CN106449148A - Method for preparing tubular manganese dioxide / poly-aniline / graphene composite material - Google Patents
Method for preparing tubular manganese dioxide / poly-aniline / graphene composite material Download PDFInfo
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- CN106449148A CN106449148A CN201611028065.2A CN201611028065A CN106449148A CN 106449148 A CN106449148 A CN 106449148A CN 201611028065 A CN201611028065 A CN 201611028065A CN 106449148 A CN106449148 A CN 106449148A
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- manganese dioxide
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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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 invention discloses a method for preparing tubular manganese dioxide / poly-aniline / graphene composite electrode material, belonging to the technical field of preparation of composite material. The method solves the problem of how to play advantages of various materials, and weakens defects caused by various materials. The preparation has material technical problems of high power density and good cycle stability of composite electrode. The preparation method is relatively simple and orderly. The tubular manganese dioxide / poly-aniline / graphene composite electrode materials prepared can take advantage of all kinds of materials, and weaken the defects caused by various materials, being a kind of composite electrode material with high power density and good cycle stability. The preparation has the advantages of low cost, high power density, and long cycle life.
Description
Technical field
The invention belongs to technical field of composite preparation, it is specifically related to a kind of tubulose manganese dioxide/polyaniline/graphite
The preparation method of alkene composite.
Background technology
Ultracapacitor is a kind of new type of energy storage device between electrolysis condenser and battery, has cycle life
Long, can high current charge-discharge the advantages of, but there is also internal resistance larger the shortcomings of.Electrode material for super capacitor mainly divides at present
For three classes, i.e. metal-oxide, conducting polymer and material with carbon element.
Manganese bioxide electrode material has rich reserves, cheap, environmentally friendly and performance in neutral electrolyte
Go out the feature of good chemical property, be a kind of important electrode material.Tubular material can make more active substances with
Electrolyte contacts, thus increase substantially the specific capacity of active substance.
Polyaniline electrode material is a kind of important conducting polymer, has that raw material is inexpensive, process is simple, electric conductivity and an electricity
The excellent advantage of chemical reversibility.But due in charging process because polyaniline is swelling and shrinks and makes the cyclicity of polyaniline
Serious impact can be received.
Graphene is a kind of more new carbon of Recent study, has good electric conductivity and high rate performance.
Graphene is combined with other materials, the special lamellar structure of Graphene can be utilized, mechanical property and the electricity of material can be improved
Sub- transmittability.
Three of the above material respectively has pluses and minuses.Above electrode material is combined making composite, using graphite
The good electric conductivity of alkene, long circulation life, high-specific surface area, metal-oxide fake capacitance capacity is high and conducting polymer is low interior
The characteristics such as resistance, low cost, make to produce cooperative effect between three kinds of electrode materials, and advantage combines, and defect weakens, and can significantly carry
The overall chemical property of high material.Have research worker at present and above material is prepared into combination electrode material, but all deposit
In certain problem.
The aqueous phase that patent 102977602A is made up of potassium permanganate solution and material with carbon element colloid solution, and by conducting polymer
The organic faciess that the monomer dispersion of thing is formed in organic solvent carry out two-phase interface oxidation polymerization obtain manganese dioxide/carbon material/
The complex of conducting polymer, in the method, the stability of manganese dioxide is improved, but electric conductivity is but affected.
Patent 103117175A describes a kind of multiple elements design nano material, including material with carbon element, metal oxygen-containing compound and
2 kinds in conducting polymer or 3 kinds.Though the method in this patent can offset defect between various materials simultaneously
Reduce the advantage of various materials.
Therefore, how can play the advantage of various materials, the defect that various materials bring can be weakened again, be to prepare one kind
There is the technical barrier of the combination electrode material art that power density is high, stable circulation performance is good.The present invention first with
Polyethyleneimine prepares tubular structure manganese dioxide for template, then coats polyaniline and Graphene successively, is prepared into one kind
Tubulose manganese dioxide/polyaniline/graphene combination electrode material, there is not been reported for correlation technique.
The present invention prepares tubular structure manganese dioxide with polyethyleneimine for template first, then coats polyaniline successively
And Graphene, it is prepared into a kind of tubulose manganese dioxide/polyaniline/graphene composite material, there is not been reported for correlation technique.
