CN103537711B - A kind of preparation method of spherical submicron cobalt powder - Google Patents
A kind of preparation method of spherical submicron cobalt powder Download PDFInfo
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Abstract
The present invention discloses the preparation method of a kind of spherical submicron cobalt powder, and this preparation method includes step: make the step of complex cobalt saline solution: stir soluble in water to cobalt salt and surfactant, adds chelating agent and carries out mixing, reacting to described cobalt salt solution；Make the step of reducing agent solvent: dissolve reduce agent in water；Heating complex cobalt saline solution, adds alkali in complex cobalt saline solution and makes it be alkalescence；Then reducing agent solvent and complex cobalt saline solution are mixed, obtain submicron cobalt powder filter cake through solid-liquid separation, the impurity in filter cake is removed in washing；Filter cake absolute ethanol washing after washing removes moisture；Submicron cobalt powder filter cake after absolute ethanol washing obtains spherical submicron cobalt powder after removing ethanol and micro-moisture by vacuum drying.Use spherical submicron cobalt powder narrow particle size distribution that the present invention makes, oxygen content is low, particle uniformity and dispersibility more preferable.
Description
Technical field
The present invention relates to super-fine material preparing technical field, in particular, relate to the preparation method of a kind of spherical submicron cobalt powder.
Background technology
Super-fine cobalt powder, due to its special physics, chemical property, shows many excellent performances in the application in the fields such as hard alloy, battery, catalyst, magnetic material, absorbing material, pottery.Scientific practice proves, when material is machined into the trickleest size, can produce skin effect, bulk effect and quantum effect, cause the change of physical property and chemical property.
Along with the development of science and technology, the requirement of dusty material performance is improved constantly by different applications, in the preparation of ultra-fine cemented carbide, it is desirable to cobalt powder Fisher particle size is less than 0.8um, just can obtain more preferable serviceability.The preparation method of super-fine cobalt powder is a lot, common are cobalt oxide, cobalt oxalate and cobalt carbonate hydrogen reduction method, cobalt oxalate thermal dissociation method, microemulsion method, polyhydric alcohol cobalt salt reducing process etc., but the preparation method and technology of the most domestic super-fine cobalt powder taked is all more complicated and highly energy-consuming, relatively costly, and the cobalt powder Relative Size obtained is relatively thick, purity is the highest, it is impossible to intactly embody the excellent properties of super-fine cobalt powder.In the various preparation methoies of superfine metal cobalt powder, due to it quickly, efficiently, particle size, pattern, character are easily-controllable, and technique is simple, with low cost for liquid phase reduction, be suitable to the advantages, the most always study hotspot of super-fine cobalt powder synthetic method such as industrialization large-scale production.The wherein super-fine cobalt powder excellent performance of hydrazine hydrate cobalt salt reduction preparation, granularity can reach nanoscale or submicron order, and preparation process is simple, the impurity introduced is few, it it is the reliable method being prepared cobalt powder by cobalt salt chemical reduction method, avoid cobalt oxalate, cobalt carbonate, cobalt oxide hydrogen reduction method cause cobalt burning owing to temperature is too high during preparing cobalt powder, harden, really up to the mark after coming out of the stove, it is difficult to be dispersed into the shortcomings such as powdery.
The chemism of cobalt powder is good, is susceptible to oxidation reaction；And cobalt powder has magnetic, easily attract each other between granule.The most prepared submicron cobalt powder most of particle size distribution width, oxygen content height, particle uniformity and poor dispersion.
Summary of the invention
The technical problem to be solved is to provide that a kind of narrow particle size distribution, oxygen content be low, particle uniformity and the preparation method of dispersibility more preferable spherical submicron cobalt powder.
