CN115849459A - Preparation method and application of cobalt hydroxide - Google Patents
Preparation method and application of cobalt hydroxide Download PDFInfo
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- CN115849459A CN115849459A CN202211704972.XA CN202211704972A CN115849459A CN 115849459 A CN115849459 A CN 115849459A CN 202211704972 A CN202211704972 A CN 202211704972A CN 115849459 A CN115849459 A CN 115849459A
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- Prior art keywords
- cobalt
- cobalt hydroxide
- solution
- ascorbic acid
- preparation
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- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 title claims abstract description 53
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 70
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 35
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 35
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 35
- 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 abstract description 21
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 9
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 9
- 239000010941 cobalt Substances 0.000 claims abstract description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000654 additive Substances 0.000 claims abstract description 8
- 230000000996 additive effect Effects 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 229910001429 cobalt ion Inorganic materials 0.000 claims description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002002 slurry Substances 0.000 description 16
- 239000002585 base Substances 0.000 description 12
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 12
- 239000011248 coating agent Substances 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 230000032683 aging Effects 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 230000002572 peristaltic effect Effects 0.000 description 5
- 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 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- -1 cobalt oxyhydroxide Chemical compound 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Images
Abstract
The invention discloses a preparation method and application of cobalt hydroxide, wherein the preparation method comprises the steps of mixing and reacting a cobalt solution, alkali liquor and an additive; the additive comprises ascorbic acid and hydrazine hydrate; the preparation method of the cobalt hydroxide realizes the control of the specific surface area of the cobalt hydroxide by adjusting the addition amount of each component, and the specific surface area of the prepared cobalt hydroxide is 35m 2 /g~45m 2 /g。
Description
Technical Field
The invention relates to the technical field of battery material preparation, in particular to a preparation method and application of cobalt hydroxide.
Background
Lithium ion batteries are widely used because of their advantages of high energy density, long cycle life, high operating voltage, high safety, and small self-discharge effect. With the development of lithium batteries, higher requirements are put on the lithium batteries, which means that higher requirements are put on key materials, particularly positive electrode materials. Surface coating is a method for improving the performance of the cathode material. However, the coating material cobalt hydroxide in the existing method has a small specific surface area and a limited coating effect, and the application of the anode material is limited.
Therefore, it is necessary to develop a method for preparing cobalt hydroxide, which can solve the problems of the existing cobalt hydroxide coating material, such as small specific surface area and poor coating property.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a preparation method of cobalt hydroxide, which can solve the problems of small specific surface area and poor coating property of the existing cobalt hydroxide coating material.
According to the first aspect of the invention, the preparation method of cobalt hydroxide comprises the steps of mixing and reacting a cobalt solution, an alkali liquor and an additive;
the additive comprises ascorbic acid and hydrazine hydrate;
340-350 g of alkali liquor and 1-2 parts of ascorbic acid in parts by weight.
According to some embodiments of the invention, the method of preparing cobalt hydroxide comprises:
s1, mixing the alkali liquor and the additive to obtain a solution A;
and S2, adding a cobalt solution into the solution A for mixing reaction.
According to an embodiment of the first aspect of the invention, at least the following advantages are achieved:
the invention discloses a preparation method of cobalt hydroxide with a large specific surface. The specific surface area of the coating material such as cobalt hydroxide on the market at present is 15-25 m 2 The specific surface area is smaller between/g. In the cobalt hydroxide prepared by the invention, in the reaction process of adding additives (ascorbic acid and hydrazine hydrate), the ascorbic acid plays a hydroxylation role, the hydrazine hydrate plays an antioxidation role, and the rapid synthesis of the reaction is promoted, so that the crystal structure of the cobalt hydroxide is changed, the sheet structure of primary particles of the cobalt hydroxide tends to be thinner and thinner, and the specific surface area of the cobalt hydroxide is enlarged; the cobalt hydroxide prepared by the method has the specific surface area of 35m 2 /g~45m 2 The specific surface area of the cobalt hydroxide can be controlled by adjusting the amount of the ascorbic acid between the concentration and the concentration.
According to some embodiments of the invention, step S2 further comprises filtering the cobalt liquid.
