CN115636444A - Preparation method of small-particle-size low-sodium-sulfur cobaltosic oxide for high-rate lithium cobaltate - Google Patents
Preparation method of small-particle-size low-sodium-sulfur cobaltosic oxide for high-rate lithium cobaltate Download PDFInfo
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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 98
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 61
- 239000011593 sulfur Substances 0.000 title claims abstract description 61
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 37
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 30
- 239000011734 sodium Substances 0.000 claims abstract description 30
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 27
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 18
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 15
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 13
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 7
- 239000010941 cobalt Substances 0.000 claims abstract description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940044175 cobalt sulfate Drugs 0.000 claims abstract description 7
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims abstract description 7
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 38
- 239000000243 solution Substances 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 239000002002 slurry Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000002245 particle Substances 0.000 abstract description 9
- 238000005056 compaction Methods 0.000 abstract description 3
- 239000008139 complexing agent Substances 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 239000012716 precipitator Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- 206010003694 Atrophy Diseases 0.000 description 1
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 1
- 102000004310 Ion Channels Human genes 0.000 description 1
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000037444 atrophy Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 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
- 230000000750 progressive effect Effects 0.000 description 1
- -1 sulfur ions Chemical class 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- 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
Abstract
The invention discloses a preparation method of small-particle-size low-sodium-sulfur cobaltosic oxide for high-rate lithium cobaltate, which comprises the steps of taking cobalt sulfate as a cobalt source, EDTA-2Na as a complexing agent, sodium hydroxide as a precipitator and hydrogen peroxide as an oxidant, adding a solution into a reaction kettle in a concurrent flow manner for wet synthesis to prepare a cobalt hydroxide product with particle size of 4~5 mu m and regular appearance, and then carrying out sulfur washing, calcination, sodium washing and drying to obtain a cobalt hydroxide product with particle size of 4~5 mu m and tap density of more than or equal to 2.0g/cm 3 Specific surface area of 3.0 +/-0.5 m 2 The content of sodium is less than or equal to 0.01 percent and the content of sulfur is less than or equal to 0.005 percent. The preparation process of the method is simple and easy to control, is environment-friendly, and is suitable for industrial popularization and application. The cobaltosic oxide obtained by the method can be used for preparing high-voltage, high-compaction and high-rate lithium cobaltate subsequently.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery preparation, and particularly relates to a preparation method of small-particle-size low-sodium-sulfur cobaltosic oxide for high-rate lithium cobalt 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.
At present, lithium cobaltate is developing towards high voltage, high compaction and high rate, and the raw material cobaltosic oxide (Co) 3 O 4 ) Is increasingly demanding. Co 3 O 4 Is a functional material with special structure and performance, and is Co with conventional particle size (6-10 mu m) 3 O 4 The market has faced a current situation of progressive atrophy. Because the single-crystal small-particle-size lithium cobaltate has a small particle size, lithium ions have shorter ion channels in the charge and discharge processes, so the single-crystal small-particle-size lithium cobaltate has the characteristic of high multiplying power, and the single-crystal structure of the lithium cobaltate is influenced by high content of sodium and sulfur ions, so that research on how to prepare small-particle-size low-sodium-sulfur cobaltosic oxide serving as a lithium cobaltate raw material becomes a hot spot.
Chinese invention patent CN202010716123.0 discloses a method for removing sulfur content in hydroxide precursor, which directly raises the pH of the slurry by changing the aging condition of the slurry to achieve the purpose of controlling the content of S impurities in the product, and can reduce the sulfur content in the synthesized product to 0.15%. Chinese invention patent CN202011117435.6 discloses a method for reducing the sulfur content of large-particle impurities of a nickel-cobalt-manganese ternary precursor, and specifically adopts hot water and a dilute alkali solution for washing twice, so that the S content in the product can be reduced to be less than 850 ppm. The method has complicated and uncontrollable process and can not reduce the content of sodium in the product at the same time.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention aims to provide a preparation method of small-particle-size low-sodium-sulfur cobaltosic oxide, which is simple and easy to control in the production process.
