CN103964514A - Preparation method of regular octahedron-type cobaltosic oxide - Google Patents
Preparation method of regular octahedron-type cobaltosic oxide Download PDFInfo
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- CN103964514A CN103964514A CN201310036466.2A CN201310036466A CN103964514A CN 103964514 A CN103964514 A CN 103964514A CN 201310036466 A CN201310036466 A CN 201310036466A CN 103964514 A CN103964514 A CN 103964514A
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Abstract
The invention discloses a preparation method of regular octahedron-type cobaltosic oxide. The preparation method comprises the following steps of 1, mixing a cobalt salt solution having a cobalt ion concentration of 1.0-2.0mol/L and a complexing agent to obtain a mixed solution, 2, preparing a hydroxide solution having a hydroxyl concentration of 5.0-10.0mol/L from a hydroxide, 3, merging the mixed solution and the hydroxide solution, feeding the mixture into a reactor and preparing a cobalt hydroxide suspension liquid, 4, filtering the cobalt hydroxide suspension liquid, washing the filter residue and carrying out drying, and 5, calcining the dried hydroxide solids in a calcining furnace to obtain the regular octahedron-type cobaltosic oxide. The preparation method avoids microwave radiation pollution, comprises a mild liquid phase reaction in a preparation early stage and a calcining oxidation reaction in a preparation later stage, has high safety in the whole preparation process, has low energy consumption, and realizes easy enlargement of the reactor. Therefore, the preparation method easily realizes industrialization.
Description
Technical field
The present invention relates to chemical industry and technical field of material, particularly a kind of preparation method of regular octahedron tricobalt tetroxide.
Background technology
The outward appearance of tricobalt tetroxide is black or black powder, be mainly used in the fields such as catalyzer, electrochemistry, corrosion-and high-temp-resistant and magneticsubstance, in catalyst field, tricobalt tetroxide is mainly used in oxidizing reaction, in solid-liquid electrochemical field, be mainly used in activated metal electrode.
Along with the fast development of lithium ion battery industry, drive the fast development of its positive pole material of lithium cobalt acid, and the main raw materials of cobalt acid lithium is tricobalt tetroxide, purity, granularity appearance structure and the size-grade distribution state of cobaltosic oxide powder have material impact for the performance of powder.
The pattern of the high performance tricobalt tetroxide that advanced foreign technology is produced is at present octahedron or polyhedron, and be not the prepared spherical cobaltic-cobaltous oxide of numerous domestic manufacturer, the external general preparation technology who adopts is spray pyrolysis, but this kind of needed facility investment of method is very large, because the energy consumption that roasting brings is also very huge, this is still difficult to realize at home at present simultaneously.
Publication number is that the Chinese patent of CN102134104A discloses the method for a kind of " preparing superfine octahedral cobaltosic oxide through cobalt salt precipitated microwave-induced pyrolysis ", publication number is that the Chinese patent of CN102491431A discloses a kind of " microwave single stage method is prepared the octahedral method of tricobalt tetroxide ", but adopt microwave induced method to be difficult to realize suitability for industrialized production, and its energy consumption is large, there is radiation pollution, and current used end liquid is ethanol class, volatile or inflammable organism, adopt microwave induced legal system also to have very large potential safety hazard for regular octahedron tricobalt tetroxide.
Summary of the invention
The object of this invention is to provide a kind of preparation method of regular octahedron tricobalt tetroxide, to realize the preparation that completes regular octahedron tricobalt tetroxide with lower energy consumption and lower cost, and improve the security in tricobalt tetroxide preparation process.
For solving the problems of the technologies described above, the preparation method of the regular octahedron tricobalt tetroxide that the present invention carries comprises the following steps:
1) cobalt salt solution and complexing agent are mixed to get to mixed solution, in described cobalt salt solution, the volumetric molar concentration of cobalt ion is 1.0-2.0mol/L;
2) preparation hydroxide solution, becomes by oxyhydroxide preparation the oxyhydroxide liquid that hydroxide radical volumetric molar concentration is 5.0-10.0mol/L;
3) prepare the oxyhydroxide of cobalt, by the mixed solution in described step 1) and described step 2) in hydroxide solution and the reaction vessel that circulates in react, prepare the hydroxide suspension liquid of cobalt;
4) the hydroxide suspension liquid of cobalt is filtered to the hydroxide solids that obtains cobalt, and it is washed, is dried;
5) the temperature lower calcination 2-6 hour at 300-500 DEG C by the hydroxide solids of the cobalt after drying, makes regular octahedron tricobalt tetroxide.