It is an object of the invention to be achieved through the following technical solutions:
A kind of preparation method of spherical submicron cobalt powder, including
Make the step of complex cobalt saline solution: stir soluble in water to cobalt salt and surfactant, add chelating agent and carry out mixing, reacting to described cobalt salt solution；
Make the step of reducing agent solvent: dissolve reduce agent in water；
Heating complex cobalt saline solution, adds alkali in complex cobalt saline solution and makes it be alkalescence；Then reducing agent solvent and complex cobalt saline solution are mixed, obtain submicron cobalt powder filter cake through solid-liquid separation, the impurity in filter cake is removed in washing；Filter cake absolute ethanol washing after washing removes moisture；Submicron cobalt powder filter cake after absolute ethanol washing obtains spherical submicron cobalt powder after removing ethanol and micro-moisture by vacuum drying.
Further, in described complex cobalt saline solution, the concentration of cobalt salt is 0.1～2.0 mol/L, and the concentration of surfactant is 1.0～60g/L；Chelating agent is 0.05～1.0:1 with the mol ratio of cobalt salt；
In described reducing agent solvent, the concentration of reducing agent is 0.4～8.0
mol/L；
Complex cobalt saline solution being heated to 50～80 DEG C, makes the pH value of described complex cobalt saline solution adjust to 11～13 with alkali, be subsequently adding described reducing agent solvent and form mixed solution, wherein complex cobalt saline solution is 3:1～1:3 with the volume ratio of reducing agent solvent；Mixed solution temperature is maintained at 50～80 DEG C of reactions 30～60min, carries out solid-liquid separation, obtain described submicron cobalt powder filter cake after being subsequently cooled to 10～30 DEG C；
Submicron cobalt powder filter cake after absolute ethanol washing is obtained spherical submicron cobalt powder at the dry removing ethanol of vacuum 40～70 DEG C and micro-moisture.
Further, in complex cobalt saline solution, cobalt salt concentration is 0.5～1.5 mol/L, and the concentration of surfactant is 10.0～40.0g/L, and chelating agent is 0.1～0.8:1 with the mol ratio of cobalt salt, and pH value is 11.5～12.5；Reducing agent solvent strength is 1.0～6.0 mol/L；Complex cobalt saline solution is 2:1～1:2 with the volume ratio of reducing agent solvent.
Further, the method for cooling is for add water in mixed solution；Solid-liquid separation uses vacuum to filter or centrifugal.
Further, described cobalt salt is CoSO4、CoCl2Or Co (NO3)2In any one；
Further, any one during described surfactant is polyvinylpyrrolidone (PVP), polyacrylic acid (PAA), Polyethylene Glycol (PEG) or polyvinyl alcohol (PVA).
Further, any one during described chelating agent is ammonia, disodiumedetate or ethylenediamine.
Further, described reducing agent is sodium borohydride or potassium borohydride and any one in the mixture of hydrazine hydrate.
Further, described alkali is sodium hydroxide or potassium hydroxide, and its concentration is 2.0～10.0
mol/L。
Further, feed time is 30～60min；The mean diameter of spherical submicron cobalt powder is 500～700nm.
Due to the fact that the present invention provide a kind of can the technology of continuous large-scale production spherical submicron cobalt powder rapidly, the submicron cobalt powder properties of product prepared are stable, reliable in quality, uniform particle sizes, good dispersion, crystallization is high, purity is high, its chemical composition, physical property are superior to country's super-fine cobalt powder quality standard grade, can meet the requirement to high-performance superfine cobalt powder of the current new high-tech product.Submicron cobalt powder prepared by the present invention has fully spherical shape structure, epigranular, and particle mean size is 500-700nm；This cobalt powder can be widely applied to the industries such as superhard alloy material, high temperature alloy, battery.Generally prepare super-fine cobalt powder with hydrazine hydrate as reducing agent, response speed is slow, percent reduction is low, and carrys out Substitute For Partial hydrazine hydrate with the stronger sodium borohydride of reproducibility or potassium borohydride in the present invention, has both significantly improved reaction rate, and react fully thoroughly, reduce again the consumption of reducing agent, improve production efficiency, reduce production cost, and prepared cobalt powder purity is high, has wide practical use in industrial circle.Use complexation-homogeneous phase reduction method to generate submicron cobalt powder, make the generation of nucleus and growth separate, pattern and the granularity of submicron cobalt powder can be controlled, make the degree of crystallinity of spherical submicron cobalt powder improve.The preparation method of the present invention is simple and easy to control, and equipment is simple, and energy consumption is low, and safety is good, and the quality of production is stable, efficiency is high, the cycle is short, low cost, and production scale can arbitrarily expand.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the preparation method of embodiment of the present invention spherical submicron cobalt powder.
