CN1376638A - Process for preparing Co3O4 - Google Patents
Process for preparing Co3O4 Download PDFInfo
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- CN1376638A CN1376638A CN 02112970 CN02112970A CN1376638A CN 1376638 A CN1376638 A CN 1376638A CN 02112970 CN02112970 CN 02112970 CN 02112970 A CN02112970 A CN 02112970A CN 1376638 A CN1376638 A CN 1376638A
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- cobalt
- tricobalt tetroxide
- precipitation agent
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Abstract
A process for preparing Co3O4 includes such steps as dissolving Co in nitric acid, hydrochloric acid or sulfuric acid to generate cobolt nitrate (or sulfate, or chloride), dissolving precipitant and complexing agent in deionized water to prepare saturated solution, adding the prepared to solution to reactor, regulating pH=4-5.5, adding complexing precipitant at 35-100 deg.c while stirring, reacting, filtering, washing with deionized water at temp higher than 90 deg.C, calcining at 300-1000 deg.C for 5-25 hr, pulverizing and classifying.
Description
Technical field
The present invention relates to a kind of manufacture method of tricobalt tetroxide, be used for the raw material of lithium ion cell anode material lithium cobaltate, also can be used for fuel cell material, catalyzer, magneticsubstance, electronic material, belong to inorganic materials and make the field.
Background technology
In recent years along with the sharp increase in notebook computer, mobile phone, small-sized electronic product market, the successful exploitation of electromobile, lithium ion battery market enlarges rapidly, its positive electrode material mainly is a cobalt acid lithium, and the critical material of cobalt acid lithium production is a tricobalt tetroxide, because the particular requirement of cobalt acid lithium material Chemical Composition and physicals, the Chemical Composition of its starting material tricobalt tetroxide and physicals are very big to cobalt acid lithium performance impact.The tricobalt tetroxide that general chemical process is produced is very common a kind of, " tricobalt tetroxide " (national science and technology achievement storehouse sequence number 9362001000108) as Chinese science and technology achievement report uses self-produced high-quality cobalt compound special synthetic as raw material, it is a kind of common cobalt compound, can finally influence crystal formation, pine ratio and the density of battery-grade cobaltosic oxide.
The employing and the synthetic cobaltous hydroxide of stream that disclose of Japanese Patent " manufacture method of tricobalt tetroxide " (spy opens flat 11-292548) and for example, the calcining cobaltous hydroxide prepares the way of tricobalt tetroxide, and its complex process, building-up process are difficult to control, and investment is big, the cost height.
Summary of the invention
Purpose of the present invention is exactly in order to address the above problem, the manufacture method of propose that a kind of particle diameter is big, density is high, crystalline structure is complete, technology is simple, cost is low, producing manageable tricobalt tetroxide.
Technical solution of the present invention: 1, a kind of manufacture method of tricobalt tetroxide, its step comprises:
A. prepare cobalt liquor
Adopt nitric acid, hydrochloric acid or sulfuric acid dissolution cobalt metal to generate Xiao Suangu, rose vitriol or cobalt chloride, cobalt contents 50-200g/l in the solution;
B. prepare the complex-precipitation agent
Precipitation agent, complexing agent are dissolved in the deionized water, the preparation saturated solution, wherein, cobalt: precipitation agent: the mol ratio of complexing agent=1.0: 0.5-5.0: 0.01-2.0;
C. prepare cobalt salt
The cobalt liquor of preparation is added in the reactor of band thermometer, agitator, adjust PH=4.0-5.5, in 35 ℃-100 ℃ adding complex-precipitation agent, the reaction end pH value is between 7.0-8.0 under agitation condition;
D. with the cobalt salt slurry filtration, and with 〉=90 ℃ deionized water wash;
E. with cobalt salt oven dry, pulverize or directly will wash the calcining furnace that good cobalt salt places adjustable air atmosphere, at 300-1000 ℃ of temperature lower calcination 5-25 hour, through pulverize, classification acquisition tricobalt tetroxide.