According to some embodiments of the invention, step S2 includes adding solution a to the pH-adjusted aqueous ammonia solution with a peristaltic pump.
According to some embodiments of the present invention, the alkali solution is 340-350 g, the ascorbic acid is 1-2 parts, and the hydrazine hydrate is 1-2 parts by weight.
According to some embodiments of the present invention, the alkali solution is 340 to 350g, the ascorbic acid is 1 to 1.2 parts, and the hydrazine hydrate is 1 to 2 parts by weight.
According to some embodiments of the invention, the lye further comprises at least one of an aqueous potassium hydroxide solution, an aqueous sodium hydroxide solution and an aqueous lithium hydroxide solution.
According to some embodiments of the present invention, the concentration of cobalt ions in the cobalt solution is 1.5-2.5 mol/L.
According to some embodiments of the invention, in step S2, the cobalt solution is added to the solution a, and the time of the addition process is 30-40 min.
According to some embodiments of the invention, the mixing reaction further comprises aging in step S2.
According to some embodiments of the invention, the aging time is 2 to 3 hours.
According to some embodiments of the invention, the aging further comprises drying.
According to some embodiments of the invention, the drying time is 95 to 105 ℃.
According to some embodiments of the invention, the drying time is 12 to 13 hours.
According to some embodiments of the invention, the mass concentration of the hydrazine hydrate in the cobalt solution is 40-80%.
According to some embodiments of the invention, the temperature of the mixing reaction is between 35 and 55 ℃.
According to some embodiments of the invention, the mixing reaction time is 2 to 4 hours.
According to some embodiments of the invention, the reaction is carried out under an atmosphere of an inert gas.
According to some embodiments of the invention, the inert gas comprises nitrogen.
According to some embodiments of the invention, the inert gas atmosphere has a flow rate of the inert gas of 10 to 12L/min.
According to some embodiments of the invention, the reaction comprises a stirred reaction.
According to some embodiments of the invention, the rotation speed of the stirring reaction is 400 to 800r/min.
An embodiment according to the second aspect of the present invention proposes an electrode whose preparation raw material includes the cobalt hydroxide.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a Scanning Electron Microscope (SEM) picture of a product obtained in example 1;
FIG. 2 is a Scanning Electron Microscope (SEM) picture of a product obtained in example 1;
FIG. 3 is a Scanning Electron Microscope (SEM) picture of the dried and crushed product obtained in example 1;
FIG. 4 is a Scanning Electron Microscope (SEM) picture of the dried and crushed product obtained in example 1.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
Example 1
The embodiment discloses a preparation method of cobalt hydroxide, which comprises the following steps:
s1: weighing 954.55g of cobalt chloride, adding pure water, fixing the volume to 2.1L, and filtering to remove solid impurities to obtain a cobalt chloride solution;
s2: weighing 1g of ascorbic acid and 0.4ml of hydrazine hydrate solution, adding the ascorbic acid and the hydrazine hydrate solution into 800ml of sodium hydroxide solution, starting stirring and nitrogen protection, wherein the stirring frequency is 400r/min, and the nitrogen flow is 10L/min, and uniformly mixing to obtain a base solution;
s3: heating the base solution obtained in the step S2 to 45 ℃, pumping a cobalt chloride solution into the base solution within 30min by using a peristaltic pump, and aging for 2h to obtain cobalt hydroxide slurry;
s4: and (3) washing the sodium content of the cobalt hydroxide slurry to be below 500ppm, then pressing the slurry to be dry, putting the dried slurry into a drying box, and keeping the temperature at 95 ℃ for 12 hours to obtain a cobalt hydroxide sample.
FIG. 1 is a Scanning Electron Microscope (SEM) picture of a product obtained in example 1;
FIG. 2 is a Scanning Electron Microscope (SEM) picture of a product obtained in example 1;
FIG. 3 is a Scanning Electron Microscope (SEM) picture of the dried and crushed product obtained in example 1;
FIG. 4 is a Scanning Electron Microscope (SEM) picture of the dried and crushed product obtained in example 1.
