CN102874881A - Method for preparing cobaltosic oxide - Google Patents
Method for preparing cobaltosic oxide Download PDFInfo
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- CN102874881A CN102874881A CN2011101986936A CN201110198693A CN102874881A CN 102874881 A CN102874881 A CN 102874881A CN 2011101986936 A CN2011101986936 A CN 2011101986936A CN 201110198693 A CN201110198693 A CN 201110198693A CN 102874881 A CN102874881 A CN 102874881A
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Abstract
The invention discloses a method for preparing cobaltosic oxide. The method comprises the following steps of: reacting a solution containing cobalt with a precipitating agent solution to generate a precipitation; calcinating the precipitation to obtain a primarily sintered material; crushing the primarily sintered material to obtain a primarily crushed material; calcinating the primarily crushed material to obtain a secondarily sintered material; and crushing the secondarily sintered material to obtain the cobaltosic oxide, wherein the secondary sintered material is obtained by calcinating the primarily crushed material in the acidic atmosphere. By the method, the tap density of the cobaltosic oxide is greatly increased.
Description
Technical field
The present invention relates to a kind of manufacture method of tricobalt tetroxide, particularly relate to a kind of manufacture method of tricobalt tetroxide of high tap density.
Background technology
At present, as lithium ion battery, very large to the requirement that improves its energy density.
In lithium ion battery, larger as the tap density of the cobalt of positive electrode material acid lithium, the actual tap density of positive electrode material is larger in the positive plate, and the positive electrode material that can pack in the battery of unit volume is more, and the energy density of battery is also just larger.
Tricobalt tetroxide is as the main raw material of lithium ion cell anode material lithium cobaltate, and the performance of cobalt acid lithium material is played a crucial role.Studies show that, adopt the cobalt acid lithium of high tap density type tricobalt tetroxide production to have good inheritance in tap density.
Therefore, produce at present cobalt acid lithium in the company standard with the tap density of cobaltosic oxide powder, usually require greater than 2.0g/cm
3, and along with the progress of technology and the reinforcement of competition, tap density requires more and more higher.
At present, existing many techniques for the production of high tap density type tricobalt tetroxide, for example, by precipitation from homogeneous solution (PFHS)-once sintered-once the technique of pulverizing-double sintering-separating twice prepares tricobalt tetroxide.But its tap density also only is to satisfy above-mentioned company standard, is not greatly improved, and is difficult to satisfy the needs of scientific-technical progress and market competition.
Summary of the invention
The object of the invention is to overcome the manufacture method of the tricobalt tetroxide that is difficult to provide a kind of high tap density that satisfies scientific-technical progress and market competition needs in the prior art, a kind of manufacture method of the tricobalt tetroxide far above the desired tap density of present company standard is provided.
The inventor is by with keen determination research discovery, in the technique of the pulverizing-double sintering-separating twice of above-mentioned precipitation from homogeneous solution (PFHS)-once sintered-once, by double sintering is carried out under acid atmosphere, can improve significantly the tap density of the tricobalt tetroxide of manufacturing, thereby finish the present invention.
The invention provides a kind of manufacture method of cobaltosic oxide powder, it comprises: the solution that contains cobalt and precipitant solution are reacted form the step of precipitation; Precipitation is calcined the step that obtains primary sintered material; Primary sintered material is pulverized the step that obtains a crushed material; A crushed material is calcined the step that obtains the double sintering material; The double sintering material being pulverized the step that obtains cobaltosic oxide powder, wherein, a crushed material is calcined the step that obtains the double sintering material, is to carry out under acid atmosphere.
Adopt the manufacture method of cobaltosic oxide powder of the present invention, the microscopic appearance of tricobalt tetroxide is improved, can produce tap density is 4.0g/cm
3Above far above company standard 2.0g/cm
3Cobaltosic oxide powder, and have good energy-saving effect.
Description of drawings
Fig. 1 is the SEM photo of embodiments of the invention 1.
Fig. 2 is the SEM photo of comparative example 1 of the present invention.
Fig. 3 is the XRD figure picture of embodiments of the invention 1.
Embodiment
Below, be described in detail by reference to the accompanying drawings for the present invention.
