CN106115801A - A kind of Cobalto-cobaltic oxide and preparation method thereof, application - Google Patents
A kind of Cobalto-cobaltic oxide and preparation method thereof, application Download PDFInfo
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- CN106115801A CN106115801A CN201610471258.9A CN201610471258A CN106115801A CN 106115801 A CN106115801 A CN 106115801A CN 201610471258 A CN201610471258 A CN 201610471258A CN 106115801 A CN106115801 A CN 106115801A
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Abstract
The invention provides a kind of Cobalto-cobaltic oxide and preparation method thereof, application, relate to chemical material technical field.The preparation method of Cobalto-cobaltic oxide comprises the following steps: be dissolved in Organic Alcohol by cabaltous nitrate hexahydrate, obtains solute, and the pH adding anhydrous ethylenediamine regulation solute is 8～12, then utilizes solvent-thermal method to react, annealing；Wherein, cabaltous nitrate hexahydrate is 145～295mg:20ml with the amount ratio of Organic Alcohol, and cabaltous nitrate hexahydrate is 1:0.5～5 with the mol ratio of anhydrous ethylenediamine.The preparation method utilizing the Cobalto-cobaltic oxide that the present invention provides can prepare the cobaltosic oxide nano granule that size, pattern are homogeneous, thus is effectively improved the catalytic performance of Cobalto-cobaltic oxide.
Description
Technical field
The present invention relates to chemical material technical field, in particular to a kind of Cobalto-cobaltic oxide and preparation method thereof, answer
With.
Background technology
At the new century that energy and environment are the theme, develop the regenerative resource of cleaning, restructure the use of energy
Become the urgent needs in the whole world.Fuel cell and metal-air battery are the new energy-storage battery systems developed rapidly in recent years,
The numerous areas such as mobile electronic product, electric automobile, military affairs, space flight have important application prospect, are the most promising new electricity
Pond.Fuel cell converts chemical energy into as electric energy, has that conversion efficiency is high, energy density is big, environmental pollution is little, running
Middle noise is low, can realize cogeneration, side-product can be used as the advantages such as the raw material of industry.Metal-air battery has high reason
Opinion energy density (close to fuel system), environmental friendliness, with low cost, therefore above two battery is the new of field of batteries in recent years
Focus.
In both cell reactions, it is directed to redox reaction, but redox reaction itself is a power
Learning slow process, it can cause battery to produce higher potential loss and relatively low transformation efficiency, seriously constrains fuel cell
Commercialized development with metal-air battery.To accelerate the dynamic performance of redox reaction, then need to add catalysis
Agent, can be effectively improved the performance of battery, therefore, developing low-cost, high efficiency, stable oxidation reduction catalyst, have
Important theory and practice meaning.Additionally, oxidation reduction catalyst itself is also widely used, not only in field of batteries, at chlorine
Alkali industry, the electrolysis field such as sodium carbonate and corrosion protection all have excellent application prospect.
At present, oxidation reduction catalyst mainly has platinum based noble metal catalyst and the big class of non-precious metal catalyst two.Although
Platinum based noble metal catalyst performance is good, but it is expensive, cycle performance is poor, therefore limits its application.Base metal is urged
Agent, due to low cost, becomes study hotspot in recent years.And in non-precious metal catalyst, transition metal oxide is electro-catalysis neck
A widest class material is studied in territory.
Cobalt oxide active height, low cost, Heat stability is good, resistance are little, environmentally friendly, are excellent hydrogen reduction catalysis
Agent material.In Cobalto-cobaltic oxide, cobalt ion has multiple quantivalence, is possible not only to catalytic oxidation-reduction and oxygen reaction of formation simultaneously, also
The Organic Electricity oxidation reaction can being catalyzed in alkaline medium.The existence of this mixing quantivalence, the chemisorbed for oxygen provides
Avtive spot, and transfer that electronics is between the cation of different valence state reduces activation energy, thus show relatively
Higher electric conductivity.Therefore, Cobalto-cobaltic oxide has application widely, such as sensor, ultracapacitor, catalysis
Agent, magnetic semiconductor, battery material etc..
