CN112429782B - Method for controlling particle size of small-particle-size cobaltosic oxide kettle - Google Patents
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- CN112429782B CN112429782B CN202011402575.8A CN202011402575A CN112429782B CN 112429782 B CN112429782 B CN 112429782B CN 202011402575 A CN202011402575 A CN 202011402575A CN 112429782 B CN112429782 B CN 112429782B
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- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000002245 particle Substances 0.000 title claims description 34
- 239000000243 solution Substances 0.000 claims abstract description 71
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 50
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 39
- 239000003112 inhibitor Substances 0.000 claims abstract description 23
- 239000011259 mixed solution Substances 0.000 claims abstract description 20
- 239000002002 slurry Substances 0.000 claims abstract description 19
- 150000001868 cobalt Chemical class 0.000 claims abstract description 17
- 239000012266 salt solution Substances 0.000 claims abstract description 16
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 229910001429 cobalt ion Inorganic materials 0.000 claims abstract description 5
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 5
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 14
- 239000012467 final product Substances 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 description 13
- 238000009826 distribution Methods 0.000 description 3
- GPKIXZRJUHCCKX-UHFFFAOYSA-N 2-[(5-methyl-2-propan-2-ylphenoxy)methyl]oxirane Chemical compound CC(C)C1=CC=C(C)C=C1OCC1OC1 GPKIXZRJUHCCKX-UHFFFAOYSA-N 0.000 description 2
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000007853 buffer solution Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 206010003694 Atrophy Diseases 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000037444 atrophy Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- -1 hydroxyl cobaltosic oxide Chemical compound 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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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
- C01G51/04—Oxides; Hydroxides
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for controlling the grain size of a small-granularity cobaltosic oxide kettle, which comprises the following steps: preparing cobalt salt solution with cobalt ion concentration of 108-112g/L, preparing sodium hydroxide solution, and preparing inhibitor solution with mass percent of 8-10%; adding ammonia water solution with the concentration of 180-200g/L into the sodium hydroxide solution to obtain a mixed solution; adding a mixed solution into a synthesis kettle with a base solution to enable the pH value in the synthesis kettle to be 10-10.2, adding a cobalt salt solution into the synthesis kettle, and finally adding an inhibitor solution into the synthesis kettle to carry out synthesis reaction to obtain slurry; and (3) sequentially carrying out centrifugal washing, drying and calcining on the slurry to obtain a small-granularity cobaltosic oxide product. The invention ensures that the grain diameter of the kettle is stably controlled to be 2.0-2.5 mu m by precisely controlling the grain diameter of the kettle, and the grain diameter of the final product can be ensured to be 4.0-6.0 mu m.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a method for controlling the particle size of a small-particle-size cobaltosic oxide kettle.
Background
The lithium ion battery prepared by taking lithium cobaltate as the positive electrode material has the characteristics of light weight, large capacity, high specific energy, high working voltage, stable discharge, suitability for large-current discharge, good cycle performance, long service life and the like, and is mainly applied to the field of 3C digital codes.
Lithium cobaltate is developing toward high voltage, high compaction and high cycle performance,therefore, the requirements for the raw material cobaltosic oxide are also increasing. Co (Co) 3 O 4 Is a functional material with special structure and performance, conventional Co 3 O 4 The market has faced the current situation of gradual atrophy, small-granularity Co 3 O 4 The market demand of (2) is gradually highlighted. The small-granularity cobaltosic oxide has small particle size, the size of the starting kettle particle size determines the size of the product particle size and the stability of the batch particle size, and how to prepare the small-granularity cobaltosic oxide is particularly important. The existing preparation technology of the hydroxyl cobaltosic oxide with small granularity has the following problems: the particle size of the stirred tank is unstable, so that the granularity fluctuation of the final product is large; the micro powder is not removed, the control is unstable in the kettle starting process, and the granularity of the batch is unstable.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a method for controlling the particle size of a small-granularity cobaltosic oxide kettle, which has high production efficiency, small product granularity and good cobaltosic oxide appearance.
The invention aims at realizing the following technical scheme:
a method for controlling the size of small-granularity cobaltosic oxide starting kettle particle size, which is characterized by comprising the following steps:
(1) Preparing a cobalt salt solution with the cobalt ion concentration of 108g/L-112g/L, preparing a sodium hydroxide solution with the concentration of 295g/L-305g/L, and preparing an inhibitor solution with the mass percent of 8% -10%;
(2) Adding ammonia water solution with the concentration of 180g/L-200g/L into the sodium hydroxide solution in the step (1) to obtain a mixed solution; the volume ratio of the sodium hydroxide solution to the ammonia water solution is 1 (0.04-0.06);
(3) Adding the mixed solution into a synthesis kettle with the base solution to enable the pH value in the synthesis kettle to be 10-10.2, adding the cobalt salt solution into the synthesis kettle until the pH value in the synthesis kettle is 8.4-8.5, adding the inhibitor solution into the synthesis kettle after 30-40 min, and carrying out synthesis reaction to obtain slurry; the process conditions of the synthesis reaction are as follows: the reaction temperature is 75-76 ℃, the reaction pH value is 8.4-8.5, and the reaction time is 21-25 h;
(4) And (3) sequentially carrying out centrifugal washing, drying and calcining on the slurry to obtain a small-granularity cobaltosic oxide product.
