CN104439283A - Method for preparing nanometer cobalt powder - Google Patents
Method for preparing nanometer cobalt powder Download PDFInfo
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- CN104439283A CN104439283A CN201410691976.8A CN201410691976A CN104439283A CN 104439283 A CN104439283 A CN 104439283A CN 201410691976 A CN201410691976 A CN 201410691976A CN 104439283 A CN104439283 A CN 104439283A
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Abstract
The invention relates to a method for preparing nanometer cobalt powder, and belongs to the field of metal smelting. The method includes the steps that (1) carbonyl cobalt raw materials, ethyl alcohol solvents and coating agents are evenly mixed according to the proportion of (1-10): (30-100): (1-20) to be injected into a high-pressure sealing container; (2) water heating is carried out on the mixture obtained in the step (1), the temperature is controlled to range from 50 DEG C to 150 DEG C, and the reaction time is controlled to range from 30 min to 60 min; (3) solutions obtained in the step (2) are cooled and filtered, and the obtained nanometer cobalt powder is washed with ethyl alcohol to be centrifuged in a low speed centrifuge, wherein the centrifuge speed is 2000 r/min; (4) vacuum drying is carried out on the nanometer cobalt powder obtained in the step (3) at the temperature ranging from 50 DEG C to 70 DEG C, and nanometer cobalt powder products with the particle sizes ranging from 5 nm to 100 nm are obtained. Compared with the prior art, the method has the advantages of being high in safety, high in production efficiency, simple in process and low in cost.
Description
Technical field
The invention belongs to metal smelt field, particularly a kind of method preparing cobalt powder.
Background technology
Cobalt is a kind of important ferrous metal, is widely used in alloy, Aeronautics and Astronautics, chemical industry, iron and steel, the fields such as electronics, plating, glass, dyeing, medicine, medical treatment and new material.Shear steel containing a certain amount of cobalt can significantly improve wearability and the cutting ability of steel; Stellite containing cobalt more than 50% has excellent high-temperature service performance; In Hardmetal materials, other metal carbides crystal grain combines by cobalt by alloy, makes the toughness that alloy tool is higher, and reduces the sensitive property to impacting; Because cobalt-base alloys defines the carbide of infusibility, therefore have good heat resistance, can be used for manufacturing high efficiency high-temperature engine; The structural material of aeroturbine uses the cobalt-base alloys containing chromium 20%-27%, and material can be made to improve non-oxidizability.In addition, cobalt is that magnetize once just can one of a few metals keeping magnetic.Magnetic steel containing 60% cobalt improves 2.5 times than the coercive force of general magnetic steel.Under vibration, general magnetic steel loses the magnetic of similar 1/3, and cobalt steels only loses the magnetic of 2%-3.5%.Thus the advantage of cobalt on magnetic material just clearly.
Nano-cobalt powder refers to that particle diameter is less than the metallic cobalt powder of 100nm.Nano-cobalt powder is owing to having great bulk effect and skin effect, and in physical property, chemism, electrical conductance, the aspects such as magnetic demonstrate many special natures, thus gathers around and has wide practical use.
Carbonyl cobalt has two kinds of existence forms, is respectively Co
2(CO)
8with HCo (CO)
4, wherein Co
2(CO)
8for orange crystal, fusing point 51 DEG C, to air-sensitive; HCo (CO)
4for yellow liquid, fusing point is-26 DEG C, decomposes more than fusing point, releases H
2.Use carbonyl cobalt can form cobalt-base alloys and the magnetic material containing cobalt for waste nano-cobalt powder in atomic level, therefore develop nano-cobalt powder and exploitation functional material or high-end cobalt-based products are extremely important.But, also do not utilize carbonyl cobalt to prepare the method for nano-cobalt powder for raw material at present.
So this area needs a kind of new technology badly to change such present situation.
Summary of the invention
Technical problem to be solved by this invention: for shortcomings and deficiencies of the prior art, the invention provides a kind of method preparing nano-cobalt powder that security is high, production efficiency is high, technique is simple, cost is low.
The present invention is design like this: a kind of method preparing nano-cobalt powder, is characterized in that: comprise the steps,
Step one, by carbonyl cobalt raw material, spirit solvent, covering according to (1 ~ 10): (30 ~ 100): the ratio of (1 ~ 20) mixes rear injection high pressure sealing container;
Step 2, the mixture Heating Water will obtained in step one, control temperature, at 50 DEG C ~ 150 DEG C, controls the reaction time at 30min ~ 60min;
Step 3, the solution cold filtration will obtained in step 2, centrifugal in low speed centrifuge after being washed by the nano-cobalt powder ethanol obtained, centrifugal speed is 2000r/min;
Step 4, by the nano-cobalt powder that obtains in step 3 in 50 DEG C ~ 70 DEG C vacuum drying, obtain the nano-cobalt powder product of granularity at 5nm ~ 100nm.