Preferably, the volumetric molar concentration of the complexing agent of step 1) is the 0.1%-0.5% of cobalt ion volumetric molar concentration in cobalt salt solution.
Preferably, the reaction vessel in described step 3) is reactor, and PH in described reactor is controlled at 9-11, and the temperature of reaction in reactor is controlled at 40 DEG C-70 DEG C, and the stirring velocity of stirring arm is 200-400rpm.
Preferably, mixed solution and the hydroxide solution in described step 3) circulate and be controlled at 200-400L/h into the total flux of reactor.
Preferably, the Aging Temperature of described aging reactor is 20 DEG C-80 DEG C.
Preferably, the washing in described step 4) is to adopt deionized water repeatedly to wash the hydroxide solids of cobalt.
Preferably, the cobalt salt in described step 1) is the mixing of a kind of in rose vitriol or cobalt chloride or two kinds, and described complexing agent is the combination of a kind of in glycine or Histidine or two kinds.
Preferably, described step 2) in oxyhydroxide be the combination of a kind of in sodium hydroxide or potassium hydroxide or two kinds.
In the preparation method of regular octahedron tricobalt tetroxide provided by the present invention, be first then passed in reaction vessel and make it react the hydroxide suspension liquid that generates cobalt with hydroxide solution stream be mixed with mixed solution by cobalt salt solution and complexing agent, then by filtering, after oven dry, make the hydroxide solids of cobalt, and the solid making is calcined and made it under the oxygenizement of air, make regular octahedron tricobalt tetroxide, compared with prior art, preparation method provided by the present invention is that conventional wet method is prepared regular octahedron tricobalt tetroxide, do not exist microwave radiation to pollute, early stage, preparation process was liquid phase reaction, reaction is mild, later stage is prepared as calcined oxide reaction, the potential safety hazard of whole preparation process is less, and energy consumption is lower with respect to prior art, thereby the security of preparation process is higher and preparation cost is relatively low, liquid reactive reaction vessel is easily realized expansion simultaneously, therefore this kind of preparation method easily realizes industrial sector.
Brief description of the drawings
Preparation method's schema of the regular octahedron tricobalt tetroxide that Fig. 1 provides for the embodiment of the present invention;
The stereoscan photograph of the cobaltosic oxide powder that Fig. 2 provides for the embodiment of the present invention one.
Embodiment
Core object of the present invention is to provide a kind of preparation method of regular octahedron tricobalt tetroxide, the method adopts liquid phase reaction legal system for hydroxide cobalt, then by calcining, hydroxide cobalt is at high temperature oxidized by oxygen and becomes regular octahedron tricobalt tetroxide, it is high that this preparation method has safe preparation process, the advantage that preparation cost is lower.
In order to make those skilled in the art person understand better the present invention program, below in conjunction with drawings and embodiments, the present invention is described in further detail.
Please refer to Fig. 1, preparation method's schema of the regular octahedron tricobalt tetroxide that Fig. 1 provides for the embodiment of the present invention.
It is higher that the preparation method of regular octahedron tricobalt tetroxide provided by the present invention mainly solves current regular octahedron tricobalt tetroxide preparation cost, the shortcoming that safe preparation process hidden danger is larger, and preparation method provided by the present invention comprises the following steps for this reason:
S1) preparation mixed solution:
Cobalt salt preparation is become to even cobalt salt solution, and the concentration of cobalt ions in cobalt salt solution is remained in the scope of 1.0-2.0mol/L, then stand-by to adding complexing agent preparation to become mixed solution in the cobalt salt solution preparing;
S2) preparation hydroxide solution:
Ready oxyhydroxide preparation is become to hydroxide solution liquid stand-by, the preferably 5.0-10.0mol/L of concentration hydroxy in this hydroxide solution;
Step S1) and step S2) in solvent can select tap water, certainly, for prioritization scheme further, also can choose more pure deionized water and prepare mixed solution and hydroxide solution as solvent.
