CN107150127A - The preparation method of spherical cobalt powder - Google Patents
The preparation method of spherical cobalt powder Download PDFInfo
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- CN107150127A CN107150127A CN201610122181.4A CN201610122181A CN107150127A CN 107150127 A CN107150127 A CN 107150127A CN 201610122181 A CN201610122181 A CN 201610122181A CN 107150127 A CN107150127 A CN 107150127A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
The present invention relates to cobalt technical field of material, a kind of preparation method of spherical cobalt powder is specifically disclosed.Methods described at least comprises the following steps:Step S01. mixes cobalt salt solution and precipitant solution cocurrent, carries out precipitation reaction;Step S01 is reacted the sediment obtained and carries out dynamic roasting by step S02. under oxidizing atmosphere;Under reducing atmosphere, the step S02 products obtained are calcined by step S03.;Wherein, the dynamic roasting temperature is 400~800 DEG C, 4~8h of roasting time.The spherical cobalt powder that the present invention is obtained has that purity height, good dispersion, particle are small, epigranular is controllable, good sphericity, the features such as regular appearance;The inventive method is suitable for industrialization large-scale production nodularization cobalt powder material.
Description
Technical field
The present invention relates to cobalt technical field of material, more particularly to a kind of preparation method of spherical cobalt powder.
Background technology
Cobalt powder has excellent physical property and chemical property because of it, and is widely used in hard alloy and electricity
In the industries such as pond material.Regardless of whether be cemented carbide industry or battery material industry, purity to cobalt powder,
Dispersiveness and the physical state such as surface topography have strict requirements, if cobalt powder purity is not high, dispersiveness is bad or
Person's pattern is in dendroid or strip, then can influence the mechanical performance of hard alloy to a certain extent and use the longevity
Life.
At present, the method that super-fine cobalt powder is prepared both at home and abroad is relatively more, mainly have polyol reduction method, electrolysis,
Precipitation-thermal dissociation method, hydrogen reduction method etc..Wherein, hydrogen reduction method due to technological process it is relatively easy, it is relatively suitable
Industrialized production is closed, one of main method of domestic production cobalt powder is had become, but at present prepared by this method
Cobalt powder, its pattern is in mainly dendroid or corynebacterium, and sphericity is poor.And due to precursor to hydrogen also
The granule-morphology of former cobalt powder has large effect, that is, precursor pattern has necessarily with cobalt powder morphology
Inheritance.Therefore, researcher both domestic and external expands many researchs to the precursor of hydrogen reduction method.
The patent of invention of Application No. 200710075929.0 discloses a kind of manufacturing process of super-fine cobalt powder, should
Technique is specially:Cobalt carbonate first carries out high-energy ball milling, obtains ultra-fine carbonic acid cobalt precursor, then in reduction
Under the atmosphere of gas, reduction prepares superfine spherical cobalt powder.But this grinding technique, is readily incorporated miscellaneous
Matter, influences the quality of cobalt powder.
And for example the patent of invention of Application No. 201010196228.4 discloses a kind of system of near-spherical aggregation cobalt powder
Preparation Method.This method adds reactor generation presoma using ammonium hydrogen carbonate as precipitating reagent with cobalt salt solution cocurrent,
Then the cobalt carbonate of acquisition is placed in progress thermal decomposition hydrogen reduction in reduction furnace, so as to obtain near-spherical aggregation
Cobalt powder.
This method focuses on to control the generation of precursor, and the control to reduction process is not fine, obtained cobalt powder
Spheroidization effect is not very good.
The content of the invention
Not good, the problems such as spheroidization is undesirable, the mesh of the embodiment of the present invention for above-mentioned pattern in the prior art
Be the provision of a kind of preparation method of spherical cobalt powder.