The manufacture method of cobaltosic oxide powder of the present invention, it comprises: the solution that contains cobalt and precipitant solution are reacted form the step of precipitation; Precipitation is calcined the step that obtains primary sintered material; Primary sintered material is pulverized the step that obtains a crushed material; A crushed material is calcined the step that obtains the double sintering material; The double sintering material being pulverized the step that obtains cobaltosic oxide powder, wherein, described a crushed material is calcined the step that obtains the double sintering material, is to carry out under acid atmosphere.
In the manufacture method of cobaltosic oxide powder of the present invention, describedly the solution that contains cobalt and precipitant solution are reacted form the step of precipitation, precipitation is calcined the step that obtains primary sintered material, primary sintered material is pulverized the step that obtains a crushed material, a crushed material is calcined the step that obtains the double sintering material, and the double sintering material pulverized in the step that obtains cobaltosic oxide powder, except make with crushed material calcine obtain the double sintering material step carrying out under the acid atmosphere, all can be the manufacturing step of the routine in this area.
The manufacture method of cobaltosic oxide powder of the present invention, describedly crushed material is calcined the step that obtains the double sintering material place under the acid atmosphere and carry out as long as make, the moulding of cobaltosic oxide powder is become easily carry out, the microscopic appearance of tricobalt tetroxide is improved and be easy to obtain the regular octahedron shape.Thus, can produce tap density is 4.0g/cm
3Above far above company standard 2.0g/cm
3Cobaltosic oxide powder.
In the technique of the pulverizing-double sintering-separating twice of traditional precipitation from homogeneous solution (PFHS)-once sintered-once, want to obtain to be higher than 2.0g/cm
3Cobaltosic oxide powder, 2.5g/cm for example
3, need calcination time more than 50 hours, calcining temperature is more than 1000 ℃.Adopt the manufacture method of cobaltosic oxide powder of the present invention, can make calcination time 20 hours with interior, calcining temperature below 1000 ℃, can produce tap density is 4.0g/cm
3Above far above company standard 2.0g/cm
3Cobaltosic oxide powder, therefore, have good energy-saving effect.
Wherein, the tap density of above-mentioned cobaltosic oxide powder is measured by GB/T 21354-2008 method.
Described acid atmosphere can be the acid atmosphere of hydrochloric acid, sulfuric acid atmosphere etc., the preferably acid atmosphere of hydrochloric acid.
The formation of above-mentioned acid atmosphere can be undertaken by variety of way, for example, can be undertaken by the mode that imports sour gas in calcination system, also can its mode that forms sour gas in the process of calcining be carried out by adding cobalt salt.Among the present invention, preferably by adding cobalt salt its mode that forms sour gas in the process of calcining is carried out.
Particularly, by adding cobalt salt its mode that forms sour gas in the process of calcining can followingly be carried out: primary sintered material can pulverized in the step that obtains a crushed material, go in pulverizing to be added with cobalt salt in the primary sintered material, make and a crushed material is calcined the step that obtains the double sintering material under acid atmosphere, carry out; Also a crushed material can calcined in the step that obtains the double sintering material, gone in a crushed material in calcining to be added with cobalt salt, make and a crushed material is calcined the step that obtains the double sintering material under acid atmosphere, carry out; Also primary sintered material can pulverized in the step that obtains a crushed material, go in pulverizing and to be added with cobalt salt in the primary sintered material, and a crushed material is being calcined in the step that obtains the double sintering material, go in a crushed material in calcining to be added with cobalt salt, make and a crushed material is calcined the step that obtains the double sintering material under acid atmosphere, carry out.
Described cobalt salt is to be selected from cobalt chloride or rose vitriol, preferably cobalt chloride.
By adding above-mentioned cobalt salt, cobalt salt decomposes the sour gas that generates tricobalt tetroxide and minute quantity under hot conditions, make the certain acid atmosphere of maintenance in the sintering process, under this acidity atmosphere, the microscopic appearance of tricobalt tetroxide is improved, and then the tap density of tricobalt tetroxide is greatly improved, and, finally should acidity atmosphere absorb by gas absorbing device.Therefore, can not add any impurity or dephasign in the tricobalt tetroxide product, this processes environmentally safe.