S3) prepare the oxyhydroxide of cobalt:
By step S1) and step S2) in the mixed solution for preparing and hydroxide solution take and the mode that flows is passed into reaction vessel, as reacted in reactor, in reaction process, control the stirring velocity of reactor stirring rake, pH value in temperature of reaction and reactor in reactor, under the stirring of stirring arm, react 5-20 hour, make cobalt salt solution and hydroxide solution generate the hydroxide suspension liquid of cobalt in reaction kettle for reaction, be the suspension of hydroxide cobalt, preferred mode, the suspension that reaction is generated is passed into and in aging reactor, carries out ageing, digestion time is 2-8 hour preferably, the temperature of aging reactor is preferably controlled within the scope of 20 DEG C-80 DEG C,
Certainly, generate hydroxide cobalt suspension for cobalt salt solution is reacted with hydroxide solution, these two kinds of reaction masses also need the proportionlity that keeps certain in the time passing into, and preferably should be: cobalt ion and the molar ratio that passes into hydroxy are Co
2+/ OH
-=3.0 ~ 3.3.
S4) filter, wash, dry:
The hydroxide suspension liquid of the cobalt after ageing is filtered, filter type can adopt common filter type, also can adopt pressure filter to carry out press filtration, the hydroxide solids of the cobalt then filtration being obtained is washed, remove foreign ion, and it is dried, thereby obtain solid hydrogen cobaltous oxide;
S5) to step S4) hydroxide solids of prepared cobalt calcines, calcining temperature is preferably controlled within the scope of 300 DEG C-500 DEG C, calcination time is 2-6 hour, and in calcination process, make pressed powder fully contact with air, thereby make the oxyhydroxide of cobalt under the oxygenizement of air, be completed into the tricobalt tetroxide of regular octahedron.
Can be found out by above preparation process, in the preparation method of regular octahedron tricobalt tetroxide provided by the present invention, first the mixed solution being mixed with by cobalt salt solution and complexing agent and hydroxide solution stream are passed in reactor, and under the stirring action of stirring rake, make its reaction generate the hydroxide suspension liquid of cobalt, then by ageing, press filtration makes the hydroxide solids powder of cobalt after drying, and the hydroxide solids powder of the cobalt making is calcined and made it under the oxygenizement of air, generate regular octahedron tricobalt tetroxide, compared with prior art, preparation method provided by the present invention is that conventional wet method is prepared regular octahedron tricobalt tetroxide, working method is convenient and ripe, the time of reaction is shorter, and do not exist microwave radiation to pollute, early stage, preparation process was liquid phase reaction, reaction is mild, later stage is prepared as calcined oxide reaction, the potential safety hazard of whole preparation process is less, and energy consumption is lower with respect to prior art, thereby the security of preparation process is higher and preparation cost is relatively low, liquid reactive reaction vessel is easily realized expansion simultaneously, therefore this kind of preparation method easily realizes industrial sector.
In order to reach best effect, such scheme step S1) in the preferably 0.1%-0.5% of cobalt ion volumetric molar concentration in cobalt salt solution of volumetric molar concentration of complexing agent.
Temperature in reactor, stirring velocity and pH value are controlled in rational scope can fast reaction speed, save the reaction times, reduce energy consumption of reaction, in reactor in this programme, PH is preferably controlled within the scope of 9-11, temperature in reactor is controlled at 40 DEG C-70 DEG C, in reactor, the stirring velocity of stirring rake is also to affect speed of response and the particularly crucial factor of reaction mass, stirring velocity is excessively slow, can cause the reaction mass speed of response in reactor slower, reaction times is longer, stirring velocity is too fast, easily cause material in reactor reaction complete not, in the embodiment of the present invention, ensureing that material reaction is completely on basis, save the reaction times as far as possible, therefore the stirring velocity of reactor stirring arm is set to 200-400rpm.
Step S3 in such scheme) in mixed solution and hydroxide solution stream be passed within total flux in reactor also should remain on certain scope in the case of stirring velocity, temperature of reaction and the pH value setting, in order to reach best effect, in this programme, mixed solution and hydroxide solution stream are passed into total flux in reactor within the scope of 200-400L/h.
Step S4) in washing, can adopt tap water to wash, but in order to make purer regular octahedron tricobalt tetroxide, the washing in this programme is to adopt deionized water repeatedly to wash the hydroxide solids of cobalt.