The purpose of the invention is realized by the following technical scheme:
a preparation method of small-particle-size low-sodium-sulfur cobaltosic oxide for high-rate lithium cobaltate comprises the following steps:
a. liquid preparation
Taking cobalt sulfate and EDTA-2Na as raw materials, preparing a mixed solution A with the cobalt concentration of 90-110g/L and the EDTA-2Na concentration of 0.8-1.2g/L; preparing a sodium hydroxide solution with the concentration of 280-320g/L as a solution B; preparing a hydrogen peroxide solution with the concentration of 160 to 180g/L as a solution C;
b. synthesis reaction
Adding the A, B, C solution into a reaction kettle in a concurrent flow manner, and carrying out small-granularity cobalt hydroxide synthesis under stirring to obtain synthetic slurry; wherein the flow rate of the solution A is 300L/h, the flow rate of the solution C is 45 to 55L/h, the reaction pH value is 10.0 to 10.5, the flow rate of the solution B is dynamically adjusted according to the reaction pH value, the reaction temperature is 74 to 78 ℃, the stirring strength is 160 to 180 r/min, and the reaction time is 25 to 30h;
c. sulfur washing
Washing the synthesized slurry in the step b to obtain a small-granularity low-sulfur cobalt hydroxide material; the washing equipment is a filter press, and the washing liquid is deionized water at 80-90 ℃; the sulfur content of the small-granularity low-sulfur cobalt hydroxide material is less than or equal to 0.005 percent;
d. calcination of
Calcining the small-granularity low-sulfur cobalt hydroxide material in the step d to obtain a small-granularity low-sulfur cobaltosic oxide material;
e. washing sodium, and drying
D, washing sodium and drying the small-granularity low-sulfur cobaltosic oxide material in the step d to obtain a small-granularity low-sodium-sulfur cobaltosic oxide product; the equipment for washing the sodium is a filter press, and the washing liquid is deionized water at the temperature of 80-90 ℃.
As a further preferable technical scheme of the invention, in the step d, the calcination condition is rotary kiln calcination, the calcination temperature is 750-780 ℃, and the calcination time is 2-4 h.
Further, the small-granularity low-sulfur cobaltosic oxide material has the laser granularity D 50 Is 4~5μm with tap density not less than 2.0g/cm 3 The specific surface area is 3.0 +/-0.5 m 2 Per g, sodium content is less than or equal to0.05 percent and the sulfur content is less than or equal to 0.005 percent.
Further, in the step e, the drying equipment is a flash evaporation machine, and the moisture content of the dried material is less than or equal to 0.05%.
Further, in the step e, the light granularity D of the small-granularity low-sodium-sulfur cobaltosic oxide product 50 4~5 μm, tap density ≧ 2.0g/cm 3 The specific surface area is 3.0 +/-0.5 m 2 The sodium content is less than or equal to 0.01 percent and the sulfur content is less than or equal to 0.005 percent, and the shape is spherical or quasi-spherical.
According to the invention, cobalt sulfate is used as a cobalt source, EDTA-2Na is used as a complexing agent, hydrogen peroxide is used as an oxidant, a specific synthesis process is adopted, sulfate radicals can be simply and easily removed from cobalt hydroxide particles to obtain a small-particle-size cobalt hydroxide material with particle size of 4~5μm and regular appearance, sulfur content of the small-particle-size cobalt hydroxide material is reduced to be less than or equal to 0.005% through sulfur washing, then the crystal lattice structure is changed through calcination, sodium washing is simple and easy, finally sodium washing is carried out by hot pure water, drying is carried out to obtain sodium content of less than or equal to 0.01%, sulfur content of less than or equal to 0.005%, and laser particle size D is obtained 50 Is a small-particle-size low-sodium sulfur cobaltosic oxide product of 4~5 mu m, and the production process is simple and easy to control. The cobaltosic oxide obtained by the method can be used for preparing high-voltage, high-compaction and high-rate lithium cobaltate subsequently.