In order to reach foregoing invention purpose, the embodiment of the present invention employs following technical scheme:
A kind of preparation method of spherical cobalt powder, at least comprises the following steps:
Step S01. mixes cobalt salt solution and precipitant solution cocurrent, carries out precipitation reaction;
Step S01 is reacted the sediment obtained and carries out dynamic roasting by step S02. under oxidizing atmosphere;
Under reducing atmosphere, the step S02 products obtained are calcined by step S03.;
Wherein, the dynamic roasting temperature is 400~800 DEG C, 4~8h of roasting time.
The preparation method for the spherical cobalt powder that the above embodiment of the present invention is provided, dynamic roasting is mutually tied with hydrogen reduction
Close, it is not necessary to add any surfactant, only dynamic roasting can obtain the preceding body with good fluidity
Body (Co3O4), provide the precursor with good fluidity, the cobalt finally obtained so as to be calcined for hydrogen reduction
Powder has that good dispersion, particle are small, epigranular is controllable, nodularization degree is high, regular appearance the features such as.
Brief description of the drawings
Technical scheme in order to illustrate the embodiments of the present invention more clearly, below will be to required in embodiment
The accompanying drawing used is briefly described, it should be apparent that, drawings in the following description are only the one of the present invention
A little embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, also
Other accompanying drawings can be obtained according to these accompanying drawings.
Fig. 1 is the process chart of the preparation method of spherical cobalt powder provided in an embodiment of the present invention;
Fig. 2 is the Co of the preparation method preparation for the spherical cobalt powder that the embodiment of the present invention 1 is provided3O4SEM
Figure.
Fig. 3 is the cobalt powder SEM figures of the preparation method preparation for the spherical cobalt powder that the embodiment of the present invention 1 is provided.
Fig. 4 is the Co of the preparation method preparation for the spherical cobalt powder that the embodiment of the present invention 2 is provided3O4SEM
Figure.
Fig. 5 is the cobalt powder SEM figures of the preparation method preparation for the spherical cobalt powder that the embodiment of the present invention 2 is provided.
Fig. 6 is the Co of the preparation method preparation for the spherical cobalt powder that the embodiment of the present invention 3 is provided3O4SEM
Figure.
Fig. 7 is the cobalt powder SEM figures of the preparation method preparation for the spherical cobalt powder that the embodiment of the present invention 3 is provided.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, below in conjunction with accompanying drawing and reality
Example is applied, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only
Only to explain the present invention, it is not intended to limit the present invention.
The embodiment of the present invention provides the preparation method for planting spherical cobalt powder one by one, at least comprises the following steps:
Step S01. mixes cobalt salt solution and precipitant solution cocurrent, carries out precipitation reaction;
Step S01 is reacted the sediment obtained and carries out dynamic roasting by step S02. under oxidizing atmosphere;
Under reducing atmosphere, the step S02 products obtained are calcined by step S03.;
Wherein, the dynamic roasting temperature is 400~800 DEG C, 4~8h of roasting time.
In a preferred embodiment, above-mentioned steps S01 consersion unit is reactor.Due to reactor certainly
Band mixing plant, and mixing speed uniform, controllable, Quick uniform mixing can be realized to reaction mixture and is kept away
The generation for exempting from bulky grain precursor plays an important roll.In embodiments of the present invention, the mixing speed is controlled to be
150~250rpm.
In a preferred embodiment, cobalt salt and precipitating reagent are 1 according to mass ratio:(1.5~2.0) are added, control
Precipitating reagent processed is somewhat excessive, is conducive to complexing and the cobalt carbonate nucleation of cobalt salt.
In a preferred embodiment, cobalt salt is configured to the cobalt salt solution that concentration is 80~120g/L, sunk simultaneously
Shallow lake agent is configured to the precipitant solution that concentration is 180~250g/L.
In a preferred embodiment, precipitating reagent uses ammonium hydrogen carbonate, mainly due to the precipitating reagent of this type,
Gas is eventually resolved into without introducing impurity, the purity of product will not be had undesirable effect.
