CN109935475A - The synthetic method of cobalt molybdate for electrode material for super capacitor - Google Patents
The synthetic method of cobalt molybdate for electrode material for super capacitor Download PDFInfo
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- CN109935475A CN109935475A CN201910209251.3A CN201910209251A CN109935475A CN 109935475 A CN109935475 A CN 109935475A CN 201910209251 A CN201910209251 A CN 201910209251A CN 109935475 A CN109935475 A CN 109935475A
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- molybdate
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- super capacitor
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The present invention provides a kind of synthetic method of cobalt molybdate for electrode material for super capacitor, the synthetic method includes: s1, cobalt salt and deionized water are carried out mixed dissolution obtains solution A；S2, pattern regulator, molybdate and deionized water are subjected to mixed dissolution, and acid-base modifier is then added and is adjusted to neutrality, obtain solution B；S3, precipitation reaction is carried out after mixing solution A in equal volume with solution B, it is cooling after precipitation reaction, and cobalt molybdate is obtained after washed drying.The synthetic method of cobalt molybdate of the present invention, the characteristics of a variety of oxidation state and the conversion reaction of low spot position for having by molybdate, by cobalt salt, cobalt molybdate obtained is used as capacitance electrode material in conjunction with molybdate, can have high invertibity and outstanding cycle performance and stability, and cobalt molybdate obtained is petal-like lamellar structure, it also has more greatly specific surface area, so that the specific capacitance value of capacitor can also be greatly improved, and can have good chemical property.
Description
Technical field
The present invention relates to capacitor electrode material preparation technical fields, in particular to a kind of to be used for electrode of super capacitor material
The synthetic method of the cobalt molybdate of material.
Background technique
Supercapacitor has many advantages, such as power density height, the charge and discharge time is long, and conduct as novel energy storage device
The primary evaluation standard of supercapacitor, the selection of electrode material for super capacitor are also particularly important.Super capacitor electrode
Mainly there are metal C compound, metal oxide and transiton metal binary oxides in the type of pole material, but due to metal C compound
And metal oxide stability, in terms of Shortcomings, so more and more people start sight to be placed on
On transiton metal binary oxides.But in the current electrode material by transiton metal binary oxides preparation, specific capacitance value
It is lower, and limit the application on electrode material for super capacitor.
Summary of the invention
In view of this, the present invention is directed to propose a kind of synthetic method of the cobalt molybdate for electrode material for super capacitor,
With can specific capacitance value with higher.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of synthetic method of the cobalt molybdate for electrode material for super capacitor, the synthetic method include following step
It is rapid:
S1, cobalt salt and deionized water progress mixed dissolution are obtained into solution A；
S2, pattern regulator, molybdate and deionized water are subjected to mixed dissolution, and acid-base modifier tune is then added
Section obtains solution B to neutrality；
S3, precipitation reaction is carried out after mixing solution A in equal volume with solution B, it is cooling after precipitation reaction and washed
Cobalt molybdate is obtained after drying.
Further, in step s1, the mass ratio of the material of cobalt salt and deionized water is (0.002-0.005): 1；Step s2
In, the molar ratio between pattern regulator, molybdate and deionized water is (0.001-0.002): (0.002-0.005): 1.
Further, in step s3, the reaction temperature of precipitation reaction is 25-90 DEG C, and the reaction time is 2-12 hours, and is walked
For by obtaining cobalt molybdate after centrifuge washing and vacuum drying in rapid s3.
Further, the centrifuge washing includes being washed respectively three times by deionized water and ethyl alcohol.
Further, the vacuum drying is 10 hours dry under the conditions of vacuum degree 0.8KPa, temperature 60 C.
Further, the cobalt salt is one of cobalt chloride hexahydrate, cobalt nitrate, cobaltous bromide and cobaltous sulfate.
Further, the molybdate is one of sodium molybdate, ammonium molybdate, nickel molybdate and magnesium molybdate.
Further, the pattern regulator be ammonium fluoride, lauryl sodium sulfate, cetyl trimethylammonium bromide and
One of hexamethylenetetramine.
Further, the acid-base modifier is one of tripotassium phosphate, potassium citrate and sodium citrate.
Further, specific capacitance value of the cobalt molybdate that step s3 is obtained under the current density of 0.25A/g is in 320F/
Between g-480F/g.