Detailed description of the invention
Seeing Fig. 1, the present invention discloses the preparation method of a kind of spherical submicron cobalt powder, including step:
Make the step of complex cobalt saline solution: stir soluble in water to cobalt salt and surfactant, add chelating agent and carry out mixing, reacting to described cobalt salt solution；
Make the step of reducing agent solvent: dissolve reduce agent in water；
Heating complex cobalt saline solution, adds alkali in complex cobalt saline solution and makes it be alkalescence；Then reducing agent solvent and complex cobalt saline solution are mixed, obtain submicron cobalt powder filter cake through solid-liquid separation, the impurity in filter cake is removed in washing；Filter cake absolute ethanol washing after washing removes moisture；Submicron cobalt powder filter cake after absolute ethanol washing obtains spherical submicron cobalt powder after removing ethanol and micro-moisture by vacuum drying.
Further, in complex cobalt saline solution, the concentration of cobalt salt is 0.1～2.0 mol/L, and the concentration of surfactant is 1.0～60g/L；Chelating agent is 0.05～1.0:1 with the mol ratio of cobalt salt；In reducing agent solvent, the concentration of reducing agent is 0.4～8.0 mol/L；Complex cobalt saline solution being heated to 50～80 DEG C, makes the pH value of described complex cobalt saline solution adjust to 11～13 with alkali, be subsequently adding described reducing agent solvent and form mixed solution, wherein complex cobalt saline solution is 3:1～1:3 with the volume ratio of reducing agent solvent；Mixed solution temperature is maintained at 50～80 DEG C of reactions 30～60min, carries out solid-liquid separation, obtain described submicron cobalt powder filter cake after being subsequently cooled to 10～30 DEG C, and the method for cooling is for add water in mixed solution；Solid-liquid separation uses vacuum to filter or centrifugal.
In complex cobalt saline solution, cobalt salt concentration is 0.5～1.5 mol/L, and the concentration of surfactant is 10.0～40.0g/L, and chelating agent is 0.1～0.8:1 with the mol ratio of cobalt salt, and pH value is 11.5～12.5；Reducing agent solvent strength is 1.0～6.0 mol/L；Complex cobalt saline solution is 2:1～1:2 with the volume ratio of reducing agent solvent.
Submicron cobalt powder filter cake after absolute ethanol washing is obtained spherical submicron cobalt powder at the dry removing ethanol of vacuum 40～70 DEG C and micro-moisture.
The method of cooling is for add water in mixed solution；Solid-liquid separation uses vacuum to filter or centrifugal.
Cobalt salt can select CoSO4、CoCl2Or Co (NO3)2；Surfactant can select polyvinylpyrrolidone (PVP), polyacrylic acid (PAA), Polyethylene Glycol (PEG) or polyvinyl alcohol (PVA)；Chelating agent can select ammonia, disodiumedetate or ethylenediamine.
Reducing agent can select the mixture of sodium borohydride or potassium borohydride and hydrazine hydrate.
Alkali can select sodium hydroxide or potassium hydroxide, and its concentration is 2.0～10.0
mol/L。
Feed time is 30～60min；The mean diameter of spherical submicron cobalt powder is 500～700nm.