Example 2
The embodiment discloses a preparation method of cobalt hydroxide, which comprises the following steps:
s1: weighing 954.55g of cobalt chloride, adding pure water, fixing the volume to 2.1L, and filtering to remove solid impurities to obtain a cobalt chloride solution;
s2: weighing 1g of ascorbic acid and 0.4ml of hydrazine hydrate solution, adding the ascorbic acid and the hydrazine hydrate solution into 800ml of sodium hydroxide solution, starting stirring and nitrogen protection, wherein the stirring frequency is 400r/min, and the nitrogen flow is 10L/min, and uniformly mixing the ascorbic acid and the hydrazine hydrate solution to obtain a base solution;
s3: heating the base solution obtained in the step S2 to 45 ℃, pumping the cobalt chloride solution into the base solution by using a peristaltic pump within 30min, and aging for 2h to obtain cobalt hydroxide slurry;
s4: and (3) washing the sodium content of the cobalt hydroxide slurry to be below 500ppm, then pressing the slurry to be dry, putting the slurry into a drying box, and keeping the temperature at 95 ℃ for 12 hours to obtain a cobalt hydroxide sample.
Example 3
The embodiment discloses a preparation method of cobalt hydroxide, which comprises the following steps:
s1: weighing 954.55g of cobalt chloride, adding pure water, fixing the volume to 2.1L, and filtering to remove solid impurities to obtain a cobalt chloride solution;
s2: weighing 1g of ascorbic acid and 0.4ml of hydrazine hydrate solution, adding the ascorbic acid and the hydrazine hydrate solution into 800ml of sodium hydroxide solution, starting stirring and nitrogen protection, wherein the stirring frequency is 400r/min, and the nitrogen flow is 10L/min, and uniformly mixing the ascorbic acid and the hydrazine hydrate solution to obtain a base solution;
s3: heating the base solution obtained in the step S2 to 45 ℃, pumping the cobalt chloride solution into the base solution by using a peristaltic pump within 30min, and aging for 2h to obtain cobalt hydroxide slurry;
s4: and (3) washing the sodium content of the cobalt hydroxide slurry to be below 500ppm, then pressing the slurry to be dry, putting the slurry into a drying box, and keeping the temperature at 95 ℃ for 12 hours to obtain a cobalt hydroxide sample.
Example 5
The embodiment discloses a preparation method of cobalt hydroxide, which comprises the following steps:
s1: weighing 954.55g of cobalt chloride, adding pure water, fixing the volume to 2.1L, and filtering to remove solid impurities to obtain a cobalt chloride solution;
s2: weighing 1g of ascorbic acid and 0.4ml of hydrazine hydrate solution, adding the ascorbic acid and the hydrazine hydrate solution into 800ml of sodium hydroxide solution, starting stirring and nitrogen protection, wherein the stirring frequency is 400r/min, and the nitrogen flow is 10L/min, and uniformly mixing the ascorbic acid and the hydrazine hydrate solution to obtain a base solution;
s3: heating the base solution obtained in the step S2 to 45 ℃, pumping a cobalt chloride solution into the base solution within 30min by using a peristaltic pump, and aging for 2h to obtain cobalt hydroxide slurry;
s4: and (3) washing the sodium content of the cobalt hydroxide slurry to be below 500ppm, then pressing the slurry to be dry, putting the slurry into a drying box, and keeping the temperature at 95 ℃ for 12 hours to obtain a cobalt hydroxide sample.
Example 6
This example discloses a method for preparing cobalt hydroxide, and differs from example 1 in that ascorbic acid is added in an amount of 1.1g in step S2, and the rest is the same.
Example 7
This example discloses a method for preparing cobalt hydroxide, and is different from example 2 in that ascorbic acid is added in an amount of 1.1g in step S2, and the rest is the same.
Example 8
This example discloses a method for preparing cobalt hydroxide, and differs from example 3 in that ascorbic acid is added in an amount of 1.1g in step S2, and the rest is the same.
Example 9
This example discloses a method for preparing cobalt hydroxide, and differs from example 4 in that ascorbic acid is added in an amount of 1.1g in step S2, and the rest is the same.
Example 10
This example discloses a method for preparing cobalt hydroxide, and differs from example 5 in that ascorbic acid is added in an amount of 1.1g in step S2, and the rest is the same.
Example 11
This example discloses a method for preparing cobalt hydroxide, and differs from example 1 in that ascorbic acid is added in an amount of 1.2g in step S2, and the rest is the same.