Tricobalt tetroxide of the present invention is exactly the product of a kind of Chemical Composition and physicals uniqueness, can satisfy the requirement that cobalt acid lithium is produced, particularly use a kind of cobalt salt of complex-precipitation prepared, the tricobalt tetroxide that obtains through calcining, particle diameter is big, density is high, crystalline structure is complete, technology is simple, cost is low, produces control easily, is a kind of method that is suitable for suitability for industrialized production.The present invention is starting raw material with the cobalt metal, a kind of cobalt salt of complex-precipitation preparation, and it is not a kind of common cobalt compound, can not influence crystal formation, pine ratio and the density of battery-grade cobaltosic oxide eventually.The present invention has following advantage:
1, adopt complex-precipitation technology, make a kind of cobalt salt, can effectively control crystalline form, granularity, the density of the finished product, and be easy to washing, as raw material, be easy to make tricobalt tetroxide of the present invention, technology is simple, and cost is low.
2, with slurry filtration, washing, the oven dry of cobalt salt or directly will wash good cobalt salt calcining through pulverize, the classification operation, the particle diameter of may command the finished product and size-grade distribution.
3, its Chemical Composition of tricobalt tetroxide of the present invention and physicals all can satisfy the requirement of lithium ion battery material Chemical Composition and physicals, also can be used for fuel cell material, and remarkable economic efficiency and social benefit are arranged.
Embodiment
The present invention is to be starting raw material with the cobalt metal, adopts complex-precipitation technology, makes a kind of cobalt salt, after filtration, washing, calcining, pulverizing, classification make tricobalt tetroxide, its Co content 73.0-74.0%, loose density 0.7-1.4g/m
3, tap density 〉=2g/m
3, average particulate diameter 1-10 μ m under 4500 times of electron microscopes, spinel structure.
Technology of the present invention is as follows:
1. the preparation of cobalt liquor
Adopt nitric acid, hydrochloric acid or sulfuric acid dissolution cobalt metal to generate Xiao Suangu, rose vitriol or cobalt chloride, cobalt contents 50-200g/l in the solution.Above-mentioned three kinds of strong acid can singlely use, and also can adopt mixed strong acids to prepare cobalt liquor as required.
2. the preparation of complex-precipitation agent
With precipitation agent yellow soda ash, sodium bicarbonate, bicarbonate of ammonia, urea, one or more of complexing agent EDTA, ammoniacal liquor, citric acid are dissolved in the deionized water, the preparation saturated solution, wherein, cobalt: precipitation agent: the mol ratio of complexing agent=1.0: 0.5-5.0: 0.01-2.0.
3. the preparation of cobalt salt
The cobalt liquor of preparation is added in the reactor of band thermometer, agitator, adjust PH=4.0-5.5, in 35 ℃-100 ℃ adding complex-precipitation agent, the reaction end pH value is between 7.0-8.0 under agitation condition.
4. with the cobalt salt slurry filtration, and with 〉=90 ℃ deionized water wash.
With cobalt salt oven dry, pulverize or directly will wash the calcining furnace that good cobalt salt places adjustable air atmosphere, at 300-1000 ℃ of temperature lower calcination 5-25 hour, through pulverize, classification acquisition tricobalt tetroxide.
The tricobalt tetroxide that the present invention makes, Co content 73.0-74.0%, loose density 0.7-1.4g/m
3, tap density 〉=2.0g/m
3Average particulate diameter 1-10 μ m under 4500 times of electron microscopes, features such as spinel structure are based on the requirement of cobalt acid lithium, cobalt acid lithiumation composition, physicals as feedstock production can satisfy the requirement that lithium ion battery is produced, and also can be used for fuel cell material.
In the aforesaid method, the cobalt salt of complex-precipitation prepared in reaction, its cobalt contents 〉=45%, loose density 0.3-0.5g/m
3The preparation of this cobalt salt finally influences crystalline structure, granularity and the density of tricobalt tetroxide.The cobalt salt of complex-precipitation prepared in reaction is filtered, after the washing, places the calcining furnace of adjustable air atmosphere, in 300 °-1000 ℃ calcinings 5-25 hour, and particle diameter and density by calcination time and temperature control the finished product.Through pulverizing, classification operation, can effectively control the size distribution of tricobalt tetroxide.
Below by example and comparative example the present invention is further described; be necessary to illustrate that following example only is used for invention is further specified; can not be interpreted as the restriction to present method protection domain, those skilled in the art can make some nonessential improvement and adjustment to the present invention by foregoing according to the present invention.