In the manufacture method of cobaltosic oxide powder of the present invention, the mass ratio of described cobalt salt and primary sintered material or cobalt salt and a crushed material is preferably 1: 1000-1: 100000, be particularly preferably 1: 10000-1: 30000.
By mass ratio is controlled at 1: 1000-1: 100000, particularly 1: 10000-1: 30000 can more easily control calcination operation, and can obtain tap density under extremely loose condition is 4.0g/cm
3Above far above company standard 2.0g/cm
3Cobaltosic oxide powder.
In the manufacture method of cobaltosic oxide powder of the present invention, described cobalt salt is amorphous and/or crystal, and is preferably amorphous.When being amorphous, because it is powder, when mixing with a crushed material, easier abundant mixing can make being heated evenly in the calcination process, more can obtain the cobaltosic oxide powder of homogeneous, makes its microscopic pattern more tend to unified regular octahedron type at cobalt salt.
Below, the present invention will be described in more detail by embodiment and comparative example.
Embodiment 1
Prepare cobaltosic oxide powder according to following step.
A, (the good sharp jade-like stone cobalt nickel material in Zhejiang company limited makes with technical grade cobalt chloride crystal, purity 99.9%) be dissolved in deionized water, be mixed with the cobalt chloride solution that cobalt concentration is 0.5mol/L, be that 2% ratio adds concentration as the ammoniacal liquor of 15mol/L take the mol ratio with cobalt contents, make the complex cobalt salts solution for subsequent use.
B, with technical grade volatile salt dissolving, add flocculation agent (polyacrylamide) and carry out after the sedimentation removal of impurities, the precipitant solution that is made into 2.5mol/L is for subsequent use.
C, in reaction vessel, add above-mentioned precipitant solution, then under the condition that stirs, the complex cobalt salts solution slowly added in the reactor react with precipitant solution, 65 ℃ of temperature of reaction, and making precipitant solution finally surpass the theoretical equivalent of complex cobalt salts solution 20%, the reaction times is 5 hours.
After d, reaction were finished, under stirring at normal temperature, then ageing 1 hour carried out washing and filtering, obtains precursor.
E, precursor packed into burn in the alms bowl, (the prosperous electric furnace of Jiangsu ten thousand company limited makes in being preheated to 10 segmentation kilns of specified temperature, ejection plate kiln) calcining, control temperature, the time is 1 section 300 ℃, plate speed 15 minutes, 2～5 sections each 500 ℃, plate speed 30 minutes, 6～10 sections each 750 ℃, plate speed 15 minutes, then, take out sintered compact, naturally cooling in air obtains primary sintered material.
F, in primary sintered material, add cobalt chloride crystal (the good sharp jade-like stone cobalt nickel material in Zhejiang company limited makes purity 99%) it is mixed, form mixture, control that the mass ratio of cobalt chloride crystal and primary sintered material is 1: 90000 in this mixture.
G, said mixture is utilized fluidized bed airflow pulverizer (model QLM350, powder company of Shenyang Aircraft Inst. make), with feeding pressure 0.8MPa, pulverize pressure 0.7MPa, obtain crushed material one time.
H, crushed material packed into burn in the alms bowl, (the prosperous electric furnace of Jiangsu ten thousand company limited makes in being preheated to 10 segmentation kilns of specified temperature, ejection plate kiln) calcining, control temperature, the time is 1 section 550 ℃, plate speed 20 minutes, then 2～10 sections each 900 ℃, plate speed 20 minutes, take out sintered compact, naturally cooling in air obtains the double sintering material.
I, the double sintering material is utilized fluidized bed airflow pulverizer (model QLM350, powder company of Shenyang Aircraft Inst. make), with feeding pressure 0.9MPa, pulverize pressure 1.0MPa, obtain the separating twice material, that is, and cobaltosic oxide powder of the present invention.
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 4.1g/cm according to GB/T 21354-2008 method
3
Fig. 1 is the SEM photo of the cobaltosic oxide powder that makes by above-mentioned steps, and Fig. 3 is the XRD figure picture of the cobaltosic oxide powder that makes by above-mentioned steps.
Embodiment 2
Except above-mentioned cobalt chloride crystal and primary sintered material mass ratio were controlled to be 1: 2000, other step was identical with embodiment 1, obtains cobaltosic oxide powder.