Example 12
This example discloses a method for preparing cobalt hydroxide, and is different from example 2 in that ascorbic acid is added in an amount of 1.2g in step S2, and the rest is the same.
Example 13
This example discloses a method for preparing cobalt hydroxide, and differs from example 3 in that ascorbic acid is added in an amount of 1.2g in step S2, and the rest is the same.
Example 14
This example discloses a method for preparing cobalt hydroxide, and differs from example 4 in that ascorbic acid is added in an amount of 1.2g in step S2, and the rest is the same.
Example 15
This example discloses a method for preparing cobalt hydroxide, and differs from example 5 in that ascorbic acid is added in an amount of 1.2g in step S2, and the rest is the same.
Test example 1
In the test example, the physicochemical indexes and the sections of the cobalt oxyhydroxide samples prepared in the above examples are subjected to electron microscope detection, and the results are shown in table 1.
Table 1 results of performance testing
According to the description in Table 1, the specific surface area of the cobalt hydroxide prepared by the present invention is 35m 2 /g~45m 2 And the specific surface area of the cobalt hydroxide is regulated and controlled by regulating the amount of the ascorbic acid between the concentration of the ascorbic acid and the concentration of the ascorbic acid.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention.
Claims (10)
1. The preparation method of the cobalt hydroxide is characterized by comprising the steps of mixing and reacting a cobalt solution, alkali liquor and an additive;
the additive comprises ascorbic acid and hydrazine hydrate;
340-350 g of alkali liquor and 1-2 parts of ascorbic acid in parts by weight.
2. The preparation method according to claim 1, characterized in that, by weight, 340 to 350g of the alkali liquor, 1 to 2 parts of the ascorbic acid and 1 to 2 parts of the hydrazine hydrate are calculated.
3. The method of claim 1, wherein the lye further comprises at least one of an aqueous potassium hydroxide solution, an aqueous sodium hydroxide solution and an aqueous lithium hydroxide solution.
4. The method according to claim 1, wherein the cobalt solution has a cobalt ion concentration of 1.5 to 2.5mol/L.
5. The method according to claim 1, wherein the mass concentration of hydrazine hydrate is 40 to 80%.
6. The method according to claim 1, wherein the temperature of the mixing reaction is 35 to 55 ℃.
7. The method according to claim 1, wherein the mixing reaction is carried out for 2 to 4 hours.
8. The production method according to claim 1, characterized in that the reaction is carried out under an inert gas atmosphere; preferably the inert gas comprises nitrogen.
9. The preparation method according to claim 1, wherein the reaction comprises a stirring reaction, and preferably, the rotation speed of the stirring reaction is 400-800 r/min.
10. An electrode, characterized in that the raw material for preparing the electrode comprises cobalt hydroxide prepared by the preparation method according to any one of claims 1 to 9.
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CN202211704972.XA CN115849459B (en) | 2022-12-29 | Preparation method and application of cobalt hydroxide |
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CN202211704972.XA CN115849459B (en) | 2022-12-29 | Preparation method and application of cobalt hydroxide |
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CN115849459B CN115849459B (en) | 2024-05-10 |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101955234A (en) * | 2009-07-15 | 2011-01-26 | 海南金亿新材料股份有限公司 | Method for preparing high purity nano cobalt hydroxide |
CN113753965A (en) * | 2021-08-24 | 2021-12-07 | 广东邦普循环科技有限公司 | Cobalt hydroxide synthesis method and cobalt hydroxide |
CN114835172A (en) * | 2022-05-31 | 2022-08-02 | 荆门市格林美新材料有限公司 | Cobalt hydroxide particles and preparation method and application thereof |
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101955234A (en) * | 2009-07-15 | 2011-01-26 | 海南金亿新材料股份有限公司 | Method for preparing high purity nano cobalt hydroxide |
CN113753965A (en) * | 2021-08-24 | 2021-12-07 | 广东邦普循环科技有限公司 | Cobalt hydroxide synthesis method and cobalt hydroxide |
CN114835172A (en) * | 2022-05-31 | 2022-08-02 | 荆门市格林美新材料有限公司 | Cobalt hydroxide particles and preparation method and application thereof |
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