At present, prepare the method for Cobalto-cobaltic oxide and mainly have hydro-thermal method, solvent-thermal method, the sedimentation method, sol-gel process, micro-
Emulsion method, thermal decomposition method, electrochemical process etc..Wherein, the crystal structure that solvent-thermal method production cost is low, technique simple, prepare
More complete, good crystallinity, oneself becomes the important method preparing metal-oxide.And utilize existing solvent-thermal method to be prepared,
Typically requiring addition surfactant, prepared Cobalto-cobaltic oxide is spherical, bar-shaped, the lamellar etc. of independent dispersion
(Mater.Lett.2010,64:1275-1278；Solid State Sci.2009,11:108-112), Cobalto-cobaltic oxide granule
Size, pattern differ.Nearest research shows again, and the particle size of nano material (including Cobalto-cobaltic oxide), pattern are with three-dimensional
The catalytic performance of space structure meeting appreciable impact material.Therefore, choosing new solvent thermal reaction system, preparation size is equal with pattern
The cobaltosic oxide nano granule one, with special three-D space structure has important theoretical and practical significance.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of Cobalto-cobaltic oxide, utilize the method can prepare size,
The cobaltosic oxide nano granule that pattern is homogeneous, thus it is effectively improved the catalytic performance of Cobalto-cobaltic oxide.
Another object of the present invention is to provide a kind of Cobalto-cobaltic oxide, the size of this Cobalto-cobaltic oxide, pattern are homogeneous, combine
Close better performances.
Another object of the present invention is to provide Cobalto-cobaltic oxide application in new forms of energy battery.
The present invention solves it and technical problem is that and realize by the following technical solutions:
The preparation method of a kind of Cobalto-cobaltic oxide, comprises the following steps:
Cabaltous nitrate hexahydrate is dissolved in Organic Alcohol, obtains solute, add the pH of anhydrous ethylenediamine regulation solute
It is 8～12, then utilizes solvent-thermal method to react, annealing；
Wherein, cabaltous nitrate hexahydrate is 145～295mg:20ml with the amount ratio of Organic Alcohol, and cabaltous nitrate hexahydrate is with anhydrous
The mol ratio of ethylenediamine is 1:0.5～5.
Preferably, in present pre-ferred embodiments, above-mentioned dissolution time is 8～12min, after adding anhydrous ethylenediamine,
4～6min need to be stirred.
Preferably, in present pre-ferred embodiments, above-mentioned reaction is particularly as follows: react 3～10h at 150～220 DEG C.
Preferably, in present pre-ferred embodiments, after reacting, before the anneal, also include: the thing after question response
Matter is down to 5～40 DEG C, washing.
Preferably, in present pre-ferred embodiments, above-mentioned annealing includes: be heated to the speed of 1.5～2.5 DEG C/min
300～800 DEG C, then insulation 3～6h, then cool down with the speed of 8～12 DEG C/min.
Preferably, in present pre-ferred embodiments, above-mentioned Organic Alcohol is ethylene glycol.
Preferably, in present pre-ferred embodiments, during above-mentioned dissolving, also include: by carbon-based material and/or solubilized precious metal
Solution is in Organic Alcohol.
It addition, a kind of Cobalto-cobaltic oxide, it is that the preparation method utilizing above-mentioned Cobalto-cobaltic oxide prepares.
It addition, the application that above-mentioned Cobalto-cobaltic oxide is in new forms of energy battery.
Preferably, in present pre-ferred embodiments, above-mentioned Cobalto-cobaltic oxide is in fuel cell, metal-air battery
Application as redox reaction catalyst.
Relative to prior art, the present invention includes following beneficial effect: introduce Organic Alcohol conduct in the raw material of the present invention
Reaction medium, it can be simultaneously as gentle reducing agent, owing to the viscosity of reaction medium is high, moderate boiling point, it is possible to have
The reunion in a solvent of the nano-particle of the suppression Cobalto-cobaltic oxide of effect, prevents particle size growth.Additionally, anhydrous ethylenediamine is
As reducing agent, it has good coordination ability, it is also possible to the pH of adjusting solvent, promotes the reaction of cabaltous nitrate hexahydrate, because of
And the homogeneity preferable cobaltosic oxide nano granule of size, pattern can be obtained.The method utilizing the present invention to provide prepares
Co3O4 nanometer material particle size can control at about 20nm, and three-dimensional dendritic nano-structure can be formed, than
Surface area is big, has more reaction site, can significantly improve dynamics of oxidation reduction performance.Therefore, with four common oxygen
Changing three cobalt granules to compare, the cobaltosic oxide nano granule that the present invention prepares has faster redox reaction speed with more preferable
Cycle performance, be the oxidation reduction catalyst of function admirable, the new forms of energy battery such as fuel cell, metal-air battery lead
Territory has extremely important using value and is widely applied prospect.
