CN106629870A - Preparation method of small-particle size spherical cobalt carbonate - Google Patents
Preparation method of small-particle size spherical cobalt carbonate Download PDFInfo
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- CN106629870A CN106629870A CN201611066226.7A CN201611066226A CN106629870A CN 106629870 A CN106629870 A CN 106629870A CN 201611066226 A CN201611066226 A CN 201611066226A CN 106629870 A CN106629870 A CN 106629870A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/06—Carbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of small-particle size spherical cobalt carbonate. The preparation method comprises the following specific steps: 1, converging cobalt salt and an ammonium bicarbonate solution, adding into a reaction kettle for reacting, controlling the pH value in the reaction process so as to adjust the pH value of a system after half an hour to 7.0+/-0.1; 2, further converging and adding the cobalt salt and an ammonium bicarbonate solution, keeping the pH in the step 1, continuing reacting for 2h, and precipitating; 3, performing solid-liquid separation and drying the solution after precipitation in the step 2 to obtain the small-particle size spherical cobalt carbonate. By the preparation method, through process control over the pH value, nucleation among cobalt carbonate particles and the uniformity of a growth condition are maintained, so that the isotropy of precipitates and the solution are achieved, and thus on the basis of the nucleation, the spherical cobalt carbonate is formed through outward, uniform and spherical growth. In addition, the preparation method is low in process cost and easy to popularize.
Description
Technical field
The invention belongs to metal powder material fabricating technology field, and in particular to a kind of small particle spherical cobaltous carbonate
Preparation method.
Background technology
Cobalt carbonate as a kind of important industrial chemicals and material precursor, be widely used in ceramic industry colouring agent,
The dressing agent of mining industry, the catalyst of organic industry, hard alloy and battery material presoma etc..Wherein in terms of materials application
Such as Processes of Cobalt Powders For Hard Alloys presoma and cobaltosic oxide precursor to the particle diameter of cobalt carbonate, pattern and every physical index all
Require, the development trend in both fields be all it is spherical under the conditions of small one and large one particle diameter two kinds of particles, respectively correspond to ball
The microns bulky grain of shape 20 and the short grained presoma of spherical 2-5 microns, the former commercial processes are ripe, and the latter is can industry
Do not have substantially in the change, preparation method of low cost, i.e., little particle cobalt carbonate it is gentle and under conditions of low cost hardly into
It is spherical.
The content of the invention
It is an object of the invention to provide a kind of preparation method of small particle spherical cobaltous carbonate, by process control pH value, solution
Existing method of having determined prepares problem of the small particle spherical cobaltous carbonate in gentle, can be under Industrialized conditions not balling-up.
The technical solution adopted in the present invention is that a kind of preparation method of small particle spherical cobaltous carbonate is specifically included following
Step：
Step 1, adds reactor to be reacted cobalt salt and ammonium bicarbonate solution cocurrent, controls course of reaction pH value so that half
System pH is adjusted to 7.0 ± 0.1 after hour；
Step 2, continues cocurrent and adds cobalt salt and ammonium bicarbonate solution, keeps the pH value of step 1 constant, continues to react and precipitates；
Step 3, to the solution after step 2 precipitation separation of solid and liquid and drying are carried out, and obtain small particle spherical cobaltous carbonate.
Of the invention the characteristics of, also resides in,
Cobalt salt in the step 1 is the one kind in cobalt chloride, cobaltous sulfate, cobalt acetate.
The concentration of cobalt salt is 60-160g/l in the step 1, and flow is 1-5L/h.
PH value in the step 1 is adjusted according to the flow of carbon ammonium.
The concentration of carbon ammonium is 120-240g/l in the step 1.
The temperature reacted in the step 2 is 35-65 DEG C.
Stir speed (S.S.) in the step 2 is 50-220r/min.
Reaction time in the step 2 is 1-5h.
The invention has the beneficial effects as follows, a kind of preparation method of small particle spherical cobaltous carbonate of the invention, by process control
PH value, maintains the uniformity of nucleation between cobalt carbonate particle particle and growth conditions so that precipitation and solution isotropism,
So can the outwards growth of uniform and globulate on the basis of nucleation, form spherical cobaltous carbonate.In addition, the method
Process costs are low, it is easy to promote.
