A CN201110212720 A CN 201110212720A CN 102886525 A CN102886525 A CN 102886525A
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Abstract
The invention provides cobalt powder with a large grain size and a preparation method thereof. The preparation method of the cobalt powder with the large grain size comprises the following steps of: providing reaction base solution; adding ammonium oxalate and cobalt salt solution into the reaction base solution, reacting at 75-95 DEG C to generate ammonium oxalate sediment, when the D50 gain size of the ammonium oxalate reaches 60 microns, stopping reaction and ageing; carrying solid-liquid separating on the aged ammonium oxalate, drying and crushing to obtain an ammonium oxalate precursor; reducing the ammonium oxalate precursor, and crushing to obtain the cobalt powder with the large grain size. The cobalt powder with the large grain size has the advantages of simple process, easy control and low cost, and is suitable for industrial production. The cobalt powder, prepared by the preparation method of the cobalt powder with the large grain size, has high purity, good dispersity and uniform grain size, the D50 gain size is larger relatively, and is 20-30 microns, so that various requirements of the cobalt powder in industry are satisfied.
Description
Technical field
The invention belongs to powder metallurgical technology, be specifically related to a kind of large particle diameter cobalt powder and preparation method thereof.
Background technology
Cobalt powder has a wide range of applications in field of metallurgy and chemical engineering, is the important raw and processed materials of producing battery electrode, high hardness alloy and the chemical metallurgy products such as diamond tool, catalyst carrier.
Along with the progress of technology, market becomes harsh and diversified to the requirement of cobalt powder quality, and except the requirement to granule-morphology, the client proposes special and special requirement to the indexs such as granularity, oxygen content and apparent density of cobalt powder more and more.Along with the development of industrial technology, the industries such as powder metallurgy, carbide alloy generally to the fine future development, require cobalt powder particle diameter FSSS＜1.8 μ m with cobalt powder.But the super-fine cobalt powder of at present conventional method production, FSSS＜1.8 μ m, D50＜10 μ m, though and the cobalt powder of this D50 particle diameter is conducive to the performances such as cobalt powder disperses in carbide alloy and improve Cemented Carbide Properties, but the specific alloys such as high temperature alloy do not wish that crystal grain is too thin, and wish that lattice is slightly thicker, to put forward the performances such as heavy alloyed fatigue resistance, creep resistant.Therefore, developing the relatively large cobalt powder tool of D50 particle diameter is of great significance.
The cobalt powder of the existing D50 of production particle diameter＜10 μ m generally adopts the cobalt carbonate presoma or adopts oxalic acid to bore presoma.But, no matter adopt existing cobalt carbonate presoma or adopt the cobalt oxalate presoma to generate cobalt powder, the D50 particle diameter of the cobalt powder that obtains＜10 μ m.All can't produce the relatively large cobalt powder of D50 particle diameter.
Summary of the invention
In view of this, the embodiment of the invention provides a kind of cobalt powder D50 particle diameter relatively large large particle diameter cobalt powder preparation method.
And, a kind of large particle diameter cobalt powder that is obtained by above-mentioned large particle diameter cobalt powder preparation method.
The present invention solves the problems of the technologies described above the technical scheme that adopts:
A kind of large particle diameter cobalt powder preparation method comprises the steps:
Reaction end liquid is provided, and liquid is the solidliquid mixture that is added with the cobalt oxalate crystal in 65～75 ℃ of water or the water at the bottom of the described reaction;
Add ammonium oxalate and cobalt salt solution at the bottom of the described reaction in the liquid, react under 75～95 ℃, oxalic cobalt precipitation when the D50 particle diameter for the treatment of described cobalt oxalate reaches 60 μ m, stops reaction and carries out ripening;
To carry out Separation of Solid and Liquid through the described cobalt oxalate of ripening, dry broken, obtain the cobalt oxalate presoma;
With described cobalt oxalate presoma reduction, fragmentation obtains described large particle diameter cobalt powder.
And, a kind of large particle diameter cobalt powder that is prepared by above-mentioned large particle diameter cobalt powder preparation method.
The large particle diameter cobalt powder of the present invention preparation method passes through to the selection of reactant with to the control of temperature with the reaction termination condition, and acquisition cobalt oxalate presoma cobalt oxalate particle diameter is large, purity is high, good dispersion.The cobalt powder purity that obtains with this large particle diameter cobalt powder preparation method is high, and particle diameter is even, and the D50 particle diameter is relatively large, the D50 particle diameter is 20～30 μ m, satisfied in the industry the diversified demand of cobalt powder, and this cobalt powder preparation method technique is simple, easily control, cost is low, is fit to suitability for industrialized production.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples, in the accompanying drawing:
Fig. 1 is the large particle diameter cobalt powder of the present invention preparation method's process chart.