Step S1 in technique scheme) in cobalt salt solution can have multiple choices, it can be for example the one in rose vitriol or cobalt chloride, or the combination of two kinds, certainly, complexing agent also can be by multiple choices, for example, can be the composition of the arbitrary proportion of a kind of or two kinds of materials in glycine or Histidine.
Oxyhydroxide in such scheme has multiple choices equally, and oxyhydroxide can be the mixture of a kind of in sodium hydroxide or potassium hydroxide or two kinds.
Concrete preparation process please refer to following specific embodiment:
Embodiment mono-
Cobalt chloride preparation is become to cobalt salt solution, and making the cobalt ion volumetric molar concentration in solution is 1.5mol/L, add glycine as complexing agent, and make the volumetric molar concentration of glycine be 0.003mol/L(be concentration of cobalt ions 0.2%), now mixed solution has been prepared, sodium hydroxide preparation is become to the alkali lye of 9.0mol/L, then mixed solution mixed with alkali lye and flow and be passed in reactor with the flow of 200L/h, and make the PH in reactor be controlled at 10.0, temperature of reaction is controlled at 65 DEG C, stirring velocity is controlled at 300rpm, suspension is passed into temperature after the stirring reaction of 8 hours and is in the aging reactor of 50 DEG C and carry out the ageing of 3 hours, then the suspension after ageing is carried out to press filtration and obtain hydroxide cobalt, after hydroxide cobalt is carried out washing for three times with deionized water, enter in stoving oven and dry and make dry hydrogen cobaltous oxide powder, the bake out temperature of stoving oven is set in 300 DEG C, dry hydroxide cobalt dust is carried out in retort furnace at the temperature of 400 DEG C to the calcining of 4 hours, finally make regular octahedron cobaltosic oxide powder, Fig. 2 is the stereoscan photograph of the cobaltosic oxide powder in this embodiment, from photo, we can clearly find out that its crystal formation is complete shape of octahedron.In this embodiment, the loose density of prepared regular octahedron tricobalt tetroxide sampling and testing sample is 0.95g/cm
3, tap density is 1.54g/cm
3, the average meso-position radius of particle (D50) is 3.5um.
Embodiment bis-
Rose vitriol preparation is become to the cobalt salt solution that cobalt ion volumetric molar concentration is 1.0mol/L, and adds Histidine as complexing agent, and make the volumetric molar concentration of Histidine be 0.005mol/L(be concentration of cobalt ions 0.5%), now complete mixed solution preparation, potassium hydroxide preparation is become to the alkali lye that concentration is 7.0mol/L, and mixed solution and alkali lye are also flowed and are passed in reactor with the flow of 300L/h, and make the PH in reactor be controlled at 9.0, temperature of reaction is controlled at 45 DEG C, stirring velocity is controlled at 380rpm, after the stirring reaction of 16 hours, the suspension in reactor is passed in the aging reactor of 70 DEG C and carries out the ageing of 3 hours, then the suspension after ageing is carried out to press filtration and obtain hydroxide cobalt, after hydroxide cobalt is carried out washing for four times with deionized water, enter in stoving oven and dry and make dry hydrogen cobaltous oxide powder, the temperature setting of stoving oven is set to 200 DEG C, dry hydroxide cobalt dust is carried out in retort furnace at the temperature of 350 DEG C to the calcining of 6 hours, finally make regular octahedron cobaltosic oxide powder, to regular octahedron tricobalt tetroxide, split is screened, remove metallic foreign body, and to carry out sampling and testing loose density be 0.99g/cm
3, tap density is 1.60g/cm
3, the average meso-position radius of particle (D50) is 2.94um.
