CN107584137A - A kind of method that solwution method prepares metallic cobalt - Google Patents
A kind of method that solwution method prepares metallic cobalt Download PDFInfo
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- CN107584137A CN107584137A CN201710827432.3A CN201710827432A CN107584137A CN 107584137 A CN107584137 A CN 107584137A CN 201710827432 A CN201710827432 A CN 201710827432A CN 107584137 A CN107584137 A CN 107584137A
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- cobalt
- metallic cobalt
- mixed liquor
- ethylene glycol
- deionized water
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Abstract
The present invention discloses a kind of method that solwution method prepares metallic cobalt, it is that four hydration cobalt acetates are dissolved in the mixed liquor of ethylene glycol and deionized water composition, solution is transferred in autoclave, and closed reactor is put into the baking oven preheated in advance, then oven temperature is gradually heating to 200 DEG C~210 DEG C according to 2~5 DEG C/min of programming rate, and it is incubated 20~24 hours at such a temperature, question response terminates reactor and is cooled to room temperature, mixed liquor after filtration, washing and drying, produces metallic cobalt.Present invention process is simple, cost is low, and the product purity finally obtained is high.
Description
Technical field
The present invention relates to the preparation field of material powder, and in particular to a kind of method that solwution method prepares metallic cobalt.
Background technology
Metallic cobalt is a kind of important functional material, and it has excellent physicochemical property, is had in many fields important
Application.Metallic cobalt has excellent magnetic performance, therefore it has extensively in high-density storage media and Magnetic Memory device field
General application.In addition metallic cobalt is also widely used in high-strength high temperature-resistant alloy, Industrial Catalysis, function ceramics, battery etc.
Numerous areas.
At present, preparing the method for metallic cobalt has many kinds, such as oxide reducing process, electrolysis, liquid phase reduction.Oxidation
Thing reducing process is by the oxide of cobalt, reduces to obtain metallic cobalt with reducing substanceses such as hydrogen and carbon monoxide.Electrolysis is logical
The method of electrochemical reduction is crossed to obtain metallic cobalt, it is mostly dendritic or needle-like that electrolysis, which prepares metallic cobalt microscopic appearance,.Liquid phase
Reducing process is that the solid chemical compound of cobalt is scattered in a liquid, and liquid is usually polyalcohol (such as ethylene glycol) and liquid-phase reduction agent
Mixed liquor, be then heated to certain temperature so that compound occur reduction reaction obtain metallic cobalt.Compared to other
Method, liquid phase reduction simple production process is easy to operate, and raw materials for production form is varied, and product granularity can effectively adjust control
System.But generally requiring to add a variety of chemical reagent in the reaction solution system of conventional liquid phase reduction to complete, and cost is high,
Product purity is not high, and complex operation.
The content of the invention
For deficiency of the prior art, the present invention proposes a kind of method that solwution method prepares metallic cobalt, this method cost
It is low, and product purity is high, concrete technical scheme is as follows：
A kind of method that solwution method prepares metallic cobalt, is comprised the following steps that：
(1) four hydration cobalt acetates are dissolved in the mixed liquor of ethylene glycol and deionized water composition, stirring makes four hydration acetic acid
Cobalt is completely dissolved in mixed liquor；
(2) solution in step (1) is transferred in autoclave, filling rate is 60~75vol%, and will be closed
Reactor is put into be preheating in 140~150 DEG C of baking oven in advance, and oven temperature is gradual according to 2~5 DEG C/min of programming rate
200 DEG C~210 DEG C are warming up to, and is incubated 20~24 hours at such a temperature, question response terminates reactor and is cooled to room temperature, mixing
Liquid after filtration, washing and drying, produces metallic cobalt.
Further, the volume ratio of described ethylene glycol and deionized water is 10：0.9~10：1.1.
Further, mixed liquor dissolving 1~2g tetra- that every 100mL ethylene glycol and deionized water form is hydrated cobalt acetate.
Compared with the prior art, the present invention has the advantages that：
Compared to the liquid phase reduction (polyalcohol) of routine, the present invention only needs a kind of chemical reagent, i.e. cobalt acetate, so that it may
With in water and ethylene glycol mixed solution direct chemical reaction prepare metallic cobalt, source chemicals are simpler, easily grasp implement；And
Preparation temperature is low, less energy consumption, short preparation period, while product purity is high.
Brief description of the drawings
Fig. 1 is the XRD, digital figure and SEM photograph of the metallic cobalt prepared according to the method for embodiment 1；
Fig. 2 is the XRD spectrum of the metallic cobalt prepared according to the method for embodiment 2；
Fig. 3 is the SEM patterns of the metallic cobalt prepared according to the method for embodiment 2.
Embodiment
Embodiment 1
Weigh 0.6g tetra- to be hydrated in the mixed liquor that cobalt acetate is dissolved in 55mL ethylene glycol and 5mL deionized waters form, stirring makes
It is sufficiently mixed dissolving, and above-mentioned solution is transferred into the reactor that volume is 100mL, closed reactor is put into and preheated in advance
Baking oven is warming up to 200 DEG C into 140 DEG C of baking ovens, and by 2 DEG C/min of speed, then insulation 20 is small under the conditions of 200 DEG C
When；Question response terminates, and after reactor is cooled to room temperature, mixed liquor after filtration, washing and drying, produces metallic cobalt.Gained metal
Shown in (a) in the XRD spectrum such as Fig. 1 of cobalt, as can be seen from the figure product is the metallic cobalt of face-centered cubic and hexaplanar, is not had
There is the diffraction maximum of other impurities；Shown in (b) in digital photograph such as Fig. 1 and in SEM microscopic appearances such as Fig. 1 shown in (c)-(d).
