CN110342587B - Preparation method of narrow-distribution large-particle-size cobaltosic oxide - Google Patents
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- CN110342587B CN110342587B CN201910330709.0A CN201910330709A CN110342587B CN 110342587 B CN110342587 B CN 110342587B CN 201910330709 A CN201910330709 A CN 201910330709A CN 110342587 B CN110342587 B CN 110342587B
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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 42
- 238000009826 distribution Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 39
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 72
- 230000015572 biosynthetic process Effects 0.000 claims description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000002002 slurry Substances 0.000 claims description 22
- 230000002194 synthesizing effect Effects 0.000 claims description 15
- 229910017052 cobalt Inorganic materials 0.000 claims description 10
- 239000010941 cobalt Substances 0.000 claims description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 230000000087 stabilizing effect Effects 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000007853 buffer solution Substances 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 150000001868 cobalt Chemical class 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- -1 hydroxyl cobaltosic oxide Chemical compound 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000843 powder Substances 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
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the technical field of chemical industry, and relates to a preparation method of narrow-distribution large-particle-size cobaltosic oxide. The method comprises the steps of solution preparation, synthesis reaction, filtration, washing and drying. The cobaltosic oxide product with narrow distribution and large particle size prepared by the method has good particle size distribution, improved product appearance, good sphericity and high production efficiency.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and relates to a preparation method of narrow-distribution large-particle-size cobaltosic oxide.
Background
The lithium ion battery prepared by taking lithium cobaltate as the anode 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 towards high voltage, high compaction and high cycle performance, and thus, the requirement for the raw material cobaltosic oxide is increasing. The Co3O4 is a functional material with special structure and performance, the conventional Co3O4 market already faces the gradually shrinking current situation, and the market demand of the large-particle-size Co3O4 is gradually highlighted. How to prepare high-performance narrow-distribution large-particle-size cobaltosic oxide is particularly important.
The prior preparation process of hydroxyl cobaltosic oxide has the following problems: the small particles (micro powder) have higher proportion, and have larger influence on the subsequent preparation of the anode material; dmax is generally larger, the whole particle size distribution is poorer, and the ratio of (D90-D10)/D50 is basically more than 85 percent; the product appearance is poor.
Disclosure of Invention
The invention aims to provide a preparation method of narrow-distribution large-particle-size cobaltosic oxide aiming at the problems in the prior art.
The specific technical scheme of the invention is as follows:
a preparation method of narrow-distribution large-particle-size cobaltosic oxide comprises the following steps:
a. cobalt salt is taken as a raw material, a cobalt solution with the cobalt concentration of 110-115g/L is prepared as an A solution, a sodium hydroxide solution with the concentration of 220-250g/L is prepared, and an ammonia water solution with the volume of 0.04-0.06 time and the concentration of 180g/L is added into the sodium hydroxide solution as a B solution; hydrazine hydrate is solution C;
b. adding 1m3 hot pure water as synthesis buffer solution into the mother kettle, adding 5-8L C solution, stirring at 74-76 deg.C, adding solution A into the mother kettle at 300 + -30L/h flow, simultaneously adding the solution B, controlling the pH =7.7-7.9, stabilizing the flow of the solution B, synthesizing for 10h, detecting the particle size distribution, enabling D50 to reach 14-16um, respectively moving a mother kettle into a first synthesis kettle and a second synthesis kettle to obtain 1/3 slurry of the total slurry volume of the mother kettle, respectively adding the solution A into the mother kettle, the first synthesis kettle and the second synthesis kettle at the flow of 300 +/-30L/h, simultaneously respectively adding the solution B, controlling the pH =7.7-7.9, stabilizing the flow of the solution B, synthesizing the slurry in the mother kettle, the first synthesizing kettle and the second synthesizing kettle for 18-20 hours, detecting the granularity, and conveying the slurry in the mother kettle, the first synthesizing kettle and the second synthesizing kettle to a slurry homogenizing kettle for mixing, wherein D50 reaches 18-19 um;
c. and (3) carrying out 80-100 ℃ deionized water centrifugal washing on the materials in the homogenizing kettle, drying at 100-120 ℃, and calcining at 750-800 ℃ in a rotary kiln to obtain the narrow-distribution large-particle-size cobaltosic oxide product.
The cobalt salt is one or a mixture of two of cobalt nitrate and cobalt chloride.