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 4.1g/cm according to GB/T 21354-2008 method
3
Embodiment 3
Except above-mentioned cobalt chloride crystal and primary sintered material mass ratio were controlled to be 1: 25000, other step was identical with embodiment 1, obtains cobaltosic oxide powder.
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 4.5g/cm according to GB/T 21354-2008 method
3
Embodiment 4
Except above-mentioned cobalt chloride crystal is replaced with rose vitriol crystal (Zhejiang Province Huayou cobalt industry Co., Ltd, purity 99%) in addition, other step is identical with embodiment 1, obtains cobaltosic oxide powder.
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 4.1g/cm according to GB/T 21354-2008 method
3
Embodiment 5
Except above-mentioned cobalt chloride crystal is replaced with rose vitriol crystal (Zhejiang Province Huayou cobalt industry Co., Ltd, purity 99%) in addition, other step is identical with embodiment 2, obtains cobaltosic oxide powder.
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 4.1g/cm according to GB/T 21354-2008 method
3
Embodiment 6
Except above-mentioned cobalt chloride crystal is replaced with rose vitriol crystal (Zhejiang Province Huayou cobalt industry Co., Ltd, purity 99%) in addition, other step is identical with embodiment 3, obtains cobaltosic oxide powder.
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 4.4g/cm according to GB/T 21354-2008 method
3
Embodiment 7
It is mixed forms mixture and replaces the cobalt chloride crystal added to and it is mixed form the mixture, other step is identical with embodiment 1, obtains cobaltosic oxide powder.
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 4.1g/cm according to GB/T 21354-2008 method
3
Embodiment 8
It is mixed forms mixture and replaces the cobalt chloride crystal added to and it is mixed form the mixture, other step is identical with embodiment 2, obtains cobaltosic oxide powder.
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 4.1g/cm according to GB/T 21354-2008 method
3
Embodiment 9
It is mixed forms mixture and replaces the cobalt chloride crystal added to and it is mixed form the mixture, other step is identical with embodiment 3, obtains cobaltosic oxide powder.
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 4.6g/cm according to GB/T 21354-2008 method
3
In addition, other step is identical with embodiment 1, obtains cobaltosic oxide powder except above-mentioned cobalt chloride crystal being replaced amorphous cobalt chloride (the good sharp jade-like stone cobalt nickel material in Zhejiang company limited makes purity 99%).
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 4.2g/cm according to GB/T 21354-2008 method
3
Embodiment 11
In addition, other step is identical with embodiment 2, obtains cobaltosic oxide powder except above-mentioned cobalt chloride crystal being replaced amorphous cobalt chloride (the good sharp jade-like stone cobalt nickel material in Zhejiang company limited makes purity 99%).
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 4.2g/cm according to GB/T 21354-2008 method
3
Embodiment 12
In addition, other step is identical with embodiment 3, obtains cobaltosic oxide powder except above-mentioned cobalt chloride crystal being replaced amorphous cobalt chloride (the good sharp jade-like stone cobalt nickel material in Zhejiang company limited makes purity 99%).
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 4.6g/cm according to GB/T 21354-2008 method
3
Comparative example 1
Except not adding cobalt chloride, other step is identical with embodiment 1, obtains cobaltosic oxide powder.
To the cobaltosic oxide powder by above-mentioned steps system, measure tap density, consequently 2.1g/cm according to GB/T 21354-2008 method
3
Fig. 2 is the SEM photo of the cobaltosic oxide powder that makes by above-mentioned steps.
Compare above-described embodiment 1～12 and comparative example 1, can find out: in embodiment 1～12, in the technique of the pulverizing-double sintering-separating twice of precipitation from homogeneous solution (PFHS)-once sintered-once, by double sintering is carried out under acid atmosphere, the moulding of cobaltosic oxide powder is become easily to be carried out, and be easy to obtain the regular octahedron shape, thus, producing tap density is 4.0g/cm
3Above far above company standard 2.0g/cm
3Cobaltosic oxide powder.Relative therewith, in the comparative example 1, double sintering is carried out under acid atmosphere, the tap density of the cobaltosic oxide powder that produces is 2.1g/cm
3
As shown in Figure 1, the method for embodiments of the invention 1 can make the microscopic appearance of tricobalt tetroxide improve, and presents the regular octahedron shape.Relative therewith, as shown in Figure 2, resulting tricobalt tetroxide in the comparative example 1 demonstrates mixed and disorderly microscopic appearance.