Content of the invention
In order to overcome the deficiencies in the prior art, the present invention provides a kind of tubulose manganese dioxide/polyaniline/Graphene to be combined
The preparation method of material, the combination electrode material prepared through the method has that with low cost, power density is high, cycle life
Long advantage, simultaneously under the premise of the advantage that can play various materials, weakens the defect that various materials bring.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of preparation method of tubulose manganese dioxide/polyaniline/graphene composite material, comprises the following steps：
1) polyethyleneimine and potassium permanganate are added in deionized water, stir, Deca additive synthesis adjust reactant
It is pH value, Hydrothermal Synthesiss are realized fully reacting；Potassium permanganate has strong oxidizing property, with reproducibility thing in certain pH value range
Qualitative response can prepare the manganese dioxide of special appearance, and polyethyleneimine is a kind of high molecular weight water soluble polymer, has relatively
High reactivity, has the effect of reducing agent and template in the present invention, in certain pH value range and potassium permanganate
Reaction Hydrothermal Synthesiss tubulose manganese dioxide.
2) reactant is washed with deionized, sucking filtration, then with absolute ethanol washing, sucking filtration, be vacuum dried, managed
Shape manganese dioxide；Deionized water cleaning is to clean the foreign ion in product, being because with washes of absolute alcohol
Dehydrated alcohol volatilization is fast, and product has more preferable dispersibility.
3) tubulose manganese dioxide is added in acid solution with aniline and stir, after fully reacting, be filtrated to get filter cake；Benzene
Easily there is oxidation reaction in amine, generate polyaniline, aniline is former on tubulose manganese dioxide surface in the present invention in an acidic solution
Position reaction generates polyaniline.
4) filter cake is washed with dilute hydrochloric acid, then deionized water is washed till filtrate neutrality, finally uses absolute ethanol washing, does
Dry, obtain tubulose manganese dioxide/polyaniline composite material；Dilute hydrochloric acid be in order to wash remove for be not combined polyaniline, go from
Sub- water washing is cleaning dilute hydrochloric acid, is because that dehydrated alcohol volatilization is fast with washes of absolute alcohol, and product has preferably divides
Scattered property.
5) tubulose manganese dioxide/polyaniline composite material is added in graphene oxide dispersion, carries out fully anti-
Should, it is filtrated to get filter cake, graphene oxide is the oxide of Graphene, make property because its oxygen-containing functional group increases compared with Graphene
More active, graphene oxide is because the basic surface in polyaniline occurs part deoxygenation to form tubulose in the present invention
Manganese dioxide/polyaniline and the combination product of graphene oxide.
6) by filter cake heat drying and reduce, that is, obtain tubulose manganese dioxide/polyaniline/graphene combination electrode material；
Oxygen-containing functional group in graphene oxide is unstable, can remove at a certain temperature.
Preferably, step 1）The consumption of middle polyethyleneimine is the 1-20wt% of deionized water in reaction system, potassium permanganate
Consumption be reaction system in deionized water 1-20wt%.
Preferably, step 1）Described in additive synthesis be ammonia, sodium hydroxide, potassium hydroxide, in Lithium hydrate one
Kind, additive synthesis set-up procedure 1）The pH value of reaction system is 7-9.In process of the test, applicant passes through lot of experimental data
Find, when the pH value of this reaction system is less than 7, product is the manganous compound of free state, when this reaction system
When pH value is more than 9, product is the manganate of free state.
Preferably, step 1）The temperature of middle Hydrothermal Synthesiss is 80 ~ 160 DEG C, and the time of Hydrothermal Synthesiss is 6 ~ 12h.
Preferably, step 2）In be washed with deionized, sucking filtration 2 times, then with absolute ethanol washing, sucking filtration 2 times, in 100-
It is vacuum dried 12h at 200 DEG C.
Preferably, step 3）Middle aniline is 0.01-0.5 with the mass ratio of tubulose manganese dioxide:1, acid solution be hydrochloric acid,
One of sulphuric acid, phosphoric acid, perchloric acid, reaction temperature is 5-10 DEG C, and the response time is 6-12h.
Preferably, step 4）The temperature of middle drying is 100 ~ 300 DEG C.