The invention has the following beneficial effects:
1. the synthetic raw materials all adopt high-concentration solution, so that the production efficiency is greatly improved on the basis of the prior art;
2. the narrow-distribution large-particle-size cobaltosic oxide product prepared by the method has good particle size distribution, Dmin is more than or equal to 6um, D10 is more than or equal to 12um, D50 is 16-18um, D90 is less than or equal to 25um, Dmax is less than or equal to 40um, (D90-D10)/D50 is less than or equal to 70 percent;
3. the product has improved appearance and better sphericity.
Drawings
FIG. 1 is a graph showing the results of detection of the product of example 1;
FIG. 2 is a graph showing the results of detection of the product of example 2.
Detailed Description
Example 1
A preparation method of narrow-distribution large-particle-size cobaltosic oxide comprises the following steps:
a. cobalt nitrate is used as a raw material, a cobalt solution with the cobalt concentration of 110g/L is prepared as an A solution, a sodium hydroxide solution with the concentration of 220g/L is prepared, and an ammonia water solution with the volume of 0.04 time and the concentration of 180g/L is added into the medium sodium hydroxide solution to be a B solution; hydrazine hydrate is solution C;
b. adding 1m into a mother kettle3Adding 5-8L C solution into hot pure water as synthesis buffer solution, stirring at 74 deg.C, adding solution A into mother kettle at flow rate of 270L/h, simultaneously adding the solution B, controlling the pH =7.7-7.9, stabilizing the flow of the solution B, synthesizing for 10h, detecting the particle size distribution, enabling D50 to reach 14-16um, respectively moving a mother kettle into a first synthesis kettle and a second synthesis kettle to obtain 1/3 slurry of the total slurry volume of the mother kettle, respectively adding the solution A into the mother kettle, the first synthesis kettle and the second synthesis kettle at the flow of 270L/h, simultaneously respectively adding the solution B, controlling the pH =7.7-7.9, stabilizing the flow of the solution B, detecting the granularity after the mother kettle, the first synthesis kettle and the second synthesis kettle are synthesized for 18 hours, and conveying the slurry of the mother kettle, the first synthesis kettle and the second synthesis kettle to a slurry homogenizing kettle for mixing, wherein D50 reaches 18-19 um;
c. and (3) centrifugally washing the materials in the homogenizing kettle by using deionized water at 80 ℃, drying at 100 ℃, and calcining in a rotary kiln at 750 ℃ to obtain a cobaltosic oxide product with narrow distribution and large particle size.
Example 2
A preparation method of narrow-distribution large-particle-size cobaltosic oxide comprises the following steps:
a. cobalt chloride is used as a raw material, a cobalt solution with the cobalt concentration of 113g/L is prepared as an A solution, a sodium hydroxide solution with the concentration of 240g/L is prepared, and an ammonia water solution with the volume of 0.05 time and the concentration of 180g/L is added into the medium sodium hydroxide solution to be a B solution; hydrazine hydrate is solution C;
b. adding 1m3 hot pure water as a synthesis buffer solution into a mother kettle, adding 6L C solution, stirring at 75 ℃, adding solution A into the mother kettle at a flow rate of 300L/h, simultaneously adding solution B, controlling pH =7.8, stabilizing the flow rate of the solution B, synthesizing for 10h, detecting the particle size distribution, wherein D50 reaches 15um, the mother kettle respectively moves slurry of 1/3 of the total slurry volume of the mother kettle into a first synthesis kettle and a second synthesis kettle, respectively adding solution A into the mother kettle, the first synthesis kettle and the second synthesis kettle at a flow rate of 300L/h, respectively adding solution B, controlling pH =7.8, stabilizing the flow rate of the solution B, synthesizing for 19 hours, detecting the particle size by using the mother kettle, the first synthesis kettle and the second synthesis kettle, and conveying the slurry of the mother kettle, the first synthesis kettle and the second synthesis kettle to a slurry homogenizing kettle for mixing, wherein D50 reaches 18-19 um;
c. and (3) centrifugally washing the materials in the homogenizing kettle by deionized water at 90 ℃, drying at 110 ℃, and calcining in a rotary kiln at 770 ℃ to obtain the cobaltosic oxide product with narrow distribution and large particle size.