Compared with the existing technology, present invention has the advantage that
The synthetic method of cobalt molybdate of the invention, a variety of oxidation state and low potential conversion reaction having using molybdate
The characteristics of, by cobalt salt, cobalt molybdate obtained is used as capacitance electrode material in conjunction with molybdate, and cobalt metal is easy to get, the introducing of Co ion
It can change the electric conductivity of electrode material, pattern regulator is also referred to as surfactant, is a kind of with hydrophilic, oleophylic knot
Structure can reduce surface tension, reduce surface energy, and can be emulsified, soaked, formed a film to solution, pattern is added in synthesis
Regulator can form one layer of molecular film in nano grain surface to prevent contacting with each other between particle, reduce and reunite now
The generation of elephant, and then the generation that can make reaction that there is bigger surface area to be more advantageous to redox reaction.
It is made of between Mo atom and O atom O-Mo-O covalent bond, one layer of Mo atom is mingled among two layers of O atom, each
Mo atom is surrounded by 6 O atoms, similar sandwich structure, due to this special structure, makes cobalt molybdate petal-shaped obtained
Lamellar structure, can have biggish specific surface area, the specific capacitance value of capacitor can be greatly improved, and can have good electricity
Chemical property.
In addition, synthetic method of the invention is relatively simple, cost of material is low, thus has wide application potential.
Detailed description of the invention
The attached drawing for constituting a part of the invention is used to provide further understanding of the present invention, schematic reality of the invention
It applies example and its explanation is used to explain the present invention, do not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is cobalt molybdate XRD diagram prepared by preparating example 1 in the embodiment of the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of cobalt molybdate prepared by preparating example 1 in the embodiment of the present invention；
Fig. 3 is specific capacitance Value Data of the cobalt molybdate as electrode material prepared by preparating example 1 in the embodiment of the present invention
Figure.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
The present embodiment is related to the synthetic method of the cobalt molybdate for electrode material for super capacitor, to be used to prepare for surpassing
The cobalt molybdate of the electrode material of grade capacitor, which, which specifically includes, obtains cobalt salt and deionized water progress mixed dissolution
Pattern regulator, molybdate and deionized water are carried out mixed dissolution by solution A, and acid-base modifier is then added and is adjusted to
Neutrality obtains solution B, and carries out precipitation reaction after above-mentioned solution A is mixed in equal volume with solution B, after precipitation reaction
It is cooling, and cobalt molybdate is obtained after washed drying.
Wherein, in the above synthetic method, the mass ratio of the material of cobalt salt and deionized water is (0.002-0.005): 1, shape
Molar ratio between looks regulator, molybdate and deionized water is (0.001-0.002): (0.002-0.005): 1.Precipitation reaction
Reaction temperature be 25-90 DEG C, the reaction time be 2-12 hour, and be by obtaining molybdic acid after centrifuge washing and vacuum drying
Cobalt.
For above-mentioned centrifuge washing, specifically includes and washed respectively three times by deionized water and ethyl alcohol.And vacuum
It is dry then for dry 10 hours under the conditions of vacuum degree 0.8KPa, temperature 60 C.In addition, in the synthetic method of the present embodiment, it is preceding
State cobalt salt concretely cobalt chloride hexahydrate (CoCl2·6H2O), cobalt nitrate (Co (NO3)2), cobaltous bromide (CoBr2) and cobaltous sulfate
(CoSO4One of).Molybdate can be sodium molybdate (Na2MoO4), ammonium molybdate ((NH4)2MoO4), nickel molybdate (NiMoO4) and molybdenum
Sour magnesium (MgMoO4One of).Pattern regulator can be ammonium fluoride, lauryl sodium sulfate, cetyl trimethylammonium bromide
One of with hexamethylenetetramine.Acid-base modifier can be then one of tripotassium phosphate, potassium citrate and sodium citrate.
Lower mask body further illustrates the cobalt molybdate synthetic method of the present embodiment with several preparating examples.
Preparating example 1
In the synthetic method of the cobalt molybdate for electrode material for super capacitor of this example, firstly, by six chloride hydrates
Cobalt (CoCl2·6H2O it is) that 0.002:1 carries out mixed dissolution by the mass ratio of the material with deionized water, obtains solution A, then by pattern
Regulator ammonium fluoride, sodium molybdate (Na2MoO4) and deionized water by the mass ratio of the material be 0.001:0.002:1 carry out mixed dissolution,
Acid-base modifier tripotassium phosphate is then added to be adjusted to neutrality, obtains solution B.Then after solution A being mixed in equal volume with solution B
Precipitation reaction is carried out, for reaction temperature at 25 DEG C, the reaction time is 2 hours, is cooled down after reaction, and through deionized water, second
Alcohol distinguishes centrifuge washing three times, and vacuum drying 10h is finally carried out under conditions of vacuum degree is 0.8KPa, temperature is 60 DEG C and is obtained
Cobalt molybdate.