The washing liquid for washing sulfur and sodium in the invention is common deionized water, the generated wastewater does not contain organic matters, the treatment can be simple and convenient, the wastewater treatment cost is reduced, the operation environment is improved, and the environment is not polluted.
Drawings
FIG. 1 is a flow chart of the process for preparing small-particle size low-sodium sulfur cobaltosic oxide of the present invention;
FIG. 2 is an electron microscope image of the micro-morphology of small-particle-size cobalt hydroxide prepared in example 1 of the present invention;
FIG. 3 is an electron microscope image of the micro-morphology of small-particle-size cobaltosic oxide prepared in example 1 of the present invention;
FIG. 4 is an electron microscope image of the micro-morphology of small-particle-size cobalt hydroxide prepared in example 2 of the present invention;
FIG. 5 is an electron microscope image of the micro-morphology of small-particle-size cobaltosic oxide prepared in example 2 of the present invention;
FIG. 6 is an electron microscope image of the micro-morphology of small-particle-size cobalt hydroxide prepared in example 3 of the present invention;
FIG. 7 is an electron microscope image of the micro-morphology of small-particle-size cobaltosic oxide prepared in example 3 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings and specific embodiments, and it is to be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation process of the invention is shown in figure 1.
Example 1
The production steps are as described above, and the specific parameters in each step are as follows:
taking cobalt sulfate and EDTA-2Na as raw materials, preparing a mixed solution A with the cobalt concentration of 90g/L and the EDTA-2Na concentration of 0.8 g/L; preparing a sodium hydroxide solution with the concentration of 280g/L as a B solution; preparing a hydrogen peroxide solution with the concentration of 160g/L into a solution C.
At 10m 3 The small-granularity cobalt hydroxide is synthesized in the reaction kettle. And (2) adding the A, B, C solution into a reaction kettle in a concurrent flow manner for synthesis, wherein in the synthesis process, the flow rate of the solution A is strictly controlled to be 300L/h, the flow rate of the solution C is strictly controlled to be 45L/h, the reaction pH value is 10.5, the flow rate of the solution B is dynamically adjusted according to the reaction pH value, the reaction temperature is 78 ℃, the stirring intensity is 160 r/min, and the reaction time is 25h.
And after the synthesis is finished, carrying out sulfur washing on the synthesized slurry by using a filter press, wherein the washing liquid is deionized water with the temperature of 80-90 ℃, and the sulfur content in the sulfur-washed material is controlled to be less than or equal to 0.005%.
And calcining the sulfur-washed small-granularity low-sulfur cobalt hydroxide material on a rotary kiln at 780 ℃ for 2 hours to obtain the small-granularity low-sulfur cobaltosic oxide material.
And (3) washing sodium of the calcined small-granularity cobaltosic oxide material by using a filter press, wherein the washing liquid is deionized water at the temperature of 80-90 ℃, the sodium content of the washed material is less than or equal to 0.01%, then drying the material after sodium washing by using a flash evaporation machine, and controlling the water content of the dried material to be less than or equal to 0.05% to obtain the small-granularity low-sodium-sulfur cobaltosic oxide product. The physicochemical indexes of the cobaltosic oxide product in this example are shown in table 1. The microcosmic appearances of the prepared small-particle-size cobalt hydroxide and cobaltosic oxide are shown in figures 2-3.
TABLE 1 partial physicochemical index of Cobaltosic oxide product in inventive example 1
Example 2
The production steps are as described above, and the specific parameters in each step are as follows:
taking cobalt sulfate and EDTA-2Na as raw materials, preparing a mixed solution A with the cobalt concentration of 100g/L and the EDTA-2Na concentration of 1.0 g/L; preparing a sodium hydroxide solution with the concentration of 300g/L as a B solution; preparing hydrogen peroxide solution with the concentration of 170g/L into solution C.