The specific embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
The embodiment of the invention provides a kind of technique simple, easily control, and cost is low, suitable suitability for industrialized production, the large particle diameter cobalt powder preparation method that cobalt powder D50 particle diameter is relatively large comprises the steps:
S1: reaction end liquid is provided, and liquid is the solidliquid mixture that is added with the cobalt oxalate crystal in 65～75 ℃ of water or the water at the bottom of the described reaction;
S2: add ammonium oxalate and cobalt salt solution at the bottom of the described reaction in the liquid, react under 75～95 ℃, oxalic cobalt precipitation when the D50 particle diameter for the treatment of described cobalt oxalate reaches 60 μ m, stops reaction and carries out ripening;
S3: will carry out Separation of Solid and Liquid through the described cobalt oxalate of ripening, drying, fragmentation obtains the cobalt oxalate presoma;
S4: with the reduction of cobalt oxalate presoma, fragmentation obtains described large particle diameter cobalt powder.
Like this, above-mentioned large particle diameter cobalt powder preparation method obtains large, the good dispersion of cobalt oxalate presoma cobalt oxalate particle diameter by to the selection of reactant with to the control of temperature with the reaction termination condition.The cobalt oxalate particle diameter is large in addition, and its specific area is less, so that cobalt oxalate adsorbed water and impurity significantly reduce, reduces the adsorbed water in the cobalt oxalate, so that cobalt oxalate has good dispersiveness in follow-up drying and reduction process; Impurity reduction is so that the purity of cobalt oxalate is high.The cobalt powder purity that obtains with this large particle diameter cobalt powder preparation method is high, particle diameter is even, the D50 particle diameter is relatively large, the D50 particle diameter is 20～30 μ m, has satisfied in the industry the diversified demand of cobalt powder, as has satisfied the specific alloy such as high temperature alloy with the requirement of cobalt powders, and this large particle diameter cobalt powder preparation method technique is simple, easily control, cost is low, is fit to suitability for industrialized production.
Particularly, among above-mentioned large particle diameter cobalt powder preparation method's the step S1, when reaction end liquid is that its compound method is preferably when being added with the solidliquid mixture of cobalt oxalate crystal: in 65～75 ℃ water, add the cobalt oxalate crystal, wherein, the quality percentage composition of cobalt oxalate crystal is 20～50%.The cobalt oxalate crystal of this concentration more is conducive to the generation of step S2 mesoxalic acid cobalt precipitation as the cobalt oxalate crystal seed.During elected water, preferably heat water to 65～75 ℃ of temperature, for participating in of impurity reduction, water is preferably distilled water.
Among above-mentioned large particle diameter cobalt powder preparation method's the step S2, the mol ratio of ammonium oxalate and cobalt salt is preferably 1: 0.5～and 0.8.This preferred proportion so that ammonium oxalate and cobalt salt complete reaction, is unlikely to cause that wherein a certain component is too excessive, the production cost that more is conducive to the generation of cobalt oxalate precipitation and reduces this cobalt oxalate precipitation.This cobalt salt is preferably at least a in cobalt chloride, cobaltous sulfate, cobalt nitrate, the cobalt acetate.The concentration of this cobalt salt solution is preferably 50～120g/L.
Among this step S2, the pH value of liquid preferably is adjusted to 0.5～1.0 at the bottom of adding ammonium oxalate and the cobalt salt solution afterreaction.This preferred pH value, for the generation of cobalt oxalate precipitation provides a favourable acid reaction condition, this acid reaction condition has further improved the generation of cobalt oxalate precipitation and growth, impurity reduction and the moisture of cobalt oxalate precipitation crystal with the condition of reaction temperature and end reaction.
Among this step S2, ripening is conducive to the growth of cobalt oxalate precipitation crystal.The temperature of this ripening is preferably 60～90 ℃, and the time is preferably 1～4 hour.The ripening of this preferred processing condition more is conducive to the growth of cobalt oxalate precipitation crystal.
Among this step S2, ammonium oxalate preferably adopts following method preparation: in the oxalic acid dissolved water, filter, being mixed with concentration is 100～200g/L oxalic acid solution, adds liquefied ammonia in oxalic acid solution, and adjust pH is 1.0～4.5, oxalic acid solution is heated to 75～95 ℃ again, is made into ammonium oxalate.