Description of the drawings
Fig. 1 provides the electron microscope that the cobalt carbonate prepared in embodiment 1 amplifies 500 times for the present invention；
Fig. 2 provides the electron microscope that the cobalt carbonate prepared in embodiment 1 amplifies 3000 times for the present invention；
Fig. 3 provides the electron microscope that the cobalt carbonate prepared in embodiment 2 amplifies 1000 times for the present invention；
Fig. 4 provides the electron microscope that the cobalt carbonate prepared in embodiment 2 amplifies 5000 times for the present invention；
Fig. 5 provides the electron microscope that the cobalt carbonate prepared in embodiment 3 amplifies 500 times for the present invention；
Fig. 6 provides the electron microscope that the cobalt carbonate prepared in embodiment 3 amplifies 5000 times for the present invention；
Fig. 7 provides the electron microscope that the cobalt carbonate prepared in contrast experiment amplifies 1000 times for the present invention；
Fig. 8 provides the electron microscope that the cobalt carbonate prepared in fullsized experiment amplifies 5000 times for the present invention；
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only to explain the present invention
Limit the present invention.
The embodiment of the present invention provides a kind of preparation method of small particle spherical cobaltous carbonate, specifically includes following steps：
Step 1, adds reactor to be reacted cobalt salt and ammonium bicarbonate solution cocurrent, controls course of reaction pH value so that half
System pH is adjusted to 7.0 ± 0.1 after hour；The cobalt salt be cobalt chloride, cobaltous sulfate, cobalt acetate in one kind, cobalt salt it is dense
Spend for 60-160g/l, flow is 1-5L/h；It is adjusted according to the flow of carbon ammonium；The concentration of carbon ammonium is 120-240g/l；
Step 2, continues cocurrent and adds cobalt salt and ammonium bicarbonate solution, keeps the pH value of step 1 constant, precipitates after reaction 2h；Instead
The temperature answered is 35-65 DEG C, and stir speed (S.S.) is 50-220r/min；
Step 3, to the solution after step 2 precipitation separation of solid and liquid and drying are carried out, and obtain small particle spherical cobaltous carbonate.
Compare compared with preparation method, the present invention mainly has following technical advantage：By process control pH value, carbon is maintained
The uniformity of nucleation and growth conditions between sour cobalt granule particle so that precipitation and solution isotropism, so can be
The outwards growth of uniform and globulate, forms spherical cobaltous carbonate on the basis of Jing nucleation.In addition, the method process costs are low, easily
In popularization.
Embodiment 1
It is the carbon ammonium hybrid reaction that the cobalt chloride and concentration of 120g/l are 220g/l by concentration, the flow of wherein cobalt chloride is
2.5L/h, the pH value of mixed solution is 7.015 after the flow of regulation carbon ammonium causes half an hour in course of reaction, keeps pH value not
Become and continue to show, stir at 40 DEG C, with the speed of 150r/min, precipitate after 2 hours of reaction, afterwards to the solution after precipitation
Separation of solid and liquid and drying are carried out, small particle spherical cobaltous carbonate is obtained, as shown in Figures 1 and 2.Wherein laser particle analyzer test D10For
18.572 μm, D50For 34.967 μm, D90For 50.655 μm, second particle Electronic Speculum size is between 3-5 μm, it may be possible to laser grain
In degree test process caused by the reunion of little spheric granules.
Embodiment 2
It is the carbon ammonium hybrid reaction that the cobalt chloride and concentration of 60g/l are 120g/l by concentration, the flow of wherein cobalt chloride is
1L/h, the flow of carbon ammonium is adjusted in course of reaction, and to cause the pH value of mixed solution after half an hour be 7.002, keep pH value constant after
Continuous reaction, stirs at 35 DEG C, with the speed of 220r/min, precipitates after 2 hours of reaction, and the solution after precipitation is carried out afterwards
Separation of solid and liquid and drying, obtain small particle spherical cobaltous carbonate, as shown in Figures 3 and 4.Wherein laser particle analyzer test D10For
9.582 μm, D50For 23.616 μm, D90For 44.681 μm, second particle Electronic Speculum size is between 3-5 μm, it may be possible to laser particle size
In test process caused by the reunion of little spheric granules.