At 10m 3 The reaction kettle is used for synthesizing the small-granularity cobaltosic oxide precursor. And (2) adding the A, B, C solution into a reaction kettle in a concurrent flow manner for synthesis, wherein in the synthesis process, the flow rate of the solution A is strictly controlled to be 300L/h, the flow rate of the solution C is strictly controlled to be 50L/h, the flow rate of the solution B is dynamically adjusted according to the reaction pH value, the reaction pH value is 10.2, the reaction temperature is 76 ℃, the stirring intensity is 170 r/min, and the reaction time is 28h.
And after the synthesis is finished, carrying out sulfur washing operation on the synthesized slurry by using a filter press, wherein the washing liquid is deionized water with the temperature of 80-90 ℃, and the sulfur content in the sulfur-washed material is controlled to be less than or equal to 0.005%.
And calcining the washed small-granularity cobalt hydroxide material on a rotary kiln at 760 ℃ for 3h to obtain the small-granularity low-sulfur cobaltosic oxide material.
And (3) washing the calcined small-particle-size cobaltosic oxide material with sodium by using a filter press, wherein the washing liquid is deionized water at the temperature of 80-90 ℃, the content of sodium in the washed material is less than or equal to 0.01%, drying the washed material with the sodium by using a flash evaporation machine, and controlling the water content of the dried material to be less than or equal to 0.05% to obtain the small-particle-size low-sodium-sulfur cobaltosic oxide product. In the present example, the physicochemical indexes of the cobaltosic oxide product are shown in table 2. The microcosmic appearances of the prepared small-particle-size cobalt hydroxide and cobaltosic oxide are shown in figures 4-5.
TABLE 2 partial physicochemical indexes of cobaltosic oxide product in example 2 of the present invention
Example 3
The production steps are as described above, and the specific parameters in each step are as follows:
taking cobalt sulfate and EDTA-2Na as raw materials, preparing a mixed solution A with the cobalt concentration of 110g/L and the EDTA-2Na concentration of 1.2 g/L; preparing a sodium hydroxide solution with the concentration of 320g/L as a B solution; preparing a hydrogen peroxide solution with the concentration of 180g/L into a solution C.
At 10m 3 The small-granularity cobalt hydroxide is synthesized in the reaction kettle. And (2) adding the A, B, C solution into a reaction kettle in a concurrent flow manner for synthesis, wherein in the synthesis process, the flow rate of the solution A is strictly controlled to be 300L/h, the flow rate of the solution C is strictly controlled to be 55L/h, the flow rate of the solution B is dynamically adjusted according to the reaction pH value, the reaction pH value is 10.0, the reaction temperature is 74 ℃, the stirring intensity is 180 r/min, and the reaction time is 30h.
And after the synthesis is finished, carrying out sulfur washing on the synthesized slurry by using a filter press, wherein the washing liquid is deionized water with the temperature of 80-90 ℃, and the sulfur content in the sulfur-washed material is controlled to be less than or equal to 0.005%.
And calcining the washed small-granularity cobalt hydroxide material on a rotary kiln at the calcining temperature of 750 ℃ for 4 hours to obtain the small-granularity low-sulfur cobaltosic oxide material.
And (3) washing the calcined small-particle-size cobaltosic oxide material with sodium by using a filter press, wherein the washing liquid is deionized water at the temperature of 80-90 ℃, the content of sodium in the washed material is less than or equal to 0.01%, drying the washed material with the sodium by using a flash evaporation machine, and controlling the water content of the dried material to be less than or equal to 0.05% to obtain the small-particle-size low-sodium-sulfur cobaltosic oxide product. The physicochemical indexes of the cobaltosic oxide product in this example are shown in table 3. The microcosmic appearances of the prepared small-particle-size cobalt hydroxide and cobaltosic oxide are shown in figures 6-7.