Accompanying drawing explanation
For the clearer explanation embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
In having technology to describe, the required accompanying drawing used is briefly described, it should be apparent that, the accompanying drawing in describing below is only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to
Other accompanying drawing is obtained according to these accompanying drawings.
Fig. 1 is the schematic diagram of the transmission electron microscope of the Cobalto-cobaltic oxide that the embodiment of the present invention one provides；
Fig. 2 is the schematic diagram of the scanning electron microscope of the Cobalto-cobaltic oxide that the embodiment of the present invention one provides；
Fig. 3 is the XRD spectra of the Cobalto-cobaltic oxide that the embodiment of the present invention one provides；
Fig. 4 is that the Cobalto-cobaltic oxide that the embodiment of the present invention one provides shows as the chemical property of oxidation reduction catalyst
Figure.
Detailed description of the invention
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearer, below will be in the embodiment of the present invention
Technical scheme be clearly and completely described.In embodiment, unreceipted actual conditions person, builds according to normal condition or manufacturer
The condition of view is carried out.Agents useful for same or instrument unreceipted production firm person, being can be by the commercially available conventional product bought and obtain
Product.
Below Cobalto-cobaltic oxide of the embodiment of the present invention and preparation method thereof, application are specifically described.
The preparation method of Cobalto-cobaltic oxide comprises the following steps:
Cabaltous nitrate hexahydrate is dissolved in Organic Alcohol, obtains solute, add the pH of anhydrous ethylenediamine regulation solute
It is 8～12, then utilizes solvent-thermal method to react, annealing；
Wherein, cabaltous nitrate hexahydrate is 145～295mg:20ml with the amount ratio of Organic Alcohol, and cabaltous nitrate hexahydrate is with anhydrous
The mol ratio of ethylenediamine is 1:0.5～5.
In above-mentioned preparation method, the order of addition of cabaltous nitrate hexahydrate and Organic Alcohol does not has requirement, is added by Organic Alcohol
In cabaltous nitrate hexahydrate good, cabaltous nitrate hexahydrate is added in Organic Alcohol good.Organic Alcohol is ethylene glycol.Certainly, it is selected
Its Organic Alcohol can also, such as 1,2-PD, glycerol.
After being joined in Organic Alcohol by cabaltous nitrate hexahydrate, the time of dissolving is 8～12min, so, it is possible to ensure to dissolve
Fully.After adding anhydrous ethylenediamine, 4～6min need to be stirred, so that each component materials mix homogeneously, it is ensured that anhydrous ethylenediamine is to molten
Solve the regulation of the pH of thing.
The pH preferably regulating solute is 8～10.
During dissolving, it is also possible to including: by carbon-based material and/or noble metal removal in Organic Alcohol.Raw material adds carbon back
Material, it is possible to prepare the complex of Cobalto-cobaltic oxide and Graphene, when adding carbon-based material, its consumption the most too much limits
System, can add according to practical situation.Carbon-based material can be activated carbon, activated coke, NACF, Graphene etc., excellent
Select Graphene.Raw material adds noble metal, it is possible to prepare the complex of Cobalto-cobaltic oxide and noble metal, to dissolve your gold
Belong to, then noble metal also selects the presoma of noble metal, such as silver nitrate.When adding noble metal, its consumption does not makes too many restrictions, but
If consideration Cost Problems, then preferred cabaltous nitrate hexahydrate is 8～12:1 with the mass ratio of noble metal precursor body.Cobalto-cobaltic oxide with
The complex of Graphene, Cobalto-cobaltic oxide all can use as catalyst with the complex of noble metal.
Utilizing solvent-thermal method to react, this reaction is particularly as follows: react 3～10h at 150～220 DEG C.Reaction preferably exists
Carrying out in autoclave, certainly, this kind is chosen and is not intended as limiting, as long as react under enclosed system.