Embodiment 3
It is the carbon ammonium hybrid reaction that the cobalt chloride and concentration of 160g/l are 240g/l by concentration, the flow of wherein cobalt chloride is
5L/h, the flow of carbon ammonium is adjusted in course of reaction, and to cause the pH value of mixed solution after half an hour be 7.096, keep pH value constant after
Continuous reaction, stirs at 65 DEG C, with the speed of 50r/min, precipitates after 2 hours of reaction, and the solution after precipitation is carried out afterwards
Separation of solid and liquid and drying, obtain small particle spherical cobaltous carbonate, as shown in Figures 5 and 6.Wherein laser particle analyzer test D10For
8.603 μm, D50For 19.409 μm, D90For 35.255 μm, second particle Electronic Speculum size is between 3-5 μm, it may be possible to laser particle size
In test process caused by the reunion of little spheric granules.
Contrast experiment：
It is the carbon ammonium hybrid reaction that the cobalt chloride and concentration of 120g/l are 220g/l by concentration, the flow of wherein cobalt chloride is
2.5L/h, the flow of carbon ammonium is 4.6L/h, and pH value is 7.15, is stirred at 40 DEG C, with the speed of 220r/min, and reaction 2 is little
When after precipitate, afterwards separation of solid and liquid and drying are carried out to the solution after precipitation, obtain small particle spherical cobaltous carbonate, such as Fig. 7 and Fig. 8
It is shown.Wherein D10For 4.401um, D50For 11.749um, D90For 23.252um.It can be seen that there is no process control pH
The cobalt carbonate dispersiveness being worth to and size distribution are poor, hardly balling-up.
The above, only presently preferred embodiments of the present invention is not intended to limit protection scope of the present invention.
Claims (8)
1. a kind of preparation method of small particle spherical cobaltous carbonate, it is characterised in that specifically implement according to following steps：
Step 1, adds reactor to be reacted cobalt salt and ammonium bicarbonate solution cocurrent, controls course of reaction pH value so that half an hour
Afterwards system pH is adjusted to 7.0 ± 0.1；
Step 2, continues cocurrent and adds cobalt salt and ammonium bicarbonate solution, keeps the pH value of step 1 constant, continues to react and precipitates；
Step 3, to the solution after step 2 precipitation separation of solid and liquid and drying are carried out, and obtain small particle spherical cobaltous carbonate.
2. a kind of preparation method of small particle spherical cobaltous carbonate according to claim 1, it is characterised in that the step 1
In cobalt salt be cobalt chloride, cobaltous sulfate, cobalt acetate in one kind.
3. a kind of preparation method of small particle spherical cobaltous carbonate according to claim 2, it is characterised in that the step 1
The concentration of middle cobalt salt is 60-160g/l, and flow is 1-5L/h.
4. a kind of preparation method of small particle spherical cobaltous carbonate according to claim 3, it is characterised in that the step 1
In pH value be adjusted according to the flow of carbon ammonium.
5. a kind of preparation method of small particle spherical cobaltous carbonate according to claim 4, it is characterised in that the step 1
The concentration of middle carbon ammonium is 120-240g/l.
6. a kind of preparation method of small particle spherical cobaltous carbonate according to claim 5, it is characterised in that the step 2
The temperature of middle reaction is 35-65 DEG C.
7. a kind of preparation method of small particle spherical cobaltous carbonate according to claim 6, it is characterised in that the step 2
In stir speed (S.S.) be 50-220r/min.