Embodiment 2
Weigh 1.3g tetra- to be hydrated in the mixed liquor that cobalt acetate is dissolved in 60mL ethylene glycol and 6.6mL deionized waters form, stirring
It is sufficiently mixed dissolving, above-mentioned solution is transferred to the reactor that volume is 90mL, closed reactor is put into pre- in advance
Baking oven is warming up to 210 DEG C in 150 DEG C of baking oven by heat by 5 DEG C/min of speed, is then incubated 24 under the conditions of 210 DEG C
Hour；Question response terminates, and after reactor is cooled to room temperature, mixed liquor after filtration, washing and drying, produces metallic cobalt.Gained gold
Belong to the XRD spectrum of cobalt as shown in Fig. 2, as can be seen from the figure product is mainly the gold of face-centered cubic and a small amount of hexaplanar
Belong to cobalt, without the diffraction maximum of other impurities；The SEM patterns of gained metallic cobalt are as shown in Figure 3.
Claims (3)
1. a kind of method that solwution method prepares metallic cobalt, it is characterised in that it is comprised the following specific steps that：
(1) four hydration cobalt acetates are dissolved in the mixed liquor of ethylene glycol and deionized water composition, stirring fills four hydration cobalt acetates
Divide and be dissolved in mixed liquor.
(2) solution in step (1) being transferred in autoclave, filling rate is 60~75vol%, and by closed reaction
Kettle is put into be preheating in 140~150 DEG C of baking oven in advance, and oven temperature gradually heats up according to 2~5 DEG C/min of programming rate
To 200 DEG C~210 DEG C, and 20~24 hours are incubated at such a temperature, question response terminates reactor and is cooled to room temperature, mixed liquor warp
Filtering, washing, after drying, produce metallic cobalt.
2. the volume of the method that solwution method according to claim 1 prepares metallic cobalt, described ethylene glycol and deionized water
Than for 10：0.9~10：1.1.
3. the method that solwution method according to claim 1 or 2 prepares metallic cobalt, per 100mL ethylene glycol and deionized water group
Into mixed liquor dissolving 1~2g tetra- be hydrated cobalt acetate.
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| CN201710827432.3A CN107584137B (en) | 2017-09-14 | 2017-09-14 | Method for preparing metal cobalt by solution method |
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| CN201710827432.3A CN107584137B (en) | 2017-09-14 | 2017-09-14 | Method for preparing metal cobalt by solution method |
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| CN107584137B CN107584137B (en) | 2020-04-03 |
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Citations (8)
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| JPS5391054A (en) * | 1977-01-21 | 1978-08-10 | Hitachi Maxell | Metal cobalt powder manufacturing process |
| US4539041A (en) * | 1982-12-21 | 1985-09-03 | Universite Paris Vii | Process for the reduction of metallic compounds by polyols, and metallic powders obtained by this process |
| CN1891635A (en) * | 2005-07-08 | 2007-01-10 | 中南大学 | Method for preparing nano cobaltous oxide |
| CN101428348A (en) * | 2008-07-29 | 2009-05-13 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| CN102642029A (en) * | 2012-04-24 | 2012-08-22 | 同济大学 | Preparation method of FeNi-Ru alloy nanosphere |
| CN103170646A (en) * | 2013-03-29 | 2013-06-26 | 太原理工大学 | Synthetic method of nanometer materials of cobalt fractal structure |
| CN104625087A (en) * | 2015-02-28 | 2015-05-20 | 济宁利特纳米技术有限责任公司 | Method for hydrothermally manufacturing silver nanowires |
| CN105108170A (en) * | 2015-09-10 | 2015-12-02 | 兰州大学 | Method for manufacturing ultrafine nickle powder |
-
2017
- 2017-09-14 CN CN201710827432.3A patent/CN107584137B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5391054A (en) * | 1977-01-21 | 1978-08-10 | Hitachi Maxell | Metal cobalt powder manufacturing process |
| US4539041A (en) * | 1982-12-21 | 1985-09-03 | Universite Paris Vii | Process for the reduction of metallic compounds by polyols, and metallic powders obtained by this process |
| CN1891635A (en) * | 2005-07-08 | 2007-01-10 | 中南大学 | Method for preparing nano cobaltous oxide |
| CN101428348A (en) * | 2008-07-29 | 2009-05-13 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| CN102642029A (en) * | 2012-04-24 | 2012-08-22 | 同济大学 | Preparation method of FeNi-Ru alloy nanosphere |
| CN103170646A (en) * | 2013-03-29 | 2013-06-26 | 太原理工大学 | Synthetic method of nanometer materials of cobalt fractal structure |
| CN104625087A (en) * | 2015-02-28 | 2015-05-20 | 济宁利特纳米技术有限责任公司 | Method for hydrothermally manufacturing silver nanowires |
| CN105108170A (en) * | 2015-09-10 | 2015-12-02 | 兰州大学 | Method for manufacturing ultrafine nickle powder |
Non-Patent Citations (1)
| Title |
|---|
| REDDY,MP ET AL.: "A facile hydrothermal synthesis, characterization and magnetic properties of mesoporous CoFe2O4 nanospheres", 《JOURNAL OF MAGNETISM AND MAGNETIC MATERIALS》 * |
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