Preferably, cobalt salt is cobalt chloride, and this mainly considers that chlorion is easily cleaned after reaction, and is difficult
Go other materials to react, impurity will not be introduced.
In a preferred embodiment, step S01 reaction need to be maintained in the range of 40~55 DEG C, can be obvious
The chemism of reactant is improved, reaction rate is improved.
In whole reaction, the pH of reaction mixture has certain shadow to realizing for the technology of the present invention effect
Ring.Therefore, the embodiment of the present invention reaction when, it is necessary to pH value be adjusted 6.98~7.30, so as to reach control
The association rate of cobalt salt and precipitating reagent processed.
In any one embodiment, to ensure that the precursor cobaltosic oxide obtained has good mobility,
During dynamic roasting, need it is Methodistic preheated, predecomposition, the product that step S01 is obtained
It is placed in the equipment such as fluidized bed furnace, fluidized bed furnace or rotary kiln, and moves, decomposes under the air-flow flowed in stove,
So as to reach the effect of modification precursor cobaltosic oxide pattern simultaneously so that precursor cobaltosic oxide has
Good dispersiveness.Here air flow is the air-flow with oxidisability, specially air or oxygen.
In a preferred embodiment, the temperature of calcining is 350~550 DEG C, and calcination time is 1~4h, also Primordial Qi
Cobaltosic oxide thoroughly can be reduced to cobalt powder by atmosphere in the calcining heat and calcination time.
In the embodiment of the present invention, terminate in above-mentioned steps S01 reactions, in addition to reaction product cobalt carbonate is entered
The step of row centrifugation or filtration washing, drying process.
The preparation method of spherical cobalt powder provided in an embodiment of the present invention, it is not necessary to add any surfactant,
And using ammonium hydrogen carbonate as precipitating reagent, other any impurities are not introduced in product, it is often more important that, before reduction
Dynamic roasting process is added, the sphericity of precursor is optimized, the scrambling of powder is reduced so that
Prepared precursor powder morphology is regular, and sphericity is high, uniform particle diameter, final to be reduced by precursor
Obtained cobalt powder shows that purity height, good dispersion, particle are small, epigranular is controllable, good sphericity, shape
The features such as looks are regular.At the same time, this is simple for process, can be using continous way production, production efficiency
Height, and the stability of product batches quality is can guarantee that, it is adapted to large-scale industrial production.
Further, the cobalt powder material of the preparation method synthesis of spherical cobalt powder provided in an embodiment of the present invention, can
Applied in lithium ion battery or hard alloy field.
In order to preferably embody the preparation method of spherical cobalt powder provided in an embodiment of the present invention, below by multiple
Embodiment is further illustrated.
Embodiment 1
(1) ammonium bicarbonate soln that configuration concentration is 80g/L cobalt chloride solution, concentration are 180g/L;
(2) it is 2 times of cobalt chloride consumption by ammonium hydrogen carbonate consumption, by ammonium bicarbonate soln and cobalt chloride solution simultaneously
Stream is added in reactor, is warming up to 45 DEG C;
(3) stirred under 200rpm mixing speed, and keep reaction temperature to be 45 DEG C, pH value is 7.0~7.1,
2h is reacted, superfine spherical Cobalt carbonate sediment is obtained;
(4) superfine spherical cobalt carbonate is centrifuged, washed and dried, then moved under oxygen atmosphere
State is calcined, and sintering temperature is 400 DEG C, is calcined 8h, obtains the precursor Co of black3O4Superfine powder.Through
Detection, the precursor Co that the present embodiment 1 is obtained3O4In superfine powder, its granularity≤1.0 μm.And to obtaining
Co3O4Superfine powder carries out SEM scannings, and scanning result is as shown in Figure of description 2;
(5) by the Co of acquisition3O4Superfine powder is placed in reducing atmosphere hydrogen, with 420 DEG C of calcining 2h, is obtained
Granularity is scanned in 0.5 μm or so of superfine spherical cobalt powder through SEM, and its pattern is as shown in Figure 3.