The method for controlling the grain size of the small-granularity cobaltosic oxide kettle is characterized in that the bottom liquid in the synthesis kettle in the step (3) is pure water, and the volume of the bottom liquid is 1m 3 -2m 3 。
The method for controlling the particle size of the small-particle-size cobaltosic oxide kettle is characterized in that in the step (4), the slurry is centrifugally washed by deionized water at 80-95 ℃, the centrifugally washed slurry is dried at 100-120 ℃, and the dried slurry is calcined at 800-900 ℃ to obtain the small-particle-size cobaltosic oxide product.
The method for controlling the particle size of the small-particle-size cobaltosic oxide kettle is characterized in that the flow rate of the mixed solution added into the synthesis kettle with the base solution in the step (3) is 150L/h-160L/h; the flow rate of the cobalt salt solution added into the synthesis kettle with the base solution is 295L/h-305L/h; the flow rate of the inhibitor solution added into the synthesis kettle with the base solution is 40L/h-60L/h.
The method for controlling the particle size of the small-particle-size cobaltosic oxide kettle is characterized in that the particle size of the small-particle-size cobaltosic oxide product in the step (4) is 4.0-6.0 μm.
The method for controlling the particle size of the small-particle-size cobaltosic oxide kettle is characterized in that the cobalt salt solution in the step (1) is cobalt nitrate solution; the inhibitor solution is a strong oxidizer.
The method for controlling the particle size of the small-particle-size cobaltosic oxide kettle is characterized in that the inhibitor solution in the step (1) is hydrogen peroxide.
Compared with the prior art, the invention has the beneficial technical effects that: the invention is a method for preparing cobaltosic oxide with small granularity of a precursor of a lithium cobalt oxide battery anode material, and the particle size of a starting kettle is controlled to be 2.0-2.5 mu m by precisely controlling the particle size of the starting kettle, so that the particle size of a final small-granularity cobaltosic oxide product can be ensured to be 4.0-6.0 mu m. Along with the growth of crystal nucleus, the disappearance time of micro powder is about 6 hours, and the granularity is stable after 6 hours. According to the invention, through controlling the adding sequence of the kettle starting solution, the pH value increment and the adding time point of the inhibitor, each technological parameter is controlled in a stable process, and the particle size distribution of the finally prepared small-particle-size cobaltosic oxide product is D0 & gt 1 mu m, dmin:2-4 μm, D50:4-6 μm, D90:6.5-9.5 μm, dmax:10-12 μm.
Drawings
FIG. 1 is a schematic process flow diagram of the method of the present invention;
FIG. 2 is a graph showing the results of detection of small-particle size tricobalt tetraoxide products obtained in the examples.
Detailed Description
Referring to fig. 1, the method for controlling the particle size of the small-particle-size cobaltosic oxide kettle comprises the following steps:
preparing a solution:
(1) Preparing cobalt salt solution with cobalt ion concentration of 108g/L-112g/L, preparing sodium hydroxide solution with concentration of 295g/L-305g/L, and preparing inhibitor solution with mass percent of 8% -10%; all solutions were stored in the front tank for use. The cobalt salt solution is cobalt nitrate solution. The inhibitor solution is a strong oxidant, preferably hydrogen peroxide.
(2) Adding ammonia water solution with the concentration of 180g/L-200g/L into the sodium hydroxide solution in the step (1) to obtain a mixed solution; the volume ratio of the sodium hydroxide solution to the ammonia water solution is 1 (0.04-0.06).