Among this step S2, reaction end liquid is when being added with the solidliquid mixture of cobalt oxalate crystal, after in this reaction end liquid, adding ammonium oxalate and cobalt salt solution, in the process of oxalic cobalt precipitation, this cobalt oxalate precipitation can be grown at the cobalt oxalate plane of crystal as crystal seed, like this, more be conducive to the generation of cobalt oxalate precipitation, and obtain relatively large cobalt oxalate precipitation crystal, further shorten the time of reaction, thereby improved formation efficiency and reduced energy consumption.
Among this step S2, the mensuration of the D50 particle diameter of cobalt oxalate can adopt online detection, has reached the variation of the particle diameter of timely monitoring cobalt oxalate.
Among above-mentioned large particle diameter cobalt powder preparation method's the step S3, the mode that the mode of Separation of Solid and Liquid preferably adopts plate and frame filter press to filter.Dry preferred employing flash dryer is also carried out fragmentation, or preferably adopts baking oven in 150 ℃ of lower bakings fragmentation in 10 hours.The D50 that obtains the cobalt oxalate presoma that obtains after the fragmentation＞50 μ m.Before drying is processed, can also wash the resulting solid of Separation of Solid and Liquid, the mode of washing preferably adopts the hot pure water more than 70 ℃ to wash, until the pH value of last washings reaches till about 7.0, the purpose of washing is away impurity that solid adheres to, and has reached the purpose of purifying cobalt oxalate presoma.
Among above-mentioned large particle diameter cobalt powder preparation method's the step S4, the temperature that the cobalt oxalate presoma is reduced is preferably 400～500 ℃, and the time is preferably 1～4 hour, and the gas of reduction is preferably hydrogen-nitrogen mixture gas.In this hydrogen-nitrogen mixture gas, the volume ratio of hydrogen and nitrogen is preferably 1: 0.1～and 0.3, this preferred reducing condition can more effectively be reduced into cobalt powder with cobalt oxalate, and shortens the recovery time, reduces energy consumption.The fragmentation of this step can be adopted the mode such as turbine fragmentation or shearing-crushing.
The embodiment of the invention also provides a kind of large particle diameter cobalt powder, and this large particle diameter cobalt powder is prepared by above-mentioned large particle diameter cobalt powder preparation method.The FSSS of this large particle diameter cobalt powder is preferably more than or equals 1.0 μ m, is less than or equal to 1.8 μ m; Its D50 is preferably 20～30 μ m.This large particle diameter cobalt powder particle diameter is even, and impurity is few, and purity is high, and particle diameter is relatively large, has satisfied in the industry the diversified demand of cobalt powder, as has satisfied the specific alloy such as high temperature alloy with the requirement of cobalt powders.
Below illustrate large particle diameter cobalt powder preparation method by a plurality of embodiment, and the aspect such as large particle diameter cobalt powder performance.
Embodiment 1
A kind of large particle diameter cobalt powder, its preparation method is as follows:
(1): preparation contains liquid at the bottom of the reaction of cobalt oxalate crystal: add the cobalt oxalate crystal in 65 ℃ water, the quality percentage composition of cobalt oxalate crystal is 50%;
(2): add the cobalt salt solution of ammonium oxalate and cobalt chloride at the bottom of the described reaction in the liquid, react under 75 ℃, oxalic cobalt precipitation when the D50 particle diameter for the treatment of described cobalt oxalate reaches 60 μ m, stops reaction and carried out ripening 1 hour at 70 ℃; Wherein, the weight ratio of ammonium oxalate and chlorination cobalt salt is 0.3: 1, and the pH value is controlled to be 0.8 ± 0.1;
(3): will carry out through the cobalt oxalate of ripening plate and frame filter press and filter, flash dryer, fragmentation obtains the cobalt oxalate presoma; This cobalt oxalate presoma D50 is 60 μ m;
(4): 400 ℃ of reduction 4 hours, fragmentation obtained described large particle diameter cobalt powder with the cobalt oxalate presoma.
The FSSS of the large particle diameter cobalt powder of present embodiment 1 preparation is 1.5 μ m, and the D50 of this large particle diameter cobalt powder is 20.0 μ m.