8. a kind of preparation method of small particle spherical cobaltous carbonate according to claim 7, it is characterised in that the step 2
In reaction time be 1-5h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110407257A (en) * | 2018-04-26 | 2019-11-05 | 荆门市格林美新材料有限公司 | A kind of preparation method of the small-particle-size cobalt carbonate of adulterated al |
| CN110540250A (en) * | 2018-05-28 | 2019-12-06 | 荆门市格林美新材料有限公司 | preparation method of aluminum-doped cobalt carbonate |
| CN110540248A (en) * | 2018-05-28 | 2019-12-06 | 荆门市格林美新材料有限公司 | Preparation method of small-particle-size cobalt oxide |
| CN112010357A (en) * | 2019-05-30 | 2020-12-01 | 荆门市格林美新材料有限公司 | Preparation method of small-particle-size and high-density cobalt carbonate |
| CN114873653A (en) * | 2022-05-11 | 2022-08-09 | 金驰能源材料有限公司 | Basic cobalt carbonate and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1693213A (en) * | 2005-05-16 | 2005-11-09 | 中南大学 | Process for preparing superfine cobalt oxide powder by booster parallel-flow precipitation |
| CN102583584A (en) * | 2012-03-27 | 2012-07-18 | 湖南雅城新材料发展有限公司 | Preparation method of spherical cobaltosic oxide |
| CN103771545A (en) * | 2012-10-17 | 2014-05-07 | 宇辰新能源材料科技无锡有限公司 | Preparation method of high-purity superfine spherical cobalt carbonate |
| CN104743613A (en) * | 2015-04-01 | 2015-07-01 | 浙江华友钴业股份有限公司 | Method for continuously preparing large-particle-size spherical cobalt carbonate |
| CN105731551A (en) * | 2014-12-09 | 2016-07-06 | 荆门市格林美新材料有限公司 | Doped cobalt carbonate, doped tricobalt tetroxide and preparation methods thereof |
| CN105800699A (en) * | 2016-04-20 | 2016-07-27 | 湖南海纳新材料有限公司 | Method for preparing high-sphericity-degree and large-particle cobaltosic oxide |
-
2016
- 2016-11-28 CN CN201611066226.7A patent/CN106629870B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1693213A (en) * | 2005-05-16 | 2005-11-09 | 中南大学 | Process for preparing superfine cobalt oxide powder by booster parallel-flow precipitation |
| CN102583584A (en) * | 2012-03-27 | 2012-07-18 | 湖南雅城新材料发展有限公司 | Preparation method of spherical cobaltosic oxide |
| CN103771545A (en) * | 2012-10-17 | 2014-05-07 | 宇辰新能源材料科技无锡有限公司 | Preparation method of high-purity superfine spherical cobalt carbonate |
| CN105731551A (en) * | 2014-12-09 | 2016-07-06 | 荆门市格林美新材料有限公司 | Doped cobalt carbonate, doped tricobalt tetroxide and preparation methods thereof |
| CN104743613A (en) * | 2015-04-01 | 2015-07-01 | 浙江华友钴业股份有限公司 | Method for continuously preparing large-particle-size spherical cobalt carbonate |
| CN105800699A (en) * | 2016-04-20 | 2016-07-27 | 湖南海纳新材料有限公司 | Method for preparing high-sphericity-degree and large-particle cobaltosic oxide |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110407257A (en) * | 2018-04-26 | 2019-11-05 | 荆门市格林美新材料有限公司 | A kind of preparation method of the small-particle-size cobalt carbonate of adulterated al |
| CN110540250A (en) * | 2018-05-28 | 2019-12-06 | 荆门市格林美新材料有限公司 | preparation method of aluminum-doped cobalt carbonate |
| CN110540248A (en) * | 2018-05-28 | 2019-12-06 | 荆门市格林美新材料有限公司 | Preparation method of small-particle-size cobalt oxide |
| CN112010357A (en) * | 2019-05-30 | 2020-12-01 | 荆门市格林美新材料有限公司 | Preparation method of small-particle-size and high-density cobalt carbonate |
| CN112010357B (en) * | 2019-05-30 | 2023-11-07 | 荆门市格林美新材料有限公司 | Preparation method of small-particle-size high-density cobalt carbonate |
| CN114873653A (en) * | 2022-05-11 | 2022-08-09 | 金驰能源材料有限公司 | Basic cobalt carbonate and preparation method thereof |
| CN114873653B (en) * | 2022-05-11 | 2023-10-13 | 金驰能源材料有限公司 | Basic cobalt carbonate and preparation method thereof |
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| CN106629870B (en) | 2018-11-06 |
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