The cobalt molybdate of this preparating example synthesis, its XRD diagram (test condition: uses Bruker as shown in fig. 1 after tested
D8 and BDX3300 type X-ray diffractometer carries out XRD test, and excitaton source is Cu-Ka light source, X-ray wavelength 1.54A, tube voltage
For 30kV, tube current 30mA), and the scanning electron microscope (SEM) photograph of the cobalt molybdate of the synthesis is as shown in Figure 2.Meanwhile the molybdic acid of the synthesis
Through electro-chemical test, (test condition: using three electrode work systems to cobalt electrode material, and three-electrode system mainly includes work electricity
Pole, three electrodes of reference electrode and auxiliary electrode and electrolyte and diaphragm, while there are also to eliminate liquid potential and reduction
The Luggin capillary and salt bridge of solution resistance.Working electrode is the electrode material of this example preparation, conductive agent (carbon black), adhesive
(PTFE emulsion), ethyl alcohol are mixed in the case where mass ratio is about 75:15:10:10, and mixed pasty mixture is uniformly coated on
Collector (nickel foam, 1 × 1cm2) on, and be dried in vacuo, then electrode slice is depressed in the pressure of about 6MPa.Reference electrode
For mercury/mercury oxide (Hg/HgO), platinum guaze (Pt mesh) is auxiliary electrode, and electrolyte is potassium hydroxide solution, and diaphragm is cellulose
Film), the datagram for testing resulting specific capacitance value is as shown in Figure 3.The cobalt molybdate synthesized it can be seen from shown in Fig. 3
Electrode material specific capacitance value under the current density of 0.25A/g reaches 420F/g.
Preparating example 2
In the synthetic method of the cobalt molybdate for electrode material for super capacitor of this example, firstly, by cobalt nitrate (Co
(NO3)2) it with deionized water by the mass ratio of the material is that 0.003:1 carries out mixed dissolution, obtain solution A, then by pattern regulator ten
Sodium dialkyl sulfate, ammonium molybdate ((NH4)2MoO4) and deionized water by the mass ratio of the material be 0.001:0.003:1 mix it is molten
Solution is then added acid-base modifier potassium citrate and is adjusted to neutrality, obtains solution B.Then solution A is mixed in equal volume with solution B
Precipitation reaction is carried out after conjunction, for reaction temperature at 40 DEG C, the reaction time is 6 hours, is cooled down after reaction, and through deionization
Water, ethyl alcohol difference centrifuge washing three times, are finally dried in vacuo under conditions of vacuum degree is 0.8KPa, temperature is 60 DEG C
10h obtains cobalt molybdate.
This example synthesis cobalt molybdate electrode material use with the same electro-chemical test of example 1, in the electric current of 0.25A/g
Specific capacitance value reaches 480F/g under density.
Preparating example 3
In the synthetic method of the cobalt molybdate for electrode material for super capacitor of this example, firstly, by cobaltous bromide
(CoBr2) it with deionized water by the mass ratio of the material is that 0.003:1 carries out mixed dissolution, obtain solution A, then by pattern regulator ten
Six alkyl trimethyl ammonium bromides, nickel molybdate (NiMoO4) and deionized water by the mass ratio of the material be 0.002:0.004:1 mixed
Dissolution is closed, acid-base modifier sodium citrate is then added and is adjusted to neutrality, obtains solution B.Then by the bodies such as solution A and solution B
Carry out precipitation reaction after product mixing, for reaction temperature at 80 DEG C, the reaction time is 8 hours, cool down after reaction, and gone from
Sub- water, ethyl alcohol difference centrifuge washing three times, are finally dried in vacuo under conditions of vacuum degree is 0.8KPa, temperature is 60 DEG C
10h obtains cobalt molybdate.
This example synthesis cobalt molybdate electrode material use with the same electro-chemical test of example 1, in the electric current of 0.25A/g
Specific capacitance value reaches 380F/g under density.