Embodiment tri-
Choose cobalt chloride and preparation becomes the cobalt salt solution that the volumetric molar concentration of cobalt ion is 2.0mol/L, add glycine that cobalt salt solution preparation is become to mixed solution, and make the volumetric molar concentration of glycine be 0.006mol/L(be concentration of cobalt ions 0.2%), sodium hydroxide preparation is become to the alkali lye of 10.0mol/L, mixed solution and alkali lye are passed into reactor bottom with the flow velocity of 400L/h stream to react, the PH controlling in reactor is 11.0, temperature of reaction is controlled at 55 DEG C, stirring velocity is 400rpm, after the stirring reaction of 10 hours, suspension is passed in the aging reactor of 65 DEG C and carries out the ageing of 5 hours, then the suspension press filtration after ageing is obtained to hydroxide cobalt, after hydroxide cobalt is carried out washing for three times with deionized water, enter in stoving oven and dry and make dry hydrogen cobaltous oxide powder, the temperature setting of stoving oven is set to 300 DEG C, dry hydroxide cobalt dust is carried out in retort furnace at the temperature of 450 DEG C to the calcining of 3 hours, finally make regular octahedron cobaltosic oxide powder, sampling and testing loose density is 0.97g/cm
3, tap density is 1.56g/cm
3, the average meso-position radius of particle (D50) is 2.96um.
By finding out in above embodiment, the present invention, with conventional wet method preparation means, completed the preparation of regular octahedron tricobalt tetroxide, and preparation process step is easy, potential safety hazard is lower, on the basis that ensures regular octahedron preparation quality, has saved preparation cost.
Above the preparation method of regular octahedron tricobalt tetroxide provided by the present invention is described in detail.Applied specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Claims (8)
1. a preparation method for regular octahedron tricobalt tetroxide, is characterized in that, comprises step:
1) cobalt salt solution and complexing agent are mixed to get to mixed solution, in described cobalt salt solution, the volumetric molar concentration of cobalt ion is 1.0-2.0mol/L;
2) preparation hydroxide solution, becomes by oxyhydroxide preparation the oxyhydroxide liquid that hydroxide radical volumetric molar concentration is 5.0-10.0mol/L;
3) prepare the oxyhydroxide of cobalt, by the mixed solution in described step 1) and described step 2) in hydroxide solution and the reaction vessel that circulates in react, prepare the hydroxide suspension liquid of cobalt;
4) the hydroxide suspension liquid of cobalt is filtered to the hydroxide solids that obtains cobalt, and it is washed, is dried;
5) the temperature lower calcination 2-6 hour at 300-500 DEG C by the hydroxide solids of the cobalt after drying, makes regular octahedron tricobalt tetroxide.
2. the preparation method of regular octahedron tricobalt tetroxide according to claim 1, is characterized in that, the volumetric molar concentration of the complexing agent of step 1) is the 0.1%-0.5% of cobalt ion volumetric molar concentration in cobalt salt solution.
3. the preparation method of regular octahedron tricobalt tetroxide according to claim 1, it is characterized in that, reaction vessel in described step 3) is reactor, and the PH in described reactor is controlled at 9-11, temperature of reaction in reactor is controlled at 40 DEG C-70 DEG C, and the stirring velocity of stirring arm is 200-400rpm.
4. the preparation method of regular octahedron tricobalt tetroxide according to claim 3, is characterized in that, the mixed solution in described step 3) and hydroxide solution also circulate and are controlled at 200-400L/h into the total flux of reactor.
5. the preparation method of regular octahedron tricobalt tetroxide according to claim 3, is characterized in that, the Aging Temperature of described aging reactor is 20 DEG C-80 DEG C.
6. the preparation method of regular octahedron tricobalt tetroxide according to claim 1, is characterized in that, the washing in described step 4) is to adopt deionized water repeatedly to wash the hydroxide solids of cobalt.
7. the preparation method of regular octahedron tricobalt tetroxide according to claim 1, it is characterized in that, cobalt salt in described step 1) is the mixing of a kind of in rose vitriol or cobalt chloride or two kinds, and described complexing agent is the combination of a kind of in glycine or Histidine or two kinds.
8. according to the preparation method of the regular octahedron tricobalt tetroxide described in claim 1-7 any one, it is characterized in that described step 2) in oxyhydroxide be the combination of a kind of in sodium hydroxide or potassium hydroxide or two kinds.
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Effective date of registration: 20141119 Address after: 315400 Zhejiang Province, Yuyao City Jia Ling Road No. 39 Applicant after: NINGBO JINHE LITHIUM BATTERY MATERIAL CO., LTD. Address before: 315475 Zhejiang city of Ningbo province Yuyao city coastal industrial park xiao-cao'e town A District No. 2 Applicant before: Ningbo Coboto Cobalt & Nickel Co., Ltd. |
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140806 |