Embodiment 2
(1) ammonium bicarbonate soln that configuration concentration is 100g/L cobalt chloride solution, concentration are 200g/L;
(2) by 1.5 times that ammonium hydrogen carbonate consumption is cobalt chloride consumption, by ammonium bicarbonate soln and cobalt chloride solution
Cocurrent is added in reactor, is warming up to 50 DEG C;
(3) stirred under 250rpm mixing speed, and keep reaction temperature to be 50 DEG C, pH value is 7.1~7.2,
3h is reacted, superfine spherical Cobalt carbonate sediment is obtained;
(4) superfine spherical cobalt carbonate is centrifuged, washed and dried, then moved under oxygen atmosphere
State is calcined, and sintering temperature is 800 DEG C, is calcined 4h, obtains the precursor Co of black3O4Superfine powder.Through
Detection, the precursor Co that the present embodiment 2 is obtained3O4In superfine powder, its granularity≤1.0 μm.And to obtaining
Co3O4Superfine powder carries out SEM scannings, and scanning result is as shown in Figure of description 4;
(5) by the Co of acquisition3O4Superfine powder is placed in reducing atmosphere hydrogen, with 420 DEG C of calcining 2h, is obtained
Granularity is scanned in 0.5 μm or so of superfine spherical cobalt powder through SEM, and its pattern is as shown in Figure 5.
Embodiment 3
(1) ammonium bicarbonate soln that configuration concentration is 120g/L cobalt chloride solution, concentration are 220g/L;
(2) by 1.8 times that ammonium hydrogen carbonate consumption is cobalt chloride consumption, by ammonium bicarbonate soln and cobalt chloride solution
Cocurrent is added in reactor, is warming up to 40 DEG C;
(3) stirred under 150rpm mixing speed, and keep reaction temperature to be 40 DEG C, pH value is 7.2~7.3,
3h is reacted, superfine spherical Cobalt carbonate sediment is obtained;
(4) superfine spherical cobalt carbonate is centrifuged, washed and dried, then moved under oxygen atmosphere
State is calcined, and sintering temperature is 550 DEG C, is calcined 7h, obtains the precursor Co of black3O4Superfine powder.Through
Detection, the precursor Co that the present embodiment 3 is obtained3O4In superfine powder, its granularity≤1.0 μm.And to obtaining
Co3O4Superfine powder carries out SEM scannings, and scanning result is as shown in Figure of description 6;
(5) by the Co of acquisition3O4Superfine powder is placed in reducing atmosphere hydrogen, with 52 DEG C of calcining 2h, is obtained
Granularity is scanned in 0.5 μm or so of superfine spherical cobalt powder through SEM, and its pattern is as shown in Figure 7.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in this hair
Any modification, equivalent substitution or improvement made within bright spirit and principle etc., should be included in the present invention
Protection domain within.
Claims (10)
1. a kind of preparation method of spherical cobalt powder, at least comprises the following steps:
Step S01. mixes cobalt salt solution and precipitant solution cocurrent, carries out precipitation reaction;
Step S01 is reacted the sediment obtained and carries out dynamic roasting by step S02. under oxidizing atmosphere;
Under reducing atmosphere, the step S02 products obtained are calcined by step S03.;
Wherein, the dynamic roasting temperature is 400~800 DEG C, 4~8h of roasting time.
2. the preparation method of spherical cobalt powder as claimed in claim 1, it is characterised in that:The cobalt salt and institute
The mass ratio for stating precipitating reagent is 1:(1.5~2.0).
3. the preparation method of the spherical cobalt powder as described in claim 1-2 is any, it is characterised in that:It is described heavy
The temperature reacted of forming sediment is 40~55 DEG C.
4. the preparation method of the spherical cobalt powder as described in claim 1-2 is any, it is characterised in that:It is described anti-
The pH value of solution is answered to control 6.98~7.30.