Embodiment 2
A kind of large particle diameter cobalt powder, its preparation method is as follows:
(1): reaction end liquid is provided, and liquid is 75 ℃ of water at the bottom of this reaction;
(2): the ammonium oxalate preparation method: in the oxalic acid dissolved water, filter, being mixed with concentration is the 200g/L oxalic acid solution, adds liquefied ammonia in oxalic acid solution, and pH value 1.0, oxalic acid solution is heated to 95 ℃ again, is made into ammonium oxalate;
(3): add the cobalt salt solution of ammonium oxalate and cobalt acetate at the bottom of the described reaction in the liquid, react under 85 ℃, oxalic cobalt precipitation when the D50 particle diameter for the treatment of described cobalt oxalate reaches 60 μ m, stops reaction and carried out ripening 4 hours at 85 ℃; Wherein, the mol ratio of ammonium oxalate and acetic acid cobalt salt is 1: 0.6, and the pH value is controlled to be 0.6 ± 0.1;
(4): will carry out through the cobalt oxalate of ripening plate and frame filter press and filter, and with 70 ℃ hot pure water washing, wash to wash water pH value 7.0, the usefulness baking oven dries by the fire 10 hours dryings, fragmentation at 150 ℃ again, obtains the cobalt oxalate presoma; This cobalt oxalate presoma D50 is 90 μ m;
(5): 500 ℃ of reduction 1 hour, fragmentation obtained described large particle diameter cobalt powder with the cobalt oxalate presoma.
The FSSS of the large particle diameter cobalt powder of present embodiment 2 preparations is 1.6 μ m, and its D50 is 25 μ m.
Embodiment 3
A kind of large particle diameter cobalt powder, its preparation method is as follows:
(1): preparation contains liquid at the bottom of the reaction of cobalt oxalate crystal: add the cobalt oxalate crystal in 70 ℃ water, the quality percentage composition of cobalt oxalate crystal is 30%;
(2): the ammonium oxalate preparation method: in the oxalic acid dissolved water, filter, being mixed with concentration is the 150g/L oxalic acid solution, adds liquefied ammonia in oxalic acid solution, and the pH value is transferred to 1.0, oxalic acid solution is heated to 85 ℃ again, is made into ammonium oxalate;
(3): add the cobalt salt solution of ammonium oxalate and cobaltous sulfate at the bottom of the described reaction in the liquid, react under 90 ℃, oxalic cobalt precipitation when the D50 particle diameter for the treatment of described cobalt oxalate reaches 60 μ m, stops reaction and carried out ripening 3 hours at 85 ℃; Wherein, the weight ratio of ammonium oxalate and sulfuric acid cobalt salt is 0.2: 1, and the pH value is controlled to be 0.9 ± 0.1;
(4): will carry out through the cobalt oxalate of ripening plate and frame filter press and filter, and with 80 ℃ hot pure water washing, wash to wash water pH value 7.0, the usefulness baking oven dries by the fire 10 hours dryings, fragmentation at 150 ℃ again, obtains the cobalt oxalate presoma; This cobalt oxalate presoma D50 is 75 μ m;
(5): at 450 ℃ of reductase 12s hour, fragmentation obtains described large particle diameter cobalt powder with the cobalt oxalate presoma.
The FSSS of the large particle diameter cobalt powder of present embodiment 3 preparations is 1.3 μ m, and its D50 is 26.1 μ m.
By above-described embodiment 1 to embodiment 3 as can be known, the large particle diameter cobalt powder of embodiment of the invention preparation method technique is simple, easily control, and cost is low, is fit to suitability for industrialized production.This large particle diameter cobalt powder preparation method passes through to the selection of reactant with to the control of temperature with the reaction termination condition, and acquisition cobalt oxalate presoma cobalt oxalate particle diameter is large, purity is high, good dispersion.The cobalt powder purity that obtains with this large particle diameter cobalt powder preparation method is high, and particle diameter is even, and the D50 particle diameter is relatively large, and the D50 particle diameter is 20～30 μ m, has satisfied in the industry the diversified demand of cobalt powder.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a large particle diameter cobalt powder preparation method comprises the steps:
Reaction end liquid is provided, and liquid is the solidliquid mixture that is added with the cobalt oxalate crystal in 65～75 ℃ of water or the water at the bottom of the described reaction;
Add ammonium oxalate and cobalt salt solution at the bottom of the described reaction in the liquid, react under 75～95 ℃, oxalic cobalt precipitation when the D50 particle diameter for the treatment of described cobalt oxalate reaches 60 μ m, stops reaction and carries out ripening;
To carry out Separation of Solid and Liquid through the described cobalt oxalate of ripening, drying, fragmentation obtains the cobalt oxalate presoma;
With described cobalt oxalate presoma reduction, fragmentation obtains described large particle diameter cobalt powder.