Carbonyl cobalt raw material in described step one is Co
2(CO)
8.
Covering in described step one is organosilan or organic siliconresin.
The maximum pressure-bearing of the high pressure sealing container in described step one is 5MPa.
High pressure sealing container in described step one is provided with seal, and the solution of described step one is joined in high pressure sealing container by seal.
Heating Water in described step 2 adopts system heating mode.
By above-mentioned design, the present invention can bring following beneficial effect:
1, a kind of material other low raw-material cost except carbonyl cobalt preparing the method employing of nano-cobalt powder of the present invention, compare the existing method preparing nano-cobalt powder, the present invention can provide the nano-cobalt powder of same quality with lower cost.
2, a kind of method preparing nano-cobalt powder of the present invention adopts Heating Water mode to prepare cobalt powder, and technique is simple, only needs high pressure sealing container to complete, do not need extra complexity or the equipment of danger, security is high, and cost is low, easy to operate, be easy to realize industrialization.
3, the covering that a kind of method preparing nano-cobalt powder of the present invention adopts is organosilan or organic siliconresin; when carbonyl cobalt is decomposed to form nano-cobalt powder, it is coated; bonding between powder can be stoped to grow up; form diaphragm and avoid oxidation; make the nano-cobalt powder product purity of production higher, production efficiency is high.
4, a kind of particle diameter preparing the nano-cobalt powder of the method for nano-cobalt powder of the present invention is determined by carbonyl cobalt concentration, reaction temperature, reaction time three aspect, direct proportionality, can by regulating ratio, reaction temperature, the reaction time regulation and control nano-cobalt powder granularity of carbonyl cobalt, production efficiency is high.
Detailed description of the invention
Prepare a method for nano-cobalt powder, it is characterized in that: comprise the steps,
Step one, by carbonyl cobalt raw material, spirit solvent, covering according to (1 ~ 10): (30 ~ 100): the ratio of (1 ~ 20) mixes rear injection high pressure sealing container;
Step 2, the mixture Heating Water will obtained in step one, control temperature, at 50 DEG C ~ 150 DEG C, controls the reaction time at 30min ~ 60min;
Step 3, the solution cold filtration will obtained in step 2, centrifugal in low speed centrifuge after being washed by the nano-cobalt powder ethanol obtained, centrifugal speed is 2000r/min;
Step 4, by the nano-cobalt powder that obtains in step 3 in 50 DEG C ~ 70 DEG C vacuum drying, obtain the nano-cobalt powder product of granularity at 5nm ~ 100nm.
Carbonyl cobalt raw material in described step one is Co
2(CO)
8.
Covering in described step one is organosilan or organic siliconresin.
The maximum pressure-bearing of the high pressure sealing container in described step one is 5MPa.
High pressure sealing container in described step one is provided with seal, and the solution of described step one is joined in high pressure sealing container by seal.
Heating Water in described step 2 adopts system heating mode.
Operation principle of the present invention is: 1, carbonyl cobalt, solvent and covering evenly dissolve each other; 2, under design temperature condition, carbonyl cobalt is decomposed into nano-cobalt powder and carbon monoxide; 3, it is completely coated that the nano-cobalt powder be decomposed to form is wrapped by agent, independent mutually each other, grows up even if collide with each other also can not bond; 4, the particle diameter of nano-cobalt powder is determined by carbonyl cobalt concentration, reaction temperature, reaction time three aspect, direct proportionality.
The present invention is raw material with carbonyl cobalt, take alcohol as solvent, with high pressure sealing container for reactor, adds organosilan or organic siliconresin as powder covering to stop Powder Oxidation and to grow up.
The solvent that the present invention uses is alcohol, and major function is dissolved and dilutes raw material and covering.
The covering that the present invention uses is organosilan or organic siliconresin, when carbonyl cobalt is decomposed to form nano-cobalt powder, it is coated, bonding between powder can be stoped to grow up, form diaphragm and avoid oxidation.
The reaction vessel that the present invention uses is high pressure sealing container, and the highest pressure-bearing 5MPa, with openable seal.This reactor can avoid alcohol to volatilize in course of reaction, stops nano-powder oxidized.
The present invention uses Heating Water for system heating mode, with keeping system stability.
For the present invention is described, spy provides following examples, and embodiments of the present invention are not limited to following examples.
Embodiment 1
Take carbonyl cobalt 1g, measure alcohol 50ml, measure silane 1ml, add in the lump in beaker to be stirred well to and dissolve completely.Mixed liquor is moved in high pressure sealing container, closing openings, put into Heating Water device.Setting reaction temperature is 75 DEG C, 30 minutes reaction time.By mixed solution cold filtration, centrifugal in 2000r/min after the nano-cobalt powder ethanol washing obtained.By nano-cobalt powder in 50 DEG C of vacuum drying, obtain the nano-cobalt powder product of granularity at 5nm ~ 10nm.