After reacting, before the anneal, also include: the material after question response is down to 5～40 DEG C, washing.Wash permissible
Wash away unreacted Organic Alcohol and other impurity, preferably by washing with alcohol.
In above-mentioned preparation method, annealing includes: is heated to 300～800 DEG C with the speed of 1.5～2.5 DEG C/min, then protects
Temperature 3～6h, then cool down with the speed of 8～12 DEG C/min.It should be noted that annealing is to carry out in air ambient.Utilizing
Solvent-thermal method reaction after, obtain is cobalt carbonate, annealed after, target product can be obtained.During cooling, it is cooled to room temperature (certainly
So temperature).
Present invention also offers a kind of Cobalto-cobaltic oxide, be that the preparation method utilizing above-mentioned Cobalto-cobaltic oxide prepares.
Present invention also offers Cobalto-cobaltic oxide application in new forms of energy battery.Preferably at fuel cell, metal-air
Battery is applied as redox reaction catalyst.
Below in conjunction with embodiment, inventive feature and performance are described in further detail:
Embodiment one
The preparation method of the Cobalto-cobaltic oxide that the present embodiment provides, comprises the following steps:
A. cabaltous nitrate hexahydrate is dissolved in ethylene glycol, obtains solute, be subsequently adding anhydrous ethylenediamine regulation and dissolve
The pH of thing is 8；Wherein, cabaltous nitrate hexahydrate is 230mg:20ml with the amount ratio of ethylene glycol, cabaltous nitrate hexahydrate and anhydrous second
The mol ratio of diamidogen is 1:3；
B. the solution that step a obtains is transferred in autoclave, at 180 DEG C, reacts 6h, product ethanol
Wash 3 times；
C. product is placed in air ambient, is heated to 500 DEG C with the speed of 2 DEG C/min, be then incubated 3h, then with
The speed cooling of 10 DEG C/min, obtains cobaltosic oxide nano granule.
The present embodiment additionally provides the Cobalto-cobaltic oxide utilizing above-mentioned preparation method to prepare, and particle size is 18nm, utilizes
Transmission electron microscope observation, it can be clearly seen that the three-dimensional branch network structure of nano material, as shown in Figure 1.Fig. 2 is four
The scanning electron microscope diagram sheet of Co 3 O, it can be seen that nanoparticle size is homogeneous.Fig. 3 is the XRD spectrum of Cobalto-cobaltic oxide
Figure, it can be seen that the purity of sample is the highest, does not has other impurity.
The cobaltosic oxide nano granule prepared by the present embodiment carries out electrochemistry rotation in the saturated alkaline solution of oxygen
Turn disk electrode test, respectively test polarization song under 0rpm, 400rpm, 900rpm, 1600rpm, 2200rpm, 2500rpm
Line, scanning speed is 10mV/s.
Fig. 4 is the chemical property curve of Cobalto-cobaltic oxide, it can be seen that sample has good oxidoreduction
Dynamic performance.
Embodiment two
The preparation method of the Cobalto-cobaltic oxide that the present embodiment provides, comprises the following steps:
A. cabaltous nitrate hexahydrate is dissolved in ethylene glycol 10min, obtains solute, be subsequently adding anhydrous ethylenediamine, stir
Mixing 5min, the pH of regulation solute is 10；Wherein, cabaltous nitrate hexahydrate is 220mg:20ml with the amount ratio of ethylene glycol, six water
The mol ratio closing cobalt nitrate and anhydrous ethylenediamine is 1:2.8；
B. being transferred in autoclave by the solution that step a obtains, react 7h at 180 DEG C, question response product is down to
After 20 DEG C, by washing with alcohol 2 times；
C. product is placed in air ambient, is heated to 500 DEG C with the speed of 2 DEG C/min, be then incubated 4.5h, then
Cool down with the speed of 10 DEG C/min, obtain cobaltosic oxide nano granule.
The present embodiment additionally provides the Cobalto-cobaltic oxide utilizing above-mentioned preparation method to prepare, and particle size is 20nm.