And (3) kettle starting control:
(3) The synthesis kettle is added with a fixed volume (1-2 m 3 ) The hot pure water of (2) is used as a synthesis buffer solution, the pH value of the starting kettle is about 8.0, and the temperature is raised to be within the technological parameter range. Adding a mixed solution into a synthesis kettle with a base solution, wherein the flow rate of the mixed solution added into the synthesis kettle with the base solution is 150L/h-160L/h, the pH value in the synthesis kettle can be rapidly increased, at the moment, the pH value increment is observed, the pH value increment is controlled to be within the range of 0.2-0.3, and when the pH value is increased to 10-10.2, a cobalt salt solution is added into the synthesis kettle, and the flow rate of the cobalt salt solution added into the synthesis kettle with the base solution is 295L/h-305L/h; the flow of the mixed solution is kept unchanged, the pH value is slowly increased at the moment, the increasing value of the pH value is observed, and the slow down is startedWhen the pH value of the mixed solution is stable within the required range of technological parameters within 30min, the pH value of the mixed solution is in the stable descending trend in the whole process, the fluctuation of the pH value is avoided, the inhibitor solution is added when the kettle is started for 30-40 min after the pH value of the kettle is kept to be stable within the required time, and the flow of the inhibitor solution added into the synthesis kettle with the base solution is 40-60L/h; the mixed solution, the cobalt salt solution and the inhibitor solution are added into a synthesis kettle from the bottom in a parallel flow mode to carry out synthesis reaction, so as to obtain slurry. The process conditions of the synthesis reaction are as follows: the reaction temperature is 75-76 ℃, the reaction pH value is 8.4-8.5, and the reaction time is 21-25 h. The grain diameter is detected after the kettle is started for 1 hour, and the grain diameter of the kettle can be stably controlled to be 2.0-2.5 mu m.
Filtering, washing and drying:
(4) And after the synthesis reaction is finished, sequentially performing centrifugal washing, drying and calcining on the slurry to obtain a small-granularity cobaltosic oxide product. And (3) centrifugally washing the slurry with deionized water at 80-95 ℃, drying the centrifugally washed slurry at 100-120 ℃, and calcining the dried slurry at 800-900 ℃ to obtain a small-granularity cobaltosic oxide product with the particle size of 4.0-6.0 mu m. The particle size distribution of the finally prepared small-particle-size cobaltosic oxide product is D0 & gt 1 mu m, dmin:2-4 μm, D50:4-6 μm, D90:6.5-9.5 μm, dmax:10-12 μm.
Example 1
Preparing a cobalt nitrate solution with cobalt ion concentration of 108g/L-112g/L, a sodium hydroxide solution with concentration of 295g/L-305g/L and an inhibitor solution with mass percent of 8% -10% by taking cobalt salt as a raw material; all solutions were stored in the front tank for use. The inhibitor solution is hydrogen peroxide.
Adding ammonia water solution with the concentration of 180g/L-200g/L into the sodium hydroxide solution to obtain a mixed solution; the volume ratio of the sodium hydroxide solution to the ammonia water solution is 1 (0.04-0.06).
The synthesis kettle is added with a fixed volume (1-2 m 3 ) The hot pure water of (2) is used as a synthesis buffer solution, the pH value of the starting kettle is about 8.0, and the temperature is raised to be within the technological parameter range. Adding the mixed solution into a synthesis kettle with the base solution, wherein the feeding flow is 150L/h-160L/h, and the synthesis kettle is internally provided withThe pH value can be rapidly increased, at the moment, the pH value increment is observed, the pH value increment is controlled within the range of 0.2-0.3, when the pH value is increased to 10-10.2, cobalt nitrate solution is added into the synthesis kettle, and the feeding flow is 300L/h; the flow of the mixed solution is kept unchanged, the pH value is slowly increased at the moment, the pH value increasing value is observed, when the pH value begins to slowly decrease, the flow of the mixed solution is regulated, the pH value is stabilized within the process parameter requirement range within 30min, the pH value in the whole process is in the stable decreasing trend, the fluctuation of the pH value is avoided, the inhibitor solution is added when the kettle is started for 30-40 min after the pH value tends to be stabilized within the required time, and the flow of the inhibitor solution added into the synthesis kettle with the base solution is 40-60L/h; the mixed solution, the cobalt salt solution and the inhibitor solution are added into a synthesis kettle from the bottom in a parallel flow mode to carry out synthesis reaction, so as to obtain slurry. The process conditions of the synthesis reaction are as follows: the reaction temperature is 75-76 ℃, the reaction pH value is 8.4-8.5, and the reaction time is 21-25 h. The particle size was measured after 1 hour of the start of the reaction, and the particle size of the start of the reaction was stably controlled to 2.0 to 2.5. Mu.m, and the results are shown in Table 1.
After the synthesis reaction is finished, centrifugally washing the slurry by using deionized water at 80-95 ℃, drying at 100-120 ℃ and calcining at 800-900 ℃ to obtain a small-granularity cobaltosic oxide product, wherein the granularity distribution of the finally prepared small-granularity cobaltosic oxide product is D0 & gt 1 mu m, dmin:2-4 μm, D50:4-6 μm, D90:6.5-9.5 μm, dmax:10-12 μm and the results are shown in Table 2.