Example 3
A preparation method of narrow-distribution large-particle-size cobaltosic oxide comprises the following steps:
a. taking a mixture of cobalt nitrate and cobalt chloride as a raw material, preparing a cobalt solution with the cobalt concentration of 115g/L as an A solution, preparing a sodium hydroxide solution with the concentration of 250g/L, adding an ammonia water solution with the volume of 0.06 time and the concentration of 180g/L into the sodium hydroxide solution to obtain a B solution, and adding hydrazine hydrate into the B solution to obtain a C solution;
b. adding 1m into a mother kettle3Hot pure water is used as a synthesis buffer solution, 8L C solution is added, the temperature is controlled to be 76 ℃ for stirring, the solution A is added into a mother kettle at a flow rate of 330L/h, the solution B is added simultaneously, the pH =7.9 is controlled, the flow rate of the solution B is stabilized, the particle size distribution is detected after 10h of synthesis, D50 reaches 16um, the mother kettle moves 1/3 slurry of the total slurry volume of the mother kettle into a first synthesis kettle and a second synthesis kettle respectively, the solution A is added into the mother kettle, the first synthesis kettle and the second synthesis kettle respectively at a flow rate of 330L/h, the solution B is added simultaneously, and the control is performed to controlThe pH =7.9, the flow of the solution B is stabilized, the mother kettle, the first synthesis kettle and the second synthesis kettle are synthesized for 20 hours, the particle size is detected, D50 reaches 19um, and slurry of the mother kettle, the first synthesis kettle and the second synthesis kettle is conveyed to a slurry homogenizing kettle to be mixed;
c. and (3) centrifugally washing the materials in the homogenizing kettle by deionized water at 100 ℃, drying at 120 ℃, and calcining in a rotary kiln at 800 ℃ to obtain the cobaltosic oxide product with narrow distribution and large particle size.
Claims (1)
1. A preparation method of cobaltosic oxide with narrow distribution and large particle size is characterized by comprising the following steps:
cobalt salt is taken as a raw material, a cobalt solution with the cobalt concentration of 110-115g/L is prepared as an A solution, a sodium hydroxide solution with the concentration of 220-250g/L is prepared, and an ammonia water solution with the volume of 0.04-0.06 time and the concentration of 180g/L is added into the sodium hydroxide solution as a B solution; hydrazine hydrate is solution C;
adding 1m into a mother kettle3Adding 5-8L C solution into hot pure water as synthesis buffer solution, stirring at 74-76 deg.C, adding solution A into mother kettle at flow rate of 300 + -30L/h, simultaneously adding the solution B, controlling the pH =7.7-7.9, stabilizing the flow of the solution B, synthesizing for 10h, detecting the particle size distribution, enabling D50 to reach 14-16um, respectively moving a mother kettle into a first synthesis kettle and a second synthesis kettle to obtain 1/3 slurry of the total slurry volume of the mother kettle, respectively adding the solution A into the mother kettle, the first synthesis kettle and the second synthesis kettle at the flow of 300 +/-30L/h, simultaneously respectively adding the solution B, controlling the pH =7.7-7.9, stabilizing the flow of the solution B, synthesizing the slurry in the mother kettle, the first synthesizing kettle and the second synthesizing kettle for 18-20 hours, detecting the granularity, and conveying the slurry in the mother kettle, the first synthesizing kettle and the second synthesizing kettle to a slurry homogenizing kettle for mixing, wherein D50 reaches 18-19 um;
and (3) carrying out 80-100 ℃ deionized water centrifugal washing on the materials in the homogenizing kettle, drying at 100-120 ℃, and calcining at 750-800 ℃ in a rotary kiln to obtain the narrow-distribution large-particle-size cobaltosic oxide product.
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| CN113735185A (en) * | 2021-08-25 | 2021-12-03 | 金川集团股份有限公司 | Preparation method of narrow-distribution medium-particle-size cobaltosic oxide |
| CN115259237A (en) * | 2022-06-30 | 2022-11-01 | 金川集团股份有限公司 | Method for eliminating cobalt hydroxide micropowder |
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Effective date of registration: 20240220 Address after: 737100 No. 2 Lanzhou Road, Beijing Road Street, Jinchuan District, Jinchang City, Gansu Province Patentee after: Jinchuan Group Nickel Cobalt Co.,Ltd. Country or region after: China Patentee after: LANZHOU JINCHUAN ADVANGCED MATERIALS TECHNOLOGY Co.,Ltd. Address before: 737103 No. 98, Jinchuan Road, Jinchang, Gansu Patentee before: JINCHUAN GROUP Co.,Ltd. Country or region before: China Patentee before: LANZHOU JINCHUAN ADVANGCED MATERIALS TECHNOLOGY Co.,Ltd. |