Preferably, step 5）The concentration of middle graphene oxide dispersion is 0.5-10mg/ml, graphene oxide and tubulose two
The mass ratio of manganese oxide is 2-5:10, reaction temperature is 40-50 DEG C, and the response time is 10-12h.
Preferably, step 6）The temperature of middle dry reduction is 100-200 DEG C.
It is an advantage of the invention that：Preparation technology is relatively easy in order, the tubulose manganese dioxide/polyaniline/graphite prepared
Alkene combination electrode material, can play the advantage of various materials, can weaken the defect that various materials bring again, be that one kind has work(
The combination electrode material that rate density is high, stable circulation performance is good, has that with low cost, power density is high, has extended cycle life
Advantage.
Brief description
The SEM of tubulose manganese dioxide/polyaniline/graphene combination electrode material that Fig. 1 obtains for the embodiment of the present invention 1
Figure；
Tubulose manganese dioxide/polyaniline/graphene combination electrode material that Fig. 2 obtains for the embodiment of the present invention 1 is through three electrodes
CV curve after system test；
The SEM figure of tubulose manganese dioxide/polyaniline/graphene combination electrode material that Fig. 3 obtains for the embodiment of the present invention 2；
Tubulose manganese dioxide/polyaniline/graphene combination electrode material that Fig. 4 obtains for the embodiment of the present invention 2 is through three electrodes
CV curve after system test；
The SEM figure of tubulose manganese dioxide/polyaniline/graphene combination electrode material that Fig. 5 obtains for the embodiment of the present invention 3；
Tubulose manganese dioxide/polyaniline/graphene combination electrode material that Fig. 6 obtains for the embodiment of the present invention 3 is through three electrodes
CV curve after system test.
The SEM figure of the final product that Fig. 7 obtains for comparative example；
CV curve after three-electrode system test for the final product that Fig. 8 obtains for comparative example.
Specific embodiment
Below in conjunction with accompanying drawing, the present invention is further illustrated：
Embodiment 1
（1）10g polyethyleneimine and 15g potassium permanganate are added in 100g deionized water, stir, Deca ammonia adjusts
Reaction system pH reacts 6h to 9,80 DEG C of hydrothermal reaction conditions, product is washed with deionized, sucking filtration 2 times, then uses
Absolute ethanol washing, sucking filtration 2 times, are finally vacuum dried 12h at 100 DEG C, prepare tubulose manganese dioxide.
（2）Addition 50ml hydrochloric acid by 1g tubulose manganese dioxide and 0.1g aniline（20wt%）In solution, stir and control anti-
Answer temperature at 5 DEG C, response time 10h, filters to product, is washed with dilute hydrochloric acid, then deionized water is washed till filtrate
Neutrality, then with absolute ethanol washing, be dried under the conditions of 100 DEG C, obtain tubulose manganese dioxide/polyaniline composite material.
（3）The above-mentioned tubulose manganese dioxide of 1g/polyaniline composite material is taken to add 50ml graphene oxide（1mg/ml）Point
In dispersion liquid, stir and controlling reaction temperature is at 40 DEG C, response time 12h, product is filtered, dry under the conditions of 200 DEG C
Dry reduction, obtains a kind of tubulose manganese dioxide/polyaniline/graphene combination electrode material.
Result and discussion：In scanning electron microscope (SEM) this combination electrode material of upper observation, result shows in composite simultaneously
There are tubular structure material and sheetlike material.CV curve after three-electrode system test for this combination electrode material（50mv/s）
Symmetry preferably, shows that this combination electrode material can play the advantage of various materials, and that can weaken that various materials bring lacks again
Fall into, be a kind of to there is the combination electrode material that power density is high, stable circulation performance is good.
Embodiment 2
（1）10g polyethyleneimine and 10g potassium permanganate are added in 150g deionized water, stir, Deca ammonia adjusts
Product is washed with deionized to 7,100 DEG C of hydrothermal reaction conditions by reaction system pH, sucking filtration 2 times, then uses anhydrous second
Alcohol washing, sucking filtration 2 times, are finally vacuum dried 12h at 150 DEG C, prepare tubulose manganese dioxide.