TABLE 1A group of small particle size cobaltosic oxide data table for 1 hour from kettle
| Numbering device | D0(μm) | D10(μm) | D50(μm) | D90(μm) | D100(μm) |
| CJL-TB6-T1 | 0.01 | 0.84 | 2.19 | 3.92 | 6.66 |
| CJL-TB6-T2 | 0.36 | 1.14 | 2.22 | 3.92 | 5.91 |
| CJL-TB6-T3 | 0.36 | 1.16 | 2.34 | 4.22 | 7.62 |
| CJL-TB6-T4 | 0.407 | 1.16 | 2.35 | 4.3 | 7.6 |
| CJL-TB6-T5 | 0.406 | 1.14 | 2.33 | 4.18 | 6.72 |
| CJL-TB6-T6 | 0.406 | 1.09 | 2.30 | 4.23 | 6.72 |
| CJL-TB6-T7 | 0.358 | 0.994 | 2.54 | 3.18 | 5.91 |
| CJL-TB6-T8 | 0.322 | 1.02 | 2.11 | 3.73 | 5.91 |
TABLE 2A small particle size tricobalt tetraoxide synthesis end data table
| Numbering device | D0(μm) | D10(μm) | D50(μm) | D90(μm) | D100(μm) |
| CJL-TB6-T1 | 1.67 | 3.11 | 4.87 | 7.54 | 11.20 |
| CJL-TB6-T2 | 1.66 | 2.88 | 4.48 | 6.83 | 9.86 |
| CJL-TB6-T3 | 1.70 | 3.13 | 4.66 | 6.93 | 12.10 |
| CJL-TB6-T4 | 1.71 | 3.61 | 4.81 | 7.29 | 12.60 |
| CJL-TB6-T5 | 1.89 | 3.32 | 4.96 | 7.33 | 12.40 |
| CJL-TB6-T6 | 1.88 | 3.11 | 4.83 | 7.32 | 9.86 |
| CJL-TB6-T7 | 1.47 | 2.90 | 4.90 | 8.14 | 12.70 |
| CJL-TB6-T8 | 1.48 | 2.96 | 4.99 | 9.31 | 12.70 |
Claims (6)
1. A method for controlling the size of small-granularity cobaltosic oxide starting kettle particle size, which is characterized by comprising the following steps:
(1) Preparing a cobalt salt solution with the cobalt ion concentration of 108g/L-112g/L, preparing a sodium hydroxide solution with the concentration of 295g/L-305g/L, and preparing an inhibitor solution with the mass percent of 8% -10%;
(2) Adding ammonia water solution with the concentration of 180g/L-200g/L into the sodium hydroxide solution in the step (1) to obtain a mixed solution; the volume ratio of the sodium hydroxide solution to the ammonia water solution is 1 (0.04-0.06);
(3) Adding the mixed solution into a synthesis kettle with the base solution to enable the pH value in the synthesis kettle to be 10-10.2, adding the cobalt salt solution into the synthesis kettle until the pH value in the synthesis kettle is 8.4-8.5, adding the inhibitor solution into the synthesis kettle after 30-40 min, and carrying out synthesis reaction to obtain slurry; the process conditions of the synthesis reaction are as follows: the reaction temperature is 75-76 ℃, the reaction pH value is 8.4-8.5, and the reaction time is 21-25 h; the flow rate of the mixed solution added into the synthesis kettle with the base solution is 150L/h-160L/h; the flow rate of the cobalt salt solution added into the synthesis kettle with the base solution is 295L/h-305L/h; the flow rate of the inhibitor solution added into the synthesis kettle with the base solution is 40L/h-60L/h;
(4) And (3) sequentially carrying out centrifugal washing, drying and calcining on the slurry to obtain a small-granularity cobaltosic oxide product.
2. The method for controlling the particle size of a small-particle-size cobaltosic oxide kettle according to claim 1, wherein the base solution in the synthesis kettle in the step (3) is pure water, and the volume of the base solution is 1m 3 -2m 3 。
3. The method for controlling the grain size of a small-granularity cobaltosic oxide kettle according to claim 2, wherein in the step (4), the slurry is centrifugally washed by deionized water at 80-95 ℃, the centrifugally washed slurry is dried at 100-120 ℃, and the dried slurry is calcined at 800-900 ℃ to obtain the small-granularity cobaltosic oxide product.
4. The method for controlling the size of the small-particle-size cobaltosic oxide pot according to claim 1, wherein the small-particle-size cobaltosic oxide product in the step (4) has a particle size of 4.0 μm to 6.0 μm.
5. The method for controlling the particle size of a small-particle size cobaltosic oxide autoclave according to any one of claims 1 to 4, wherein the cobalt salt solution in the step (1) is a cobalt nitrate solution; the inhibitor solution is a strong oxidizer.
6. The method for controlling the particle size of a small-particle-size cobaltosic oxide autoclave according to claim 5, wherein the inhibitor solution in the step (1) is hydrogen peroxide.
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