5. the preparation method of the spherical cobalt powder as described in claim 1-2 is any, it is characterised in that:It is described anti-
It is 2~3h between seasonable.
6. the preparation method of the spherical cobalt powder as described in claim 1-2 is any, it is characterised in that:It is described anti-
During answering, the step of being also accompanied by stir process, the mixing speed of the stir process is 150~250rpm.
7. the preparation method of the spherical cobalt powder as described in claim 1-2 is any, it is characterised in that:It is described heavy
Shallow lake agent is ammonium hydrogen carbonate.
8. the preparation method method of the spherical cobalt powder as described in claim 1-2 is any, it is characterised in that:It is described
Oxidizing atmosphere is air or oxygen.
9. the preparation method of the spherical cobalt powder as described in claim 1-2 is any, it is characterised in that:It is described to forge
It is 350~550 DEG C to burn temperature, and/or the calcination time is 1~4h.
10. the preparation method of the spherical cobalt powder as described in claim 1-2 is any, it is characterised in that:The cobalt
The concentration of salting liquid is 80~120g/L, and/or the concentration of the precipitating reagent is 180~250g/L.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109550972A (en) * | 2019-01-22 | 2019-04-02 | 宇辰新能源材料科技无锡有限公司 | A kind of preparation method of high temperature cemented carbide cobalt powder |
CN109622988A (en) * | 2019-01-22 | 2019-04-16 | 宇辰新能源材料科技无锡有限公司 | A kind of preparation method of anticorrosive Processes of Cobalt Powders For Hard Alloys |
CN110935886A (en) * | 2018-09-21 | 2020-03-31 | 荆门市格林美新材料有限公司 | Class C60Preparation method of type cobalt powder |
CN111702184A (en) * | 2020-06-30 | 2020-09-25 | 荆门市格林美新材料有限公司 | Preparation method of large FSSS cobalt powder |
CN111842921A (en) * | 2019-04-25 | 2020-10-30 | 荆门市格林美新材料有限公司 | Preparation method of small FSSS high-apparent-density cobalt powder |
CN111922355A (en) * | 2020-06-30 | 2020-11-13 | 荆门市格林美新材料有限公司 | Preparation method of superfine cobalt powder |
CN112355317A (en) * | 2020-10-19 | 2021-02-12 | 衢州华友钴新材料有限公司 | Preparation method of superfine spherical cobalt powder |
CN112974823A (en) * | 2021-02-02 | 2021-06-18 | 安徽寒锐新材料有限公司 | Preparation method and preparation equipment of superfine spherical cobalt powder |
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CN110935886A (en) * | 2018-09-21 | 2020-03-31 | 荆门市格林美新材料有限公司 | Class C60Preparation method of type cobalt powder |
CN109550972A (en) * | 2019-01-22 | 2019-04-02 | 宇辰新能源材料科技无锡有限公司 | A kind of preparation method of high temperature cemented carbide cobalt powder |
CN109622988A (en) * | 2019-01-22 | 2019-04-16 | 宇辰新能源材料科技无锡有限公司 | A kind of preparation method of anticorrosive Processes of Cobalt Powders For Hard Alloys |
CN111842921A (en) * | 2019-04-25 | 2020-10-30 | 荆门市格林美新材料有限公司 | Preparation method of small FSSS high-apparent-density cobalt powder |
CN111702184A (en) * | 2020-06-30 | 2020-09-25 | 荆门市格林美新材料有限公司 | Preparation method of large FSSS cobalt powder |
CN111922355A (en) * | 2020-06-30 | 2020-11-13 | 荆门市格林美新材料有限公司 | Preparation method of superfine cobalt powder |
CN112355317A (en) * | 2020-10-19 | 2021-02-12 | 衢州华友钴新材料有限公司 | Preparation method of superfine spherical cobalt powder |
CN112974823A (en) * | 2021-02-02 | 2021-06-18 | 安徽寒锐新材料有限公司 | Preparation method and preparation equipment of superfine spherical cobalt powder |
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