Due to the fact that the present invention provide a kind of can the technology of continuous large-scale production spherical submicron cobalt powder rapidly, the submicron cobalt powder properties of product prepared are stable, reliable in quality, uniform particle sizes, good dispersion, crystallization is high, purity is high, its chemical composition, physical property are superior to country's super-fine cobalt powder quality standard grade, can meet the requirement to high-performance superfine cobalt powder of the current new high-tech product.Submicron cobalt powder prepared by the present invention has fully spherical shape structure, epigranular, and particle mean size is 500-700nm；This cobalt powder can be widely applied to the industries such as superhard alloy material, high temperature alloy, battery.Generally prepare super-fine cobalt powder with hydrazine hydrate as reducing agent, response speed is slow, percent reduction is low, and carrys out Substitute For Partial hydrazine hydrate with the stronger sodium borohydride of reproducibility or potassium borohydride in the present invention, has both significantly improved reaction rate, and react fully thoroughly, reduce again the consumption of reducing agent, improve production efficiency, reduce production cost, and prepared cobalt powder purity is high, has wide practical use in industrial circle.Use complexation-homogeneous phase reduction method to generate submicron cobalt powder, make the generation of nucleus and growth separate, pattern and the granularity of submicron cobalt powder can be controlled, make the degree of crystallinity of spherical submicron cobalt powder improve.The preparation method of the present invention is simple and easy to control, and equipment is simple, and energy consumption is low, and safety is good, and the quality of production is stable, efficiency is high, the cycle is short, low cost, and production scale can arbitrarily expand.
The invention will be further described with preferred embodiment below in conjunction with the accompanying drawings.
Embodiment 1:
A kind of preparation method of submicron cobalt powder, including:
By 0.225 mol CoCl2Uniform mixing soluble in water with 4.5gPVP, is subsequently adding 0.135mol ammonia and is sufficiently stirred for obtaining 450ml complex cobalt saline solution；By 0.43
molN2H4·H2O and 0.02 mol sodium borohydride mix and soluble in water obtain 450ml reducing agent solvent；
Complex cobalt saline solution is heated to 80 DEG C, with the sodium hydroxide solution of 6.0mol/L, complex cobalt saline solution pH value is adjusted to 12.0, then reducing agent solvent is added complex cobalt saline solution, feed time is 30min, temperature of reaction system maintains 80 DEG C of reaction 40min, is subsequently adding cold water and is cooled to room temperature (10～30 DEG C)；Product being performing centrifugal separation on, filter cake impurity in filter cake is removed in washing, by Wastewater Concentrated；Filter cake absolute ethanol washing after washing removes moisture, is reclaimed by dehydrated alcohol；Cobalt powder filter cake after absolute ethanol washing is obtained spherical submicron cobalt powder at 40 DEG C of vacuum removing ethanol and micro-moisture.
Embodiment 2:
A kind of preparation method of submicron cobalt powder, including:
By 0.35 mol CoSO4Uniform mixing soluble in water with 7.0gPVA, is subsequently adding 0.175mol ethylenediamine and is sufficiently stirred for obtaining 350ml complex cobalt saline solution；By 1.65 molN2H4·H2O、0.01
Mol potassium borohydride mixes and soluble in water obtains 550ml reducing agent solvent；
Complex cobalt saline solution is heated to 60 DEG C, with the potassium hydroxide sodium solution of 2.0mol/L, complex cobalt saline solution pH value is adjusted to 11.5, then reducing agent solvent is added complex cobalt saline solution, feed time is 50min, temperature of reaction system maintains 60 DEG C of reaction 50min, is subsequently adding cold water and is cooled to room temperature (10～30 DEG C)；Product being performing centrifugal separation on, filter cake impurity in filter cake is removed in washing, by Wastewater Concentrated；Filter cake absolute ethanol washing after washing removes moisture, is reclaimed by dehydrated alcohol；Cobalt powder filter cake after absolute ethanol washing is obtained spherical submicron cobalt powder at 70 DEG C of vacuum removing ethanol and micro-moisture.