Example 1. is dissolved in cobalt metal in the nitric acid, and the cobalt contents 60g/l of cobalt nitrate solution is dissolved in preparation complex-precipitation agent in the deionized water with bicarbonate of ammonia, EDTA, and its consumption is: Co: NH
4HCO
3: EDTA=1: 2.5: 0.3 (mole), get in the reactor that above-mentioned cobalt nitrate solution 200l adds belt stirrer and thermometer, under stirring condition, when 45 ℃ of temperature, the complex-precipitation agent of preparation is added reaction kettle for reaction.Finish reaction during PH=7.2, sedimentary cobalt salt is filtered, use, place strand burning stove, calcine pulverizing, classification gained tricobalt tetroxide Co content 73.6%, loose density 1.0g/m 14 hours in 300 °-1000 ℃ of temperature greater than 90 ℃ deionized water wash 7 times
3, tap density 2.6g/m
3, average particulate diameter 3 μ m under 4500 times of electron microscopes.
Example 2. is with in the cobalt metal vitriolization, and cobalt contents 100g/l in the cobalt sulfate solution is dissolved in preparation complex-precipitation agent, wherein Co: NH in the deionized water with bicarbonate of ammonia, ammoniacal liquor
4HCO
3: NH
3.H
2O=1: 1.0: 1.0 (mole), get in the reactor of above-mentioned cobalt sulfate solution 200l adding belt stirrer and thermometer, under agitation condition, complex-precipitation agent with preparation when 90 ℃ of temperature adds reaction kettle for reaction, finishes reaction during PH=7.4, and sedimentary cobalt salt is filtered, use greater than 90 ℃ of deionized water wash 8 times, place calcining furnace in 300 °-1000 ℃ calcinings of temperature 18 hours, pulverizing, classification gained tricobalt tetroxide Co content 73.3%, loose density 1.0g/m
3, tap density 2.5g/m
3, average particulate diameter 5 μ m under 4500 times of electron microscopes.
Example 3. is dissolved in cobalt metal in the nitric acid, and the cobalt contents 60g/l of cobalt nitrate solution is dissolved in yellow soda ash, ammoniacal liquor in the deionized water Co: Na
2CO
3: NH
3.H
2O=1: 1.1: 2.0 (mole), get in the reactor of above-mentioned cobalt nitrate solution 200l adding belt stirrer and thermometer, under agitation condition, complex-precipitation agent with preparation when 70 ℃ of temperature adds reaction kettle for reaction, finishes reaction during PH=7.6, and sedimentary cobalt salt is filtered, use greater than 90 ℃ of deionized water wash 6 times, place calcining furnace in 300 °-1000 ℃ calcinings of temperature 20 hours, pulverizing, classification gained tricobalt tetroxide Co of the present invention content 73.5%, loose density 0.9g/m
3, tap density 2.5g/m
3, average particulate diameter 6 μ m under 4500 times of electron microscopes.
Example 4. is with in the cobalt metal vitriolization, the cobalt contents 80g/l of cobalt sulfate solution, ammoniacal liquor, citric acid, yellow soda ash are dissolved in preparation complex-precipitation agent in the deionized water, and its consumption is cobalt: ammoniacal liquor: citric acid: the mol ratio of yellow soda ash=1: 0.5: 0.4: 1.05.Get in the reactor of above-mentioned cobalt sulfate solution 200l adding belt stirrer and thermometer, under agitation condition, complex-precipitation agent with preparation when 85 ℃ of temperature adds reaction kettle for reaction, finishes reaction during PH=7.6, and sedimentary cobalt salt is filtered, use greater than 90 ℃ of deionized water wash 8 times, oven dry, pulverizing are placed on calcining furnace, at temperature 300-1000 ℃ of calcining 15 hours, pulverizing, classification gained tricobalt tetroxide of the present invention, Co content 73.0%, loose density 0.8g/m
3, tap density 2.2g/m
3, average particulate diameter 3-5 μ m under 4000 times of electron microscopes.
Example 5. is dissolved in cobalt metal in the nitric acid, and the cobalt contents 100g/l of cobalt nitrate solution is dissolved in bicarbonate of ammonia, urea, ammoniacal liquor in the deionized water, and its consumption is cobalt: ammoniacal liquor: bicarbonate of ammonia: the mol ratio of urea=1: 2.0: 0.6: 0.5.Get in the reactor of above-mentioned cobalt nitrate solution 200l adding belt stirrer and thermometer, under agitation condition, complex-precipitation agent with preparation when 90 ℃ of temperature adds reaction kettle for reaction, finishes reaction during PH=7.0, and sedimentary cobalt salt is filtered, use greater than 90 ℃ of deionized water wash 6 times, place calcining furnace, in temperature 300-1000 ℃ of calcining 18 hours, pulverizing, classification gained tricobalt tetroxide of the present invention, Co content 73.6%, loose density 1.2g/m
3, tap density 2.5g/m
3, average particulate diameter 3-5 μ m under 4000 times of electron microscopes.
Comparative example: cobalt nitrate solution (cobalt contents 60g/l) is added unsaturated carbonate hydrogen ammonium solution to PH=7.2-7.6, be heated to 70 ℃ of stirrings, reacted 30 minutes, filtration washing, oven dry, pulverizing are placed on calcining furnace in 850 ℃ of calcinings of temperature 10 hours, pulverizing, classification gained tricobalt tetroxide, Co content 73.2%, loose density 0.6g/m
3, tap density 1.8g/m
3, average particulate diameter 3 μ m under 4500 times of electron microscopes.
Claims (5)
1, a kind of manufacture method of tricobalt tetroxide, its step comprises:
A. prepare cobalt liquor
Adopt nitric acid, hydrochloric acid or sulfuric acid dissolution cobalt metal to generate Xiao Suangu, rose vitriol or cobalt chloride, cobalt contents 50-200g/l in the solution;
B. prepare the complex-precipitation agent
Precipitation agent, complexing agent are dissolved in the deionized water, the preparation saturated solution, wherein, cobalt: precipitation agent: the mol ratio of complexing agent=1.0: 0.5-5.0: 0.01-2.0;
C. prepare cobalt salt
The cobalt liquor of preparation is added in the reactor of band thermometer, agitator, adjust PH=4.0-5.5, in 35 ℃-100 ℃ adding complex-precipitation agent, the reaction end pH value is between 7.0-8.0 under agitation condition;
D. with the cobalt salt slurry filtration, and with 〉=90 ℃ deionized water wash;
E. with cobalt salt oven dry, pulverize or directly will wash the calcining furnace that good cobalt salt places adjustable air atmosphere, at 300-1000 ℃ of temperature lower calcination 5-25 hour, through pulverize, classification acquisition tricobalt tetroxide.
2, by the manufacture method of the described tricobalt tetroxide of claim 1, it is characterized in that described three kinds of strong acid or single use, or adopt mixed strong acids to prepare cobalt liquor as required.
3, by the manufacture method of the described tricobalt tetroxide of claim 1, it is characterized in that described precipitation agent adopts yellow soda ash, sodium bicarbonate, bicarbonate of ammonia, urea, they or use separately, or mix and use.
4, by the manufacture method of the described tricobalt tetroxide of claim 1, it is characterized in that described complexing agent is EDTA, ammoniacal liquor, citric acid, they or use separately, or mix and use.
5, by the manufacture method of the described tricobalt tetroxide of claim 1, it is characterized in that the tricobalt tetroxide that described method makes, Co content 73.0-74.0%, loose density 0.7-1.4g/m
3, tap density 〉=2.0g/m
3, average particulate diameter 1-10 μ m under 4500 times of electron microscopes, spinel structure.
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|---|---|---|---|---|
| CN1302999C (en) * | 2004-06-03 | 2007-03-07 | 曾福兴 | Method for manufacturing high-density cobaltosic oxide |
| CN1331761C (en) * | 2005-05-13 | 2007-08-15 | 中南大学 | Solid phase interface induced precipitation method for preparing nickel oxide, cobalt oxide powder |
| CN100345324C (en) * | 2005-09-06 | 2007-10-24 | 天津力神电池股份有限公司 | Method for preparing lithium ion cell cobaltic-cobaltous oxide negative pole material |
| CN100348502C (en) * | 2004-06-27 | 2007-11-14 | 曾福兴 | Process for preparing high purity cobalto-cobaltic oxide |
| CN100363099C (en) * | 2005-09-16 | 2008-01-23 | 山西大学 | CO low temperature oxidation catalyst and its preparation process |
| CN100398454C (en) * | 2004-06-28 | 2008-07-02 | 南通奥克赛德新材料有限公司 | New process for preparing high quality Co3O4 |
| CN101509069B (en) * | 2009-03-30 | 2010-10-06 | 南通新玮镍钴科技发展有限公司 | Method for selective solvent extraction of heterogenite with full-wet-process |
| CN101913659A (en) * | 2010-08-10 | 2010-12-15 | 江苏东新能源科技有限公司 | Battery-grade cobaltosic oxide preparation method |
| CN101982422A (en) * | 2010-10-21 | 2011-03-02 | 江苏东新能源科技有限公司 | Method for preparing cobaltosic oxide with large grain size and high safety |
| CN101982421A (en) * | 2010-10-21 | 2011-03-02 | 江苏东新能源科技有限公司 | Preparation method of nano cobalt oxide |
| CN101508471B (en) * | 2009-03-30 | 2011-08-24 | 南通新玮镍钴科技发展有限公司 | Process for producing cobaltic-cobaltous oxide |
| CN104058468A (en) * | 2013-03-19 | 2014-09-24 | 南通瑞翔新材料有限公司 | Compact spherical cobalt oxide and preparation method thereof |
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| CN106082358A (en) * | 2016-06-22 | 2016-11-09 | 荆门市格林美新材料有限公司 | The preparation method of Cobalto-cobaltic oxide |
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| CN114634211A (en) * | 2022-03-17 | 2022-06-17 | 宜昌邦普时代新能源有限公司 | Preparation method and application of tin-based lithium cobaltate precursor |
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2002
- 2002-04-22 CN CNB021129703A patent/CN1151971C/en not_active Expired - Fee Related
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|---|---|---|---|---|
| CN1302999C (en) * | 2004-06-03 | 2007-03-07 | 曾福兴 | Method for manufacturing high-density cobaltosic oxide |
| CN100348502C (en) * | 2004-06-27 | 2007-11-14 | 曾福兴 | Process for preparing high purity cobalto-cobaltic oxide |
| CN100398454C (en) * | 2004-06-28 | 2008-07-02 | 南通奥克赛德新材料有限公司 | New process for preparing high quality Co3O4 |
| CN1331761C (en) * | 2005-05-13 | 2007-08-15 | 中南大学 | Solid phase interface induced precipitation method for preparing nickel oxide, cobalt oxide powder |
| CN100345324C (en) * | 2005-09-06 | 2007-10-24 | 天津力神电池股份有限公司 | Method for preparing lithium ion cell cobaltic-cobaltous oxide negative pole material |
| CN100363099C (en) * | 2005-09-16 | 2008-01-23 | 山西大学 | CO low temperature oxidation catalyst and its preparation process |
| CN101508471B (en) * | 2009-03-30 | 2011-08-24 | 南通新玮镍钴科技发展有限公司 | Process for producing cobaltic-cobaltous oxide |
| CN101509069B (en) * | 2009-03-30 | 2010-10-06 | 南通新玮镍钴科技发展有限公司 | Method for selective solvent extraction of heterogenite with full-wet-process |
| CN101913659A (en) * | 2010-08-10 | 2010-12-15 | 江苏东新能源科技有限公司 | Battery-grade cobaltosic oxide preparation method |
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| CN101982422A (en) * | 2010-10-21 | 2011-03-02 | 江苏东新能源科技有限公司 | Method for preparing cobaltosic oxide with large grain size and high safety |
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| CN110420639A (en) * | 2019-08-08 | 2019-11-08 | 中南大学 | A kind of cobaltosic oxide material and its methods for making and using same |
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| CN112661200A (en) * | 2020-12-24 | 2021-04-16 | 格林美（江苏）钴业股份有限公司 | Synthetic method of cobaltosic oxide with high tap density |
| CN113233516A (en) * | 2021-05-28 | 2021-08-10 | 金川集团股份有限公司 | Preparation method of single crystal small-granularity cobaltosic oxide |
| CN113620350A (en) * | 2021-08-19 | 2021-11-09 | 珠海市科立鑫金属材料有限公司 | Preparation method of large-particle cobaltosic oxide |
| CN114634211A (en) * | 2022-03-17 | 2022-06-17 | 宜昌邦普时代新能源有限公司 | Preparation method and application of tin-based lithium cobaltate precursor |
| CN114634211B (en) * | 2022-03-17 | 2024-04-09 | 宜昌邦普时代新能源有限公司 | Preparation method and application of tin-based lithium cobalt oxide precursor |
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|---|---|
| CN1151971C (en) | 2004-06-02 |
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