Embodiment 2
Take carbonyl cobalt 2g, measure alcohol 60ml, measure silane 2ml, add in the lump in beaker to be stirred well to and dissolve completely.Mixed liquor is moved in high pressure sealing container, closing openings, put into Heating Water device.Setting reaction temperature is 100 DEG C, 40 minutes reaction time.By mixed solution cold filtration, centrifugal in 2000r/min after the nano-cobalt powder ethanol washing obtained.By nano-cobalt powder in 60 DEG C of vacuum drying, obtain the nano-cobalt powder product of granularity at 10nm ~ 25nm.
Embodiment 3
Take carbonyl cobalt 5g, measure alcohol 70ml, measure silane 5ml, add in the lump in beaker to be stirred well to and dissolve completely.Mixed liquor is moved in high pressure sealing container, closing openings, put into Heating Water device.Setting reaction temperature is 125 DEG C, 45 minutes reaction time.By mixed solution cold filtration, centrifugal in 2000r/min after the nano-cobalt powder ethanol washing obtained.By nano-cobalt powder in 65 DEG C of vacuum drying, obtain the nano-cobalt powder product of granularity at 25nm ~ 50nm.
Embodiment 4
Take carbonyl cobalt 8g, measure alcohol 80ml, measure silane 8ml, add in the lump in beaker to be stirred well to and dissolve completely.Mixed liquor is moved in high pressure sealing container, closing openings, put into Heating Water device.Setting reaction temperature is 150 DEG C, 60 minutes reaction time.By mixed solution cold filtration, centrifugal in 2000r/min after the nano-cobalt powder ethanol washing obtained.By nano-cobalt powder in 55 DEG C of vacuum drying, obtain the nano-cobalt powder product of granularity at 50nm ~ 80nm.
Claims (6)
1. prepare a method for nano-cobalt powder, it is characterized in that: comprise the steps,
Step one, by carbonyl cobalt raw material, spirit solvent, covering according to (1 ~ 10): (30 ~ 100): the ratio of (1 ~ 20) mixes rear injection high pressure sealing container;
Step 2, the mixture Heating Water will obtained in step one, control temperature, at 50 DEG C ~ 150 DEG C, controls the reaction time at 30min ~ 60min;
Step 3, the solution cold filtration will obtained in step 2, centrifugal in low speed centrifuge after being washed by the nano-cobalt powder ethanol obtained, centrifugal speed is 2000r/min;
Step 4, by the nano-cobalt powder that obtains in step 3 in 50 DEG C ~ 70 DEG C vacuum drying, obtain the nano-cobalt powder product of granularity at 5nm ~ 100nm.
2. a kind of method preparing nano-cobalt powder according to claim 1, is characterized in that: the carbonyl cobalt raw material in described step one is Co
2(CO)
8.
3. a kind of method preparing nano-cobalt powder according to claim 1, is characterized in that: the covering in described step one is organosilan or organic siliconresin.
4. a kind of method preparing nano-cobalt powder according to claim 1, is characterized in that: the maximum pressure-bearing of the high pressure sealing container in described step one is 5MPa.
5. a kind of method preparing nano-cobalt powder according to claim 1, it is characterized in that: the high pressure sealing container in described step one is provided with seal, the solution of described step one is joined in high pressure sealing container by seal.
6. a kind of method preparing nano-cobalt powder according to claim 1, is characterized in that: the Heating Water in described step 2 adopts system heating mode.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410691976.8A CN104439283B (en) | 2014-11-26 | 2014-11-26 | A kind of method preparing nano-cobalt powder |
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|---|---|---|---|
| CN201410691976.8A CN104439283B (en) | 2014-11-26 | 2014-11-26 | A kind of method preparing nano-cobalt powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106563802A (en) * | 2015-10-08 | 2017-04-19 | 荆门市格林美新材料有限公司 | Granular coating cobalt powder preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006095002A1 (en) * | 2005-03-11 | 2006-09-14 | Institut Català D'investigació Química | Method for the one-pot preparation of stable nano-sized particles under mild conditions |
| JP4700374B2 (en) * | 2005-03-03 | 2011-06-15 | 学校法人東京理科大学 | Method for producing SmCo magnetic fine particles |
-
2014
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4700374B2 (en) * | 2005-03-03 | 2011-06-15 | 学校法人東京理科大学 | Method for producing SmCo magnetic fine particles |
| WO2006095002A1 (en) * | 2005-03-11 | 2006-09-14 | Institut Català D'investigació Química | Method for the one-pot preparation of stable nano-sized particles under mild conditions |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106563802A (en) * | 2015-10-08 | 2017-04-19 | 荆门市格林美新材料有限公司 | Granular coating cobalt powder preparation method |
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