Embodiment 3:
A kind of preparation method of submicron cobalt powder, including:
By 0.45 mol Co (NO3)2Uniform mixing soluble in water with 12.0gPEG, is subsequently adding 0.045mol disodiumedetate and is sufficiently stirred for obtaining 300ml complex cobalt saline solution；By 1.2 molN2H4·H2O、0.03
Mol potassium borohydride mixes and soluble in water obtains 600ml reducing agent solvent；
Complex cobalt saline solution is heated to 70 DEG C, with the sodium hydroxide solution of 10.0mol/L, complex cobalt saline solution pH value is adjusted to 11.5, then reducing agent solvent is added complex cobalt saline solution, feed time is 60min, temperature of reaction system maintains 70 DEG C of reaction 30min, is subsequently adding cold water and is cooled to room temperature (10～30 DEG C)；Product being performing centrifugal separation on, filter cake impurity in filter cake is removed in washing, by Wastewater Concentrated；Filter cake absolute ethanol washing after washing removes moisture, is reclaimed by dehydrated alcohol；Cobalt powder filter cake after absolute ethanol washing is obtained spherical submicron cobalt powder at 60 DEG C of vacuum removing ethanol and micro-moisture.
Embodiment 4:
A kind of preparation method of submicron cobalt powder, including:
By 0.60 mol CoCl2Uniform mixing soluble in water with 6.0gPVA, is subsequently adding 0.48mol ammonia and is sufficiently stirred for obtaining 600ml complex cobalt saline solution；By 1.77
molN2H4·H2O, 0.03 mol sodium borohydride mix and soluble in water obtain 300ml reducing agent solvent；
Complex cobalt saline solution is heated to 50 DEG C, with the potassium hydroxide sodium solution of 8.0mol/L, complex cobalt saline solution pH value is adjusted to 12.5, then reducing agent solvent is added complex cobalt saline solution, feed time is 40min, temperature of reaction system maintains 50 DEG C of reaction 60min, is subsequently adding cold water and is cooled to room temperature (10～30 DEG C)；Product being performing centrifugal separation on, filter cake impurity in filter cake is removed in washing, by Wastewater Concentrated；Filter cake absolute ethanol washing after washing removes moisture, is reclaimed by dehydrated alcohol；Cobalt powder filter cake after absolute ethanol washing is obtained spherical submicron cobalt powder at 50 DEG C of vacuum removing ethanol and micro-moisture.
Embodiment 5:
A kind of preparation method of submicron cobalt powder, including:
By 0.45 mol CoSO4Uniform mixing soluble in water with 10.5gPAA, is subsequently adding 0.135mol ethylenediamine and is sufficiently stirred for obtaining 350ml complex cobalt saline solution；By 2.2 molN2H4·H2O、0.02
Mol sodium borohydride mixes and soluble in water obtains 550ml reducing agent solvent；
Complex cobalt saline solution is heated to 80 DEG C, with the sodium hydroxide solution of 5.0mol/L, complex cobalt saline solution pH value is adjusted to 12.0, then reducing agent solvent is added complex cobalt saline solution, feed time is 50min, temperature of reaction system maintains 80 DEG C of reaction 30min, is subsequently adding cold water and is cooled to room temperature (10～30 DEG C)；Product being performing centrifugal separation on, filter cake impurity in filter cake is removed in washing, by Wastewater Concentrated；Filter cake absolute ethanol washing after washing removes moisture, is reclaimed by dehydrated alcohol；Cobalt powder filter cake after absolute ethanol washing is obtained spherical submicron cobalt powder at 40 DEG C of vacuum removing ethanol and micro-moisture.