2. large particle diameter cobalt powder preparation method according to claim 1, it is characterized in that: the mol ratio of described ammonium oxalate and cobalt salt is 1: 0.5～0.8.
3. large particle diameter cobalt powder preparation method according to claim 1 is characterized in that: in the described oxalic cobalt precipitation reaction step, add that the pH value of liquid is adjusted to 0.5～1.0 at the bottom of ammonium oxalate and the cobalt salt solution afterreaction.
4. large particle diameter cobalt powder preparation method according to claim 1 is characterized in that: in the described solidliquid mixture that is added with the cobalt oxalate crystal, the quality percentage composition of described cobalt oxalate crystal is 20～50%.
5. large particle diameter cobalt powder preparation method according to claim 1 is characterized in that: described cobalt salt is at least a in cobalt chloride, cobaltous sulfate, cobalt nitrate, the cobalt acetate; The concentration of described cobalt salt solution is 50～120g/L.
6. large particle diameter cobalt powder preparation method according to claim 1, it is characterized in that: the temperature of described ripening is 60～90 ℃, the time is 1～4 hour.
7. large particle diameter cobalt powder preparation method according to claim 1, it is characterized in that: the temperature of described reduction is 400～500 ℃, the time is 1～4 hour.
8. large particle diameter cobalt powder preparation method according to claim 1, it is characterized in that: described ammonium oxalate method preparation: in the oxalic acid dissolved water, filter, being mixed with concentration is 100～200g/L oxalic acid solution, oxalic acid solution is heated to 75～95 ℃ again, then in oxalic acid solution, add liquefied ammonia, and adjust pH is 1.0～4.5, is made into ammonium oxalate.
9. large particle diameter cobalt powder, it is characterized in that: described large particle diameter cobalt powder is prepared by the claims 1 to 8 arbitrary described large particle diameter cobalt powder preparation method.
10. large particle diameter cobalt powder according to claim 9 is characterized in that: the FSSS of described large particle diameter cobalt powder is less than or equal to 1.8 μ m for more than or equal to 1.0 μ m; The D50 of described large particle diameter cobalt powder is 20～30 μ m.
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| CN104478700A (en) * | 2014-12-09 | 2015-04-01 | 英德佳纳金属科技有限公司 | Large-particle size cobalt oxalate and preparation method thereof |
| 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 |
| CN110899718A (en) * | 2018-09-14 | 2020-03-24 | 上海铁路通信有限公司 | Preparation method of large-particle-size cobalt particles with shell-core structures |
| CN112195350A (en) * | 2020-08-19 | 2021-01-08 | 衢州华友钴新材料有限公司 | Preparation method of coarse particle cobalt cluster |
| CN112355318A (en) * | 2020-10-21 | 2021-02-12 | 荆楚理工学院 | Large-particle-size porous spherical nickel powder and preparation method thereof |
| JP2022500564A (en) * | 2018-09-21 | 2022-01-04 | 河南科技大学 | Tungsten Alloy Precursor Composite Powder Preparation Method, Ceramic Alumina Reinforced Tungsten Alloy and Its Manufacturing Method |
| CN115229176A (en) * | 2022-06-17 | 2022-10-25 | 北京科技大学 | Preparation method of sphere-like cobalt oxalate particles |
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| CN104478700A (en) * | 2014-12-09 | 2015-04-01 | 英德佳纳金属科技有限公司 | Large-particle size cobalt oxalate and preparation method thereof |
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| JP2022500564A (en) * | 2018-09-21 | 2022-01-04 | 河南科技大学 | Tungsten Alloy Precursor Composite Powder Preparation Method, Ceramic Alumina Reinforced Tungsten Alloy and Its Manufacturing Method |
| JP7104450B2 (en) | 2018-09-21 | 2022-07-21 | 河南科技大学 | Tungsten Alloy Precursor Composite Powder Preparation Method and Ceramic Alumina Reinforced Tungsten Alloy Manufacturing Method |
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| CN112355318A (en) * | 2020-10-21 | 2021-02-12 | 荆楚理工学院 | Large-particle-size porous spherical nickel powder and preparation method thereof |
| CN112355318B (en) * | 2020-10-21 | 2023-05-19 | 荆楚理工学院 | Large-particle-size porous spherical nickel powder and preparation method thereof |
| CN115229176A (en) * | 2022-06-17 | 2022-10-25 | 北京科技大学 | Preparation method of sphere-like cobalt oxalate particles |
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