CN106629870B - A kind of preparation method of small particle spherical cobaltous carbonate - Google Patents
A kind of preparation method of small particle spherical cobaltous carbonate Download PDFInfo
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- CN106629870B CN106629870B CN201611066226.7A CN201611066226A CN106629870B CN 106629870 B CN106629870 B CN 106629870B CN 201611066226 A CN201611066226 A CN 201611066226A CN 106629870 B CN106629870 B CN 106629870B
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- cobaltous carbonate
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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)
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Abstract
The invention discloses a kind of preparation methods of small particle spherical cobaltous carbonate, specifically include following steps：Step 1, reaction kettle is added in cobalt salt and ammonium bicarbonate solution cocurrent to react, controls reaction process pH value so that system pH is adjusted to 7.0 ± 0.1 after half an hour；Step 2, continue cocurrent and cobalt salt and ammonium bicarbonate solution is added, keep the pH value of step 1 constant, precipitated after the reaction was continued 2h；Step 3, the solution after being precipitated to step 2 is separated by solid-liquid separation and is dried, and small particle spherical cobaltous carbonate is obtained.The present invention passes through process control pH value, maintain the uniformity of the nucleation and growth conditions between cobalt carbonate particle particle, so that precipitation and solution isotropism, can form spherical cobaltous carbonate on the basis of being nucleated outward uniformly and at spherical growth in this way.In addition, this method process costs are low, it is easy to spread.
Description
Technical field
The invention belongs to metal powder material fabricating technology fields, 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 colorant,
The dressing agent of mining industry, the catalyst of organic industry, hard alloy and battery material presoma etc..Wherein material application aspect
Such as Processes of Cobalt Powders For Hard Alloys presoma and cobaltosic oxide precursor to the grain size of cobalt carbonate, pattern and every physical index all
It requires, the development trend in the two field is all the two kinds of particles of small one and large one grain size under the conditions of spherical shape, corresponds to ball respectively
20 microns bulky grain of shape and 2-5 microns of short grained presomas of spherical shape, the former commercial processes maturation, the latter is can industry
Do not have substantially in preparation method change, at low cost, i.e., little particle cobalt carbonate under conditions of mild and at low cost hardly at
It is spherical.
Invention content
The object of the present invention is to provide a kind of preparation methods of small particle spherical cobaltous carbonate, pass through process control pH value, solution
Existing method of having determined prepares small particle spherical cobaltous carbonate mild, can be under Industrialized conditions the not balling-up the problem of.
The technical solution adopted in the present invention is that a kind of preparation method of small particle spherical cobaltous carbonate specifically includes following
Step：
Step 1, reaction kettle is added in cobalt salt and ammonium bicarbonate solution cocurrent to react, controls reaction process pH value so that half
System pH is adjusted to 7.0 ± 0.1 after hour；
Step 2, continue cocurrent and cobalt salt and ammonium bicarbonate solution is added, keep the pH value of step 1 constant, the reaction was continued and precipitates；
Step 3, the solution after being precipitated to step 2 is separated by solid-liquid separation and is dried, and small particle spherical cobaltous carbonate is obtained.
The features of the present invention also characterized in that
Cobalt salt in the step 1 is one kind in cobalt chloride, cobaltous sulfate, cobalt acetate.
A concentration of 60-160g/l of cobalt salt, flow 1-5L/h in the step 1.
PH value in the step 1 is adjusted according to the flow of ammonium bicarbonate.
A concentration of 120-240g/l of ammonium bicarbonate 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 advantages that a kind of preparation method of small particle spherical cobaltous carbonate of the present invention, passes through process control
PH value maintains the uniformity of the nucleation and growth conditions between cobalt carbonate particle particle so that precipitation and solution isotropism,
Spherical cobaltous carbonate can be formed on the basis of being nucleated outward uniformly and at spherical growth in this way.In addition, this method
Process costs are low, easy to spread.
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 implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
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, reaction kettle is added in cobalt salt and ammonium bicarbonate solution cocurrent to react, controls reaction process pH value so that half
System pH is adjusted to 7.0 ± 0.1 after hour；The cobalt salt is cobalt chloride, cobaltous sulfate, one kind in cobalt acetate, cobalt salt it is dense
Degree is 60-160g/l, flow 1-5L/h；It is adjusted according to the flow of ammonium bicarbonate；A concentration of 120-240g/l of ammonium bicarbonate；
Step 2, continue cocurrent and cobalt salt and ammonium bicarbonate solution is added, keep the pH value of step 1 constant, precipitated after reacting 2h；Instead
The temperature answered is 35-65 DEG C, stir speed (S.S.) 50-220r/min；
Step 3, the solution after being precipitated to step 2 is separated by solid-liquid separation and is dried, and small particle spherical cobaltous carbonate is obtained.