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert the present invention be embodied as be confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, it is also possible to make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Claims (5)
1. the preparation method of a spherical submicron cobalt powder, it is characterised in that include step:
Make the step of complex cobalt saline solution: stir soluble in water to cobalt salt and surfactant, add chelating agent and carry out mixing, reacting to described cobalt salt solution；
Make the step of reducing agent solvent: dissolve reduce agent in water；
Heating complex cobalt saline solution, adds alkali in complex cobalt saline solution and makes it be alkalescence；Then reducing agent solvent and complex cobalt saline solution are mixed, obtain submicron cobalt powder filter cake through solid-liquid separation, the impurity in filter cake is removed in washing；Filter cake absolute ethanol washing after washing removes moisture；Submicron cobalt powder filter cake after absolute ethanol washing obtains spherical submicron cobalt powder after removing ethanol and micro-moisture by vacuum drying；
Described chelating agent is any one in ammonia, disodiumedetate or ethylenediamine, described surfactant is any one in polyvinylpyrrolidone (PVP), polyacrylic acid (PAA), Polyethylene Glycol (PEG) or polyvinyl alcohol (PVA), and described reducing agent is any one in the mixture of sodium borohydride or potassium borohydride and hydrazine hydrate;
In described complex cobalt saline solution, in complex cobalt saline solution, cobalt salt concentration is 0.5～1.5mol/L, and the concentration of surfactant is 10.0～40.0g/L, and chelating agent is 0.1～0.8:1 with the mol ratio of cobalt salt；Reducing agent solvent strength is 1.0～6.0mol/L；
Complex cobalt saline solution being heated to 60～80 DEG C, makes with alkali the pH value of described complex cobalt saline solution adjust most 11.5～12.5, be subsequently adding described reducing agent solvent and form mixed solution, wherein complex cobalt saline solution is 2:1～1:2 with the volume ratio of reducing agent solvent；Mixed solution temperature is maintained at 60～80 DEG C of reactions 30～60min, carries out solid-liquid separation, obtain described submicron cobalt powder filter cake after being subsequently cooled to 10～30 DEG C；
Submicron cobalt powder filter cake after absolute ethanol washing is obtained spherical submicron cobalt powder at the dry removing ethanol of vacuum 40～70 DEG C and micro-moisture.
2. the preparation method of spherical submicron cobalt powder as claimed in claim 1, it is characterised in that the method for cooling is for add water in mixed solution；Solid-liquid separation uses vacuum to filter or centrifugal.
3. the preparation method of the spherical submicron cobalt powder as described in as arbitrary in claim 1～2, it is characterised in that described cobalt salt is CoSO4、CoCl2Or Co (NO3)2In any one.
4. the preparation method of the spherical submicron cobalt powder as described in as arbitrary in claim 1～2, it is characterised in that described alkali is sodium hydroxide or potassium hydroxide, and its concentration is 2.0～10.0mol/L.
5. the preparation method of the spherical submicron cobalt powder as described in as arbitrary in claim 1～2, it is characterised in that feed time is 30～60min；The mean diameter of spherical submicron cobalt powder is 500～700nm.
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| CN113059179B (en) * | 2021-03-17 | 2022-06-03 | 电子科技大学 | Preparation method of magnetic cobalt particles |
| CN113500203A (en) * | 2021-06-23 | 2021-10-15 | 安徽寒锐新材料有限公司 | Preparation process of nano cobalt powder |
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| JP2005220380A (en) * | 2004-02-03 | 2005-08-18 | Dowa Mining Co Ltd | Silver powder and manufacturing method therefor |
| CN101875130A (en) * | 2009-12-08 | 2010-11-03 | 华中科技大学 | Method for preparing nano silver particles |
| CN101890504A (en) * | 2010-07-07 | 2010-11-24 | 江苏技术师范学院 | Method for preparing flaky nano copper powder |
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Denomination of invention: A preparation method of spherical submicron cobalt powder Effective date of registration: 20220308 Granted publication date: 20160914 Pledgee: Bank of Jiangsu Limited by Share Ltd. Wuxi science and Technology Branch Pledgor: YUCHEN ADVANCED ENERGY MATERIALS & TECHNOLOGY WUXI Co.,Ltd. Registration number: Y2022990000132 |