Preparating example 4
In the synthetic method of the cobalt molybdate for electrode material for super capacitor of this example, firstly, by cobaltous sulfate
(CoSO4) it with deionized water by the mass ratio of the material is that 0.005:1 carries out mixed dissolution, obtain solution A, then by pattern regulator six
Methine tetramine, magnesium molybdate (MgMoO4) and deionized water by the mass ratio of the material be 0.002:0.005:1 carry out mixed dissolution, with
Acid-base modifier sodium citrate is added afterwards to be adjusted to neutrality, obtains solution B.Then solution A is mixed in equal volume with solution B laggard
Row precipitation reaction, for reaction temperature at 90 DEG C, the reaction time is 12 hours, is cooled down after reaction, and through deionized water, ethyl alcohol
Centrifuge washing three times, vacuum drying 10h is finally carried out under conditions of vacuum degree is 0.8KPa, temperature is 60 DEG C and obtains molybdenum respectively
Sour cobalt.
This example synthesis cobalt molybdate electrode material use with the same electro-chemical test of example 1, in the electric current of 0.25A/g
Specific capacitance value reaches 320F/g under density.
The obtained cobalt molybdate electrode material of synthetic method of the present embodiment exists it can be seen from above each preparating example
Specific capacitance value under the current density of 0.25A/g is between 320F/g-480F/g, substantially compared to existing molybdic acid cobalt electrode
Degree improves specific capacitance value.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of synthetic method of the cobalt molybdate for electrode material for super capacitor, it is characterised in that: the synthetic method packet
Include following step:
S1, cobalt salt and deionized water progress mixed dissolution are obtained into solution A；
S2, pattern regulator, molybdate and deionized water are subjected to mixed dissolution, and acid-base modifier is then added and is adjusted to
Neutrality obtains solution B；
S3, precipitation reaction is carried out after mixing solution A in equal volume with solution B, it is cooling after precipitation reaction, and washed drying
After obtain cobalt molybdate.
2. the synthetic method of the cobalt molybdate according to claim 1 for electrode material for super capacitor, it is characterised in that:
In step s1, the mass ratio of the material of cobalt salt and deionized water is (0.002-0.005): 1；In step s2, pattern regulator, molybdic acid
Molar ratio between salt and deionized water is (0.001-0.002): (0.002-0.005): 1.
3. the synthetic method of the cobalt molybdate according to claim 2 for electrode material for super capacitor, it is characterised in that:
In step s3, the reaction temperature of precipitation reaction is 25-90 DEG C, and the reaction time is 2-12 hours, and is to pass through centrifugation in step s3
Cobalt molybdate is obtained after washing and vacuum drying.
4. the synthetic method of the cobalt molybdate according to claim 3 for electrode material for super capacitor, it is characterised in that:
The centrifuge washing includes being washed respectively three times by deionized water and ethyl alcohol.
5. the synthetic method of the cobalt molybdate according to claim 3 for electrode material for super capacitor, it is characterised in that:
The vacuum drying is 10 hours dry under the conditions of vacuum degree 0.8KPa, temperature 60 C.
6. the synthetic method of the cobalt molybdate according to any one of claim 1 to 5 for electrode material for super capacitor,
It is characterized by: the cobalt salt is one of cobalt chloride hexahydrate, cobalt nitrate, cobaltous bromide and cobaltous sulfate.
7. the synthetic method of the cobalt molybdate according to any one of claim 1 to 5 for electrode material for super capacitor,
It is characterized by: the molybdate is one of sodium molybdate, ammonium molybdate, nickel molybdate and magnesium molybdate.
8. the synthetic method of the cobalt molybdate according to any one of claim 1 to 5 for electrode material for super capacitor,
It is characterized by: the pattern regulator is ammonium fluoride, lauryl sodium sulfate, cetyl trimethylammonium bromide and six first
One of urotropine.
9. the synthetic method of the cobalt molybdate according to any one of claim 1 to 5 for electrode material for super capacitor,
It is characterized by: the acid-base modifier is one of tripotassium phosphate, potassium citrate and sodium citrate.
10. the synthetic method of the cobalt molybdate according to claim 1 for electrode material for super capacitor, feature exist
In: specific capacitance value of the cobalt molybdate that step s3 is obtained under the current density of 0.25A/g is between 320F/g-480F/g.
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| CN110776016A (en) * | 2019-09-29 | 2020-02-11 | 河北科技大学 | Method for synthesizing electrode material cobalt tungstate for super capacitor |
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