Embodiment three
The preparation method of the Cobalto-cobaltic oxide that the present embodiment provides, comprises the following steps:
A. cabaltous nitrate hexahydrate is dissolved in 1,2-PD, obtains solute, be subsequently adding anhydrous ethylenediamine regulation
The pH of solute is 8；Wherein, cabaltous nitrate hexahydrate is 145mg:20ml with the amount ratio of 1,2-PD, cabaltous nitrate hexahydrate
It is 1:0.5 with the mol ratio of anhydrous ethylenediamine；
B. the solution that step a obtains is transferred in autoclave, at 150 DEG C, reacts 10h；
C. product is placed in air ambient, is heated to 300 DEG C with the speed of 1.5 DEG C/min, be then incubated 6h, then
Cool down with the speed of 8 DEG C/min, obtain cobaltosic oxide nano granule.
The present embodiment additionally provides the Cobalto-cobaltic oxide utilizing above-mentioned preparation method to prepare, and particle size is 22nm.
Embodiment four
The preparation method of the Cobalto-cobaltic oxide that the present embodiment provides, comprises the following steps:
A. cabaltous nitrate hexahydrate is dissolved in ethylene glycol, obtains solute, be subsequently adding anhydrous ethylenediamine regulation and dissolve
The pH of thing is 12；Wherein, cabaltous nitrate hexahydrate is 295mg:20ml with the amount ratio of ethylene glycol, cabaltous nitrate hexahydrate and anhydrous second
The mol ratio of diamidogen is 1:5；
B. the solution that step a obtains is transferred in autoclave, at 220 DEG C, reacts 3h；
C. product is placed in air ambient, is heated to 800 DEG C with the speed of 2.5 DEG C/min, be then incubated 3h, then
Cool down with the speed of 12 DEG C/min, obtain cobaltosic oxide nano granule.
The present embodiment additionally provides the Cobalto-cobaltic oxide utilizing above-mentioned preparation method to prepare, and particle size is 21nm.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, that is made any repaiies
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (10)
1. the preparation method of a Cobalto-cobaltic oxide, it is characterised in that comprise the following steps:
Cabaltous nitrate hexahydrate is dissolved in Organic Alcohol, obtains solute, add anhydrous ethylenediamine and regulate the pH of described solute
It is 8～12, then utilizes solvent-thermal method to react, annealing；
Wherein, described cabaltous nitrate hexahydrate is 145～295mg:20ml with the amount ratio of described Organic Alcohol, described six nitric hydrates
Cobalt is 1:0.5～5 with the mol ratio of described anhydrous ethylenediamine.
The preparation method of Cobalto-cobaltic oxide the most according to claim 1, it is characterised in that described dissolution time be 8～
12min, after adding described anhydrous ethylenediamine, need to stir 4～6min.
The preparation method of Cobalto-cobaltic oxide the most according to claim 1, it is characterised in that described reaction is particularly as follows: 150
～at 220 DEG C, react 3～10h.
The preparation method of Cobalto-cobaltic oxide the most according to claim 1, it is characterised in that after said reaction, in institute
Before stating annealing, also include: the material after question response is down to 5～40 DEG C, washing.
The preparation method of Cobalto-cobaltic oxide the most according to claim 1, it is characterised in that described annealing includes: with 1.5～
The speed of 2.5 DEG C/min is heated to 300～800 DEG C, then insulation 3～6h, then cools down with the speed of 8～12 DEG C/min.
The preparation method of Cobalto-cobaltic oxide the most according to claim 1, it is characterised in that described Organic Alcohol is ethylene glycol.
The preparation method of Cobalto-cobaltic oxide the most according to claim 1, it is characterised in that during described dissolving, also includes: will
Carbon-based material and/or noble metal removal are in described Organic Alcohol.
8. a Cobalto-cobaltic oxide, it is characterised in that utilize the preparation of Cobalto-cobaltic oxide described in any one of claim 1～7
Method prepares.
9. the application in new forms of energy battery of the Cobalto-cobaltic oxide described in claim 8.
10. the Cobalto-cobaltic oxide described in claim 8 is urged as redox reaction in fuel cell, metal-air battery
The application of agent.
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| CN114620772A (en) * | 2020-12-12 | 2022-06-14 | 中国科学院大连化学物理研究所 | Doped transition metal oxide and preparation method and application thereof |
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Application publication date: 20161116 |