TABLE 3 partial physicochemical indexes of Cobaltosic oxide product in example 3 of the present invention
Claims (5)
1. A preparation method of small-particle-size low-sodium-sulfur cobaltosic oxide for high-rate lithium cobaltate is characterized by comprising the following steps of:
a. liquid preparation
Taking cobalt sulfate and EDTA-2Na as raw materials, preparing a mixed solution A with the cobalt concentration of 90-110g/L and the EDTA-2Na concentration of 0.8-1.2g/L; preparing a sodium hydroxide solution with the concentration of 280-320g/L as a solution B; preparing a hydrogen peroxide solution with the concentration of 160 to 180g/L as a solution C;
b. synthesis reaction
Adding A, B, C solution into a reaction kettle in a concurrent flow manner, and carrying out small-particle-size cobalt hydroxide synthesis under stirring to obtain synthetic slurry; wherein the flow rate of the solution A is 300L/h, the flow rate of the solution C is 45 to 55L/h, the reaction pH value is 10.0 to 10.5, the flow rate of the solution B is dynamically adjusted according to the reaction pH value, the reaction temperature is 74 to 78 ℃, the stirring strength is 160 to 180 r/min, and the reaction time is 25 to 30h;
c. sulfur washing
Washing the synthetic slurry in the step b to obtain a small-granularity low-sulfur cobalt hydroxide material; the washing equipment is a filter press, and the washing liquid is deionized water at the temperature of 80-90 ℃; the sulfur content of the small-granularity low-sulfur cobalt hydroxide material is less than or equal to 0.005 percent;
d. calcination of
Calcining the small-granularity low-sulfur cobalt hydroxide material in the step d to obtain a small-granularity low-sulfur cobaltosic oxide material;
e. washing sodium, and drying
D, washing sodium and drying the small-granularity low-sulfur cobaltosic oxide material in the step d to obtain a small-granularity low-sodium-sulfur cobaltosic oxide product; the equipment for washing the sodium is a filter press, and the washing liquid is deionized water at 80-90 ℃.
2. The method for preparing small-particle-size low-sodium-sulfur cobaltosic oxide for high-rate lithium cobaltate according to claim 1, wherein the method comprises the following steps: in the step d, the calcining condition is calcining in a rotary kiln, the calcining temperature is 750-780 ℃, and the calcining time is 2-4 h.
3. The method for preparing small-particle-size low-sodium-sulfur cobaltosic oxide for high-rate lithium cobaltate according to claim 2, wherein the method comprises the following steps: the small-granularity low-sulfur cobaltosic oxide material has the laser granularity D 50 Is 4~5μm with tap density not less than 2.0g/cm 3 The specific surface area is 3.0 +/-0.5 m 2 The content of sodium is less than or equal to 0.01 percent and the content of sulfur is less than or equal to 0.005 percent.
4. The method for preparing small-particle-size low-sodium sulfur cobaltosic oxide for high-rate lithium cobaltate according to any one of claims 1 to 3, wherein the method comprises the following steps: in the step e, the drying equipment is a flash evaporation machine, and the moisture content of the dried material is less than or equal to 0.05 percent.
5. The method for preparing small-particle-size low-sodium-sulfur cobaltosic oxide for high-rate lithium cobaltate according to claim 4, wherein the method comprises the following steps: in step e, the light granularity D of the small-granularity low-sodium-sulfur cobaltosic oxide product 50 4~5 μm, tap density ≧ 2.0g/cm 3 The specific surface area is 3.0 +/-0.5 m 2 The sodium content is less than or equal to 0.01 percent and the sulfur content is less than or equal to 0.005 percent, and the shape is spherical or quasi-spherical.
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|---|---|---|---|---|
| CN101585559A (en) * | 2009-06-14 | 2009-11-25 | 宁波科博特钴镍有限公司 | Preparation method of spherical cobaltosic oxide with high battery security |
| CN112408500A (en) * | 2020-11-26 | 2021-02-26 | 格林美（江苏）钴业股份有限公司 | Production method of battery-grade cobalt oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101585559A (en) * | 2009-06-14 | 2009-11-25 | 宁波科博特钴镍有限公司 | Preparation method of spherical cobaltosic oxide with high battery security |
| CN112408500A (en) * | 2020-11-26 | 2021-02-26 | 格林美（江苏）钴业股份有限公司 | Production method of battery-grade cobalt oxide |
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