（2）Addition 10ml phosphoric acid by 1g tubulose manganese dioxide and 0.5g aniline（20wt%）In solution, stir and control anti-
Answer temperature at 8 DEG C, response time 12h, filters to product, is washed with dilute hydrochloric acid, then deionized water is washed till filtrate
Neutrality, then with absolute ethanol washing, be dried under the conditions of 60 DEG C, obtain tubulose manganese dioxide/polyaniline composite material.
（3）The above-mentioned tubulose manganese dioxide of 1g/polyaniline composite material is taken to add 40ml graphene oxide（5mg/ml）Point
In dispersion liquid, stir and controlling reaction temperature is at 40 DEG C, response time 12h, product is filtered, dry under the conditions of 150 DEG C
Dry reduction, obtains a kind of tubulose manganese dioxide/polyaniline/graphene combination electrode material.
Result and discussion：In scanning electron microscope (SEM) this combination electrode material of upper observation, result shows in composite simultaneously
There are tubular structure material and sheetlike material.CV curve after three-electrode system test for this combination electrode material（50mv/s）
Symmetry preferably, shows that this combination electrode material can play the advantage of various materials, and that can weaken that various materials bring lacks again
Fall into, be a kind of to there is the combination electrode material that power density is high, stable circulation performance is good.
Embodiment 3
（1）5g polyethyleneimine and 8g potassium permanganate are added in 120g deionized water, stir, the adjustment of Deca ammonia is anti-
Answer system pH to be washed with deionized product to 8,120 DEG C of hydrothermal reaction conditions, sucking filtration 2 times, then use dehydrated alcohol
Washing, sucking filtration 2 times, are finally vacuum dried 12h at 200 DEG C, prepare tubulose manganese dioxide.
（2）Addition 15ml phosphoric acid by 1g tubulose manganese dioxide and 0.4g aniline（20wt%）In solution, stir and control anti-
Answer temperature at 10 DEG C, response time 6h, filters to product, is washed with dilute hydrochloric acid, then deionized water is washed till filtrate
Neutrality, then with absolute ethanol washing, be dried under the conditions of 300 DEG C, obtain tubulose manganese dioxide/polyaniline composite material.
（3）The above-mentioned tubulose manganese dioxide of 1g/polyaniline composite material is taken to add 30ml graphene oxide（10mg/ml）Point
In dispersion liquid, stir and controlling reaction temperature is at 50 DEG C, response time 10h, product is filtered, dry under the conditions of 100 DEG C
Dry reduction, obtains a kind of tubulose manganese dioxide/polyaniline/graphene combination electrode material.
Result and discussion：In scanning electron microscope (SEM) this combination electrode material of upper observation, result shows in composite simultaneously
There are tubular structure material and sheetlike material.CV curve after three-electrode system test for this combination electrode material（50mv/s）
Symmetry preferably, shows that this combination electrode material can play the advantage of various materials, and that can weaken that various materials bring lacks again
Fall into, be a kind of to there is the combination electrode material that power density is high, stable circulation performance is good.
Comparative example
（1）10g polyethyleneimine and 15g potassium permanganate are added in 100g deionized water, stir, Deca ammonia adjusts
Reaction system pH reacts 6h to 10,80 DEG C of hydrothermal reaction conditions, product is washed with deionized, sucking filtration 2 times, then uses
Absolute ethanol washing, sucking filtration 2 times, are finally vacuum dried 12h at 100 DEG C, prepare black precipitate.
（2）Addition 50ml hydrochloric acid by 1g black precipitate and 0.1g aniline（20wt%）In solution, stir and control reaction temperature
Spend at 5 DEG C, response time 10h, product filtered, is washed with dilute hydrochloric acid, then deionized water is washed till filtrate neutrality,
Use absolute ethanol washing again, be dried under the conditions of 100 DEG C, obtain black precipitate.
（3）The above-mentioned black precipitate of 1g is taken to add 50ml graphene oxide（1mg/ml）In dispersion liquid, stir and control anti-
Answer temperature at 40 DEG C, response time 12h, filters to product, reduction is dried, obtains final product under the conditions of 200 DEG C.
Result and discussion：In scanning electron microscope (SEM) this product of upper observation, result shows not occurring tubulose in composite
Structural material and sheetlike material.CV curve after three-electrode system test for this product（50mv/s）Deviate considerably from square
Shape, and electric conductivity and specific capacity decline substantially, shows to deviate the preