CN101434417A - Dry preparation of battery grade spherical cobaltosic oxide particle - Google Patents
Dry preparation of battery grade spherical cobaltosic oxide particle Download PDFInfo
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- CN101434417A CN101434417A CNA2008101626905A CN200810162690A CN101434417A CN 101434417 A CN101434417 A CN 101434417A CN A2008101626905 A CNA2008101626905 A CN A2008101626905A CN 200810162690 A CN200810162690 A CN 200810162690A CN 101434417 A CN101434417 A CN 101434417A
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- lithium
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- anode material
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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 relates to a wet preparation method of battery-level spherical cobaltosic oxide, which comprises the specific steps of: preparing cobalt salt into a first mixed solution with the concentration of 1-3mol/L; preparing a hydrate solution with the concentration of 2-10mol/L into a second mixed solution; preparing a complexing agent A with the concentration of 0.001-200g/L into a third mixed solution; introducing the three mixed solutions into a reaction vessel by adopting a parallel flow method; stirring the mixed solution intensively to cause the three solutions to react; adding a certain amount of oxidizer continually into a reaction system during the reaction process; aging the mixed solution for 2-48 hours under normal temperature; centrifugalizing, washing and drying the material; and calcining the mixture of a pretreated precursor and lithium salt under 750-1000 DEG C to obtain the lithium battery cathode material. The method has the advantage that the cobaltosic oxide powder can be directly obtained from the oxidation of a cobalt compound in the solution owing to the fact that the cobalt compound can be oxidized in the solution under alkaline condition. The material is a relatively ideal battery cathode material for mobile telephones, video cameras, laptops and portable electric appliances.
Description
Technical field
The invention belongs to technical field of lithium ion, be specifically related to a kind of precursor of lithium ionic cell positive material---the wet preparation method of battery grade spherical cobaltosic oxide particle.
Background technology
Since Sony corporation of Japan in 1991 was successfully developed lithium cobaltate cathode material, lithium ion battery developed to the industrialization direction rapidly, and widely applied on mobile telephone, pick up camera, notebook computer, portable electronics.Because China is in the advantage of aspects such as resource, labor force, national policy, the lithium ion battery industry development is very fast, has very strong international competitiveness.The cobalt acid lithium production of China was fast-developing in recent years, thereby to Co
3O
4Also corresponding the increasing sharply of demand.Cell-grade Co
3O
4As the main raw material of lithium ion cell anode material lithium cobaltate, also the demand with lithium-ion secondary cell increases.Cell-grade Co
3O
4The Co that uses with traditional industry
3O
4Difference is its purity requirement height, and the physicals (as density, granularity, specific surface area, size distribution, crystal morphology) of product, chemical property, stability etc. are all had very strict requirement.
Chinese invention patent 03148092.6 discloses " preparation method of high purity spherical cobaltic-cobaltous oxide "; Patent of invention 200510015002.9 discloses " preparation method of lithium ion cell cobaltic-cobaltous oxide negative pole material ".The related technology of these two patents has certain enlightenment effect to relevant product.
Co
3O
4Production method roughly can be divided into three major types, that is: vapor phase process, liquid phase method, solid phase method.Co
3O
4The synthetic general calcination or the thermal decomposition method of adopting of micro mist.The Co that the calcination method makes
3O
4Micro mist purity is low, granularity is bigger, the requirement that size-grade distribution is wide, sintering activity is poor, physicochemical property are difficult to reach electronic industry; Thermal decomposition method is generally selected CoAc
2, CoC
2O
4, Co (OH) 2, divalent cobalt such as CoCO3 thermolysis at a certain temperature obtain, and the problem of this method is that energy expenditure is big, the Co that obtains
3O
4Poor activity.Famous scholar Huang Kelong etc. has utilized Hydrothermal Preparation mono-dispersed nano Co
3O
4The powder theory, the shortcoming point is to adapt to suitability for industrialized production.Famous scholar Ni Haiyong etc. have prepared by conditions such as control precipitation agent consumption, dosage of surfactant and kinds that dispersing property is good, spheric Co
3O
4Powder, used precipitation agent are NH
4HCO
3, the application of high-molecular weight tensio-active agent causes certain difficulty to sedimentation and filtration.The refined grade of famous scholar Zhong Wen is with Co (NO
3)
2, H
2O
2, NaOH is a raw material, the synthetic Co of direct oxidation from the aqueous solution
3O
4, but containing the oxyhydroxide and the hydrate thereof of part cobalt in the precipitation, product drying, calcining back are about the coacervate of the particle of 0.5 μ m for particle diameter.Therefore, reunion how to eliminate particle is the subject matter that preparation tricobalt tetroxide particulate need solve.Famous scholar's Li Yadong etc. has been reported with Na
2CO
3For precipitation agent prepares Co
3O
4, throw out is difficult to realize solid-liquid separation, and is adsorbed on impurity Na+ on the micelle and is difficult to washing and eliminates; With NH
4HCO
3Be precipitation agent, the gained precipitation is a cobaltous dihydroxycarbonate, though be easy to solid-liquid separation and washing, just can obtain Co through high-temperature heat treatment
3O
4, the big and granule-morphology of energy consumption is owed.Utilize NH
4HCO
3For precipitation agent prepares cobaltous dihydroxycarbonate or cobaltous carbonate, obtain Co through thermolysis again
3O
4, the problem of existence also has precipitation not exclusively to cause the metal flow vector bigger, and the waste water that contains the ammonia root in a large number needs to handle, and the environmental issue expectation that relates to solves.
Summary of the invention
For overcoming above-mentioned deficiency, the present invention seeks to provide a kind of wet preparation method of battery grade spherical cobaltosic oxide particle to this area.Make its can solve its prepared spherical cobaltic-cobaltous oxide powder size and density evenly, washing easily, technology be simple, easy to operate, realizes suitability for industrialized production easily.The objective of the invention is to realize by the following technical solutions.
A kind of battery-grade cobaltosic oxide preparation method originally, the characteristics of this method are that direct oxidation obtains the spherical cobaltic-cobaltous oxide powder in the aqueous solution, the concrete steps of this method are:
1), cobalt salt is mixed with first mixing solutions that concentration is 1～3mol/L;
2), compound concentration is that the hydroxide solution of 2～10mol/L is second mixing solutions;
3), compound concentration is that the complexing agent A of 0.001～200g/L is the 3rd mixing solutions;
4), adopt and the method for stream feeds first mixing solutions, second mixing solutions, the 3rd mixing solutions in the reaction vessel simultaneously, under violent stirring, the three is reacted, strict pH value and the temperature of reaction controlled of pilot process;
5), in reaction process, constantly in reaction system, add a certain amount of oxygenant;
6), the reaction finish after, constant temperature ageing 2～48 hours;
7), centrifugal, the washing of material, dry oven dry;
8), with pretreated presoma and lithium salts mixture, 750～1000 ℃ of down calcinings, obtain anode material of lithium battery.
Cobalt salt described in above-mentioned described preparation method's the step (1) is a kind of or this two kinds the mixing salt in rose vitriol, the cobalt chloride.
Oxyhydroxide in described preparation method's the step (2) is sodium hydroxide, potassium hydroxide.
Complexing agent A in described preparation method's the step (3) is sodium tartrate, disodium ethylene diamine tetraacetate, quadrol, six methynes, four ammonia, polyacrylamide, citric acid, the 3rd mixing solutions in the step (3) directly join first mixing solutions or second mixing solutions in.
Lithium salts described in described preparation method's the step (8) is a kind of of lithium hydroxide, Quilonum Retard, Lithium Acetate, lithium nitrate, lithium chloride or their mixture.
The pH value span of control of described preparation method's step (4) is PH7～14.
The temperature of reaction of described preparation method's step (4) is 30～90 ℃.
Oxygenant in described preparation method's the step (5) is oxygen, air and hydrogen peroxide.
But the present invention only adopt inexpensive relatively cobalt salt, caustic soda, air and a small amount of complexing agent commonly used just building-up reactions active high, density is high, the powder of even particle size distribution, almost spherical, does not need high-temperature calcination directly to synthesize tricobalt tetroxide from liquid phase.Solved shortcomings such as conventional solid-state method purity is low, granularity is bigger, and size-grade distribution is wide, sintering activity is poor, energy expenditure is big, also solved traditional method, particle is easily reunited, the shortcoming of inconvenience washing.Therefore, but use the inventive method industrialization and produce battery-grade cobaltosic oxide.Advantage is to utilize cobalt compound oxidized characteristic of solution very under alkaline condition, and directly oxidation obtains cobaltosic oxide powder from solution, easily washing, density height, energy consumption is low, technology is simple, and is easy to operate, is easy to realize suitability for industrialized production.Be mobile telephone, pick up camera, notebook computer, a kind of comparatively ideal of portable electronics cell positive material.
Embodiment
Embodiment 1
Preparation 2mol/L rose vitriol feed liquid, in feed liquid, add a certain amount of citric acid, feed liquid and alkali lye simultaneously and stream be passed in the reactor, the pH value of control intermediate reaction is 11, temperature of reaction is 50 ℃, reaction finishes the back and continues constant temperature ageing 10 hours, at 110 ℃ of oven dry down, the loose density 1.7g/cm of the presoma that obtains
3, tap density 2.5g/cm
3
Embodiment 2
Preparation 2mol/L rose vitriol feed liquid, in feed liquid, add a certain amount of six methynes, four ammonia, feed liquid and alkali lye simultaneously and stream be passed in the reactor, the pH value of control intermediate reaction is 11.5, temperature of reaction is 30 ℃, reaction finishes the back and continues constant temperature ageing 10 hours, at 110 ℃ of oven dry down, the loose density 1.6g/cm of the presoma that obtains
3, tap density 2.4g/cm
3
Embodiment 3
Preparation 1mol/L cobalt chloride feed liquid, in feed liquid, add a certain amount of sodium tartrate, feed liquid and alkali lye simultaneously and stream be passed in the reactor, the pH value of control intermediate reaction is 12, temperature of reaction is 45 ℃, reaction finishes the back and continues constant temperature ageing 10 hours, at 110 ℃ of oven dry down, the loose density 1.6g/cm of the presoma that obtains
3, tap density 2.6g/cm
3
Embodiment 4
Preparation 1mol/L cobalt chloride feed liquid, in alkali lye, add a certain amount of disodium ethylene diamine tetraacetate, feed liquid and alkali lye simultaneously and stream be passed in the reactor, the pH value of control intermediate reaction is 10.8, temperature of reaction is 45 ℃, reaction finishes the back and continues constant temperature ageing 10 hours, at 110 ℃ of oven dry down, the loose density 1.6g/cm of the presoma that obtains
3, tap density 2.6g/cm
3
Embodiment 5
Preparation 1.5mol/L cobalt chloride feed liquid, in feed liquid, add a certain amount of disodium ethylene diamine tetraacetate, feed liquid and alkali lye simultaneously and stream be passed in the reactor, the pH value of control intermediate reaction is 9, temperature of reaction is 75 ℃, reaction finishes the back and continues constant temperature ageing 10 hours, at 110 ℃ of oven dry down, the loose density 1.8g/cm of the presoma that obtains
3, tap density 2.8g/cm
3
Embodiment 6
Preparation 1mol/L cobalt chloride feed liquid, the sodium hydroxide solution of 2mol/L, the disodium ethylene diamine tetra-acetic acid solution of 1g/L, feed liquid, sodium hydroxide solution, disodium ethylene diamine tetra-acetic acid solution were passed in the reactor by certain flow while and stream, the pH value of control intermediate reaction is 12, and temperature of reaction is 55 ℃, and reaction finishes the back and continues constant temperature ageing 10 hours, at 110 ℃ of oven dry down, the loose density 1.75g/cm of the presoma that obtains
3, tap density 2.75g/cm
3
Claims (8)
1, a kind of wet preparation method of battery grade spherical cobaltosic oxide particle the method is characterized in that concrete steps are:
1), cobalt salt is mixed with first mixing solutions that concentration is 1～3mol/L;
2), compound concentration is that the hydroxide solution of 2～10mol/L is second mixing solutions;
3), compound concentration is that the complexing agent A of 0.001～200g/L is the 3rd mixing solutions;
4), adopt and the method for stream feeds first mixing solutions, second mixing solutions, the 3rd mixing solutions in the reaction vessel simultaneously, under violent stirring, the three is reacted, strict pH value and the temperature of reaction controlled of pilot process;
5), in reaction process, constantly in reaction system, add a certain amount of oxygenant;
6), the reaction finish after, constant temperature ageing 2～48 hours;
7), centrifugal, the washing of material, dry oven dry;
8), with pretreated presoma and lithium salts mixture, 750～1000 ℃ of down calcinings, obtain anode material of lithium battery.
2, the preparation method of anode material for lithium-ion batteries as claimed in claim 1 is characterized in that the cobalt salt described in described preparation method's the step (1) is a kind of or this two kinds the mixing salt in rose vitriol, the cobalt chloride.
3, the preparation method of anode material for lithium-ion batteries as claimed in claim 1 is characterized in that the oxyhydroxide in described preparation method's the step (2) is sodium hydroxide, potassium hydroxide.
4, the preparation method of anode material for lithium-ion batteries as claimed in claim 1, it is characterized in that the complexing agent A in described preparation method's the step (3) is sodium tartrate, disodium ethylene diamine tetraacetate, quadrol, six methynes, four ammonia, polyacrylamide, citric acid, the 3rd mixing solutions in the step (3) directly join first mixing solutions or second mixing solutions in.
5, the preparation method of anode material for lithium-ion batteries as claimed in claim 1 is characterized in that the lithium salts described in described preparation method's the step (8) is a kind of of lithium hydroxide, Quilonum Retard, Lithium Acetate, lithium nitrate, lithium chloride or their mixture.
6, the preparation method of anode material for lithium-ion batteries as claimed in claim 1 is characterized in that the pH value span of control of described preparation method's step (4) is PH7～14.
7, the preparation method of anode material for lithium-ion batteries as claimed in claim 1 is characterized in that the temperature of reaction of described preparation method's step (4) is 30～90 ℃.
8, the preparation method of anode material for lithium-ion batteries as claimed in claim 1 is characterized in that the oxygenant in described preparation method's the step (5) is oxygen, air and hydrogen peroxide.
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|---|---|---|---|
| CNA2008101626905A CN101434417A (en) | 2008-11-28 | 2008-11-28 | Dry preparation of battery grade spherical cobaltosic oxide particle |
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|---|---|---|---|
| CNA2008101626905A CN101434417A (en) | 2008-11-28 | 2008-11-28 | Dry preparation of battery grade spherical cobaltosic oxide particle |
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| CN101434417A true CN101434417A (en) | 2009-05-20 |
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|---|---|---|---|
| CNA2008101626905A Pending CN101434417A (en) | 2008-11-28 | 2008-11-28 | Dry preparation of battery grade spherical cobaltosic oxide particle |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863518A (en) * | 2010-07-01 | 2010-10-20 | 上海应用技术学院 | Co3O4 nano hollow sphere material and preparation method and application thereof |
| CN101585559B (en) * | 2009-06-14 | 2011-02-16 | 宁波科博特钴镍有限公司 | Preparation method of spherical cobaltosic oxide with high battery security |
| CN102259934A (en) * | 2011-05-17 | 2011-11-30 | 周红阳 | Process for producing high-density spherical cobaltosic oxide by virtue of low temperature liquid phase precipitation oxidization |
| CN102336444A (en) * | 2010-07-16 | 2012-02-01 | 同济大学 | Method for preparing nanoscale disk-like cobaltosic oxide |
| CN103145200A (en) * | 2013-03-25 | 2013-06-12 | 安徽亚兰德新能源材料股份有限公司 | Method for synthesizing spherical cobaltosic oxide through mixing type oxidation |
| CN103274480A (en) * | 2013-06-06 | 2013-09-04 | 南通瑞翔新材料有限公司 | Precursor of polynary positive electrode material for lithium ion battery, and preparation method thereof |
| WO2013130983A2 (en) * | 2012-03-01 | 2013-09-06 | Excellatron Solid State, Llc | Impregnated sintered solid state composite electrode, solid state battery, and methods of preparation |
| CN103318976A (en) * | 2013-07-04 | 2013-09-25 | 中南大学 | Technology for preparing cobaltosic oxide by cobalt-containing solution |
| CN104986807A (en) * | 2015-04-23 | 2015-10-21 | 金川集团股份有限公司 | Spherical tricobalt tetraoxide preparation method |
| CN105668650A (en) * | 2016-03-23 | 2016-06-15 | 荆门市格林美新材料有限公司 | Method for preparing low-sodium cobaltosic oxide |
| CN106340643A (en) * | 2015-07-10 | 2017-01-18 | 北京当升材料科技股份有限公司 | Method for preparing large-grain spherical cobaltosic oxide |
| US9793525B2 (en) | 2012-10-09 | 2017-10-17 | Johnson Battery Technologies, Inc. | Solid-state battery electrodes |
| US10333123B2 (en) | 2012-03-01 | 2019-06-25 | Johnson Ip Holding, Llc | High capacity solid state composite cathode, solid state composite separator, solid-state rechargeable lithium battery and methods of making same |
| US10566611B2 (en) | 2015-12-21 | 2020-02-18 | Johnson Ip Holding, Llc | Solid-state batteries, separators, electrodes, and methods of fabrication |
| CN111048776A (en) * | 2019-12-18 | 2020-04-21 | 深圳大学 | Morphology-adjustable cubic cobaltosic oxide, preparation method thereof and lithium ion battery |
| CN112408499A (en) * | 2020-11-09 | 2021-02-26 | 格林美（江苏）钴业股份有限公司 | Method for synthesizing cobaltosic oxide by adopting high-pressure reaction |
| USRE49205E1 (en) | 2016-01-22 | 2022-09-06 | Johnson Ip Holding, Llc | Johnson lithium oxygen electrochemical engine |
| CN115050977A (en) * | 2022-06-20 | 2022-09-13 | 江苏展鸣新能源有限公司 | Porous carbon loaded Co applied to zinc-air battery 3 O 4 Electrocatalyst and method of making |
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2008
- 2008-11-28 CN CNA2008101626905A patent/CN101434417A/en active Pending
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| CN101585559B (en) * | 2009-06-14 | 2011-02-16 | 宁波科博特钴镍有限公司 | Preparation method of spherical cobaltosic oxide with high battery security |
| CN101863518A (en) * | 2010-07-01 | 2010-10-20 | 上海应用技术学院 | Co3O4 nano hollow sphere material and preparation method and application thereof |
| CN102336444B (en) * | 2010-07-16 | 2013-07-24 | 同济大学 | Method for preparing nanoscale disk-like cobaltosic oxide |
| CN102336444A (en) * | 2010-07-16 | 2012-02-01 | 同济大学 | Method for preparing nanoscale disk-like cobaltosic oxide |
| CN102259934A (en) * | 2011-05-17 | 2011-11-30 | 周红阳 | Process for producing high-density spherical cobaltosic oxide by virtue of low temperature liquid phase precipitation oxidization |
| CN102259934B (en) * | 2011-05-17 | 2013-02-06 | 湖南红太阳电源新材料股份有限公司 | Oxidization process for producing high-density spherical cobaltosic oxide by virtue of low temperature liquid phase precipitation |
| US10333123B2 (en) | 2012-03-01 | 2019-06-25 | Johnson Ip Holding, Llc | High capacity solid state composite cathode, solid state composite separator, solid-state rechargeable lithium battery and methods of making same |
| WO2013130983A2 (en) * | 2012-03-01 | 2013-09-06 | Excellatron Solid State, Llc | Impregnated sintered solid state composite electrode, solid state battery, and methods of preparation |
| WO2013130983A3 (en) * | 2012-03-01 | 2013-10-24 | Excellatron Solid State, Llc | Impregnated sintered solid state composite electrode, solid state battery, and methods of preparation |
| US10084168B2 (en) | 2012-10-09 | 2018-09-25 | Johnson Battery Technologies, Inc. | Solid-state battery separators and methods of fabrication |
| US9793525B2 (en) | 2012-10-09 | 2017-10-17 | Johnson Battery Technologies, Inc. | Solid-state battery electrodes |
| CN103145200B (en) * | 2013-03-25 | 2015-08-05 | 安徽亚兰德新能源材料股份有限公司 | A kind of method of hybrid oxidative synthesis spherical cobaltic-cobaltous oxide |
| CN103145200A (en) * | 2013-03-25 | 2013-06-12 | 安徽亚兰德新能源材料股份有限公司 | Method for synthesizing spherical cobaltosic oxide through mixing type oxidation |
| CN103274480A (en) * | 2013-06-06 | 2013-09-04 | 南通瑞翔新材料有限公司 | Precursor of polynary positive electrode material for lithium ion battery, and preparation method thereof |
| CN103318976A (en) * | 2013-07-04 | 2013-09-25 | 中南大学 | Technology for preparing cobaltosic oxide by cobalt-containing solution |
| CN103318976B (en) * | 2013-07-04 | 2015-12-09 | 中南大学 | A kind of technique being prepared tricobalt tetroxide by cobalt-carrying solution |
| CN104986807A (en) * | 2015-04-23 | 2015-10-21 | 金川集团股份有限公司 | Spherical tricobalt tetraoxide preparation method |
| CN106340643A (en) * | 2015-07-10 | 2017-01-18 | 北京当升材料科技股份有限公司 | Method for preparing large-grain spherical cobaltosic oxide |
| US10566611B2 (en) | 2015-12-21 | 2020-02-18 | Johnson Ip Holding, Llc | Solid-state batteries, separators, electrodes, and methods of fabrication |
| US11417873B2 (en) | 2015-12-21 | 2022-08-16 | Johnson Ip Holding, Llc | Solid-state batteries, separators, electrodes, and methods of fabrication |
| USRE49205E1 (en) | 2016-01-22 | 2022-09-06 | Johnson Ip Holding, Llc | Johnson lithium oxygen electrochemical engine |
| CN105668650A (en) * | 2016-03-23 | 2016-06-15 | 荆门市格林美新材料有限公司 | Method for preparing low-sodium cobaltosic oxide |
| CN111048776A (en) * | 2019-12-18 | 2020-04-21 | 深圳大学 | Morphology-adjustable cubic cobaltosic oxide, preparation method thereof and lithium ion battery |
| CN111048776B (en) * | 2019-12-18 | 2022-09-09 | 深圳大学 | Shape-adjustable cubic cobaltosic oxide, preparation method and lithium ion battery |
| CN112408499A (en) * | 2020-11-09 | 2021-02-26 | 格林美（江苏）钴业股份有限公司 | Method for synthesizing cobaltosic oxide by adopting high-pressure reaction |
| CN115050977A (en) * | 2022-06-20 | 2022-09-13 | 江苏展鸣新能源有限公司 | Porous carbon loaded Co applied to zinc-air battery 3 O 4 Electrocatalyst and method of making |
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Open date: 20090520 |