It is compared 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, it in this way can be
Through, outward uniformly and at spherical growth, forming spherical cobaltous carbonate on the basis of nucleation.In addition, this method process costs are low, easily
In popularization.
Embodiment 1
By the ammonium bicarbonate hybrid reaction of the cobalt chloride of a concentration of 120g/l and a concentration of 220g/l, the flow of wherein cobalt chloride is
2.5L/h, the flow that ammonium bicarbonate is adjusted in reaction process so that the pH value of mixed solution after half an hour is 7.015, keep pH value not
Change continues to show, and stirs, is precipitated after reacting 2 hours, later to the solution after precipitation at 40 DEG C, with the speed of 150r/min
It is separated by solid-liquid separation and is dried, obtain small particle spherical cobaltous carbonate, as shown in Figures 1 and 2.Wherein laser particle analyzer tests D10For
18.572 μm, D50It is 34.967 μm, D90It it is 50.655 μm, second particle Electronic Speculum size is between 3-5 μm, it may be possible to laser grain
It spends in test process caused by the reunion of small spheric granules.
Embodiment 2
By the ammonium bicarbonate hybrid reaction of the cobalt chloride of a concentration of 60g/l and a concentration of 120g/l, the flow of wherein cobalt chloride is
1L/h, the flow that ammonium bicarbonate is adjusted in reaction process so that the pH value of mixed solution after half an hour is 7.002, keep pH value constant after
Continuous reaction is stirred at 35 DEG C, with the speed of 220r/min, is precipitated after reacting 2 hours, carried out later to the solution after precipitation
It is separated by solid-liquid separation and dry, obtains small particle spherical cobaltous carbonate, as shown in Figures 3 and 4.Wherein laser particle analyzer tests D10For
9.582 μm, D50It is 23.616 μm, D90It it is 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 small spheric granules.
Embodiment 3
By the ammonium bicarbonate hybrid reaction of the cobalt chloride of a concentration of 160g/l and a concentration of 240g/l, the flow of wherein cobalt chloride is
5L/h, the flow that ammonium bicarbonate is adjusted in reaction process so that the pH value of mixed solution after half an hour is 7.096, keep pH value constant after
Continuous reaction is stirred at 65 DEG C, with the speed of 50r/min, is precipitated after reacting 2 hours, carried out later to the solution after precipitation
It is separated by solid-liquid separation and dry, obtains small particle spherical cobaltous carbonate, as shown in Figures 5 and 6.Wherein laser particle analyzer tests D10For
8.603 μm, D50It is 19.409 μm, D90It it is 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 small spheric granules.
Contrast experiment：
By the ammonium bicarbonate hybrid reaction of the cobalt chloride of a concentration of 120g/l and a concentration of 220g/l, the flow of wherein cobalt chloride is
The flow of 2.5L/h, ammonium bicarbonate are 4.6L/h, and pH value 7.15 stirs at 40 DEG C, with the speed of 220r/min, and reaction is 2 small
When after precipitate, the solution after precipitation is separated by solid-liquid separation and is dried later, obtains 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 from the figure that there is no process control pH
The cobalt carbonate dispersibility and size distribution being worth to are poor, hardly balling-up.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention.
Claims (5)
1. a kind of preparation method of small particle spherical cobaltous carbonate, which is characterized in that be specifically implemented according to the following steps：
Step 1, reaction kettle is added in cobalt salt and ammonium bicarbonate solution cocurrent to react, controls reaction process pH value so that half an hour
System pH is adjusted to 7.0 ± 0.1 afterwards；
Wherein, a concentration of 60-160g/l of cobalt salt, flow 1-5L/h, pH value are adjusted according to the flow of ammonium bicarbonate, ammonium bicarbonate
A concentration of 120-240g/l；
Step 2, continue cocurrent and cobalt salt and ammonium bicarbonate solution is added, keep the pH value of step 1 constant, the reaction was continued and precipitates；
Step 3, the solution after being precipitated to step 2 is separated by solid-liquid separation and is dried, and small particle spherical cobaltous carbonate is obtained.
2. a kind of preparation method of small particle spherical cobaltous carbonate according to claim 1, which is characterized in that the step 1
In cobalt salt be cobalt chloride, cobaltous sulfate, one kind in cobalt acetate.
3. a kind of preparation method of small particle spherical cobaltous carbonate according to claim 2, which is characterized in that the step 2
The temperature of middle reaction is 35-65 DEG C.
4. a kind of preparation method of small particle spherical cobaltous carbonate according to claim 3, which is characterized in that the step 2
In stir speed (S.S.) be 50-220r/min.
5. a kind of preparation method of small particle spherical cobaltous carbonate according to claim 4, which is characterized in that the step 2
In reaction time be 1-5h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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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| 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 |
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| 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 |
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