In addition, since acid atmosphere by on kiln with gas absorbing device absorb.As shown in Figure 3, in the tricobalt tetroxide product, do not add any impurity or dephasign.
Claims (10)
1. the manufacture method of a cobaltosic oxide powder, it comprises: the solution that contains cobalt and precipitant solution are reacted form the step of precipitation; Precipitation is calcined the step that obtains primary sintered material; Primary sintered material is pulverized the step that obtains a crushed material; A crushed material is calcined the step that obtains the double sintering material; The double sintering material is pulverized the step that obtains cobaltosic oxide powder, it is characterized in that,
Described a crushed material being calcined the step that obtains the double sintering material, is to carry out under acid atmosphere.
2. the manufacture method of cobaltosic oxide powder according to claim 1, wherein, described acid atmosphere is the acid atmosphere of hydrochloric acid or sulfuric acid atmosphere.
3. the manufacture method of cobaltosic oxide powder according to claim 1, wherein, primary sintered material is pulverized in the step that obtains a crushed material described, go in pulverizing to be added with cobalt salt in the primary sintered material, make and describedly a crushed material is calcined the step that obtains the double sintering material under acid atmosphere, carry out.
4. the manufacture method of cobaltosic oxide powder according to claim 1, wherein, described a crushed material is calcined in the step that obtains the double sintering material, go in a crushed material in calcining to be added with cobalt salt, make and describedly a crushed material is calcined the step that obtains the double sintering material under acid atmosphere, carry out.
5. according to claim 3 or the manufacture method of 4 described cobaltosic oxide powders, wherein, described cobalt salt is to be selected from cobalt chloride or rose vitriol.
6. the manufacture method of cobaltosic oxide powder according to claim 3, wherein, the mass ratio of described cobalt salt and primary sintered material is 1: 1000-1: 100000.
7. the manufacture method of cobaltosic oxide powder according to claim 3, wherein, the mass ratio of described cobalt salt and primary sintered material is 1: 10000-1: 30000.
8. the manufacture method of cobaltosic oxide powder according to claim 4, wherein, the mass ratio of described cobalt salt and a crushed material is 1: 1000-1: 100000.
9. the manufacture method of cobaltosic oxide powder according to claim 4, wherein, the mass ratio of described cobalt salt and a crushed material is 1: 10000-1: 30000.
10. according to claim 3 or the manufacture method of 4 described cobaltosic oxide powders, wherein, described cobalt salt is amorphous and/or crystal.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271440A (en) * | 2015-09-29 | 2016-01-27 | 曲阜师范大学 | Structured octahedral nanometer cobaltosic oxide, and preparation method and application thereof |
| US10995014B1 (en) | 2020-07-10 | 2021-05-04 | Northvolt Ab | Process for producing crystallized metal sulfates |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1623909A (en) * | 2003-12-05 | 2005-06-08 | 北京当升材料科技有限公司 | Cobalt oxide of lithium battery grade and its preparation method |
| CN101787433A (en) * | 2010-02-22 | 2010-07-28 | 紫金矿业集团股份有限公司 | Chloridizing roasting method of material containing alunite |
-
2011
- 2011-07-15 CN CN201110198693.6A patent/CN102874881B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1623909A (en) * | 2003-12-05 | 2005-06-08 | 北京当升材料科技有限公司 | Cobalt oxide of lithium battery grade and its preparation method |
| CN101787433A (en) * | 2010-02-22 | 2010-07-28 | 紫金矿业集团股份有限公司 | Chloridizing roasting method of material containing alunite |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271440A (en) * | 2015-09-29 | 2016-01-27 | 曲阜师范大学 | Structured octahedral nanometer cobaltosic oxide, and preparation method and application thereof |
| CN105271440B (en) * | 2015-09-29 | 2017-03-08 | 曲阜师范大学 | A kind of preparation method of nano-cobaltic-cobaltous oxide |
| US10995014B1 (en) | 2020-07-10 | 2021-05-04 | Northvolt Ab | Process for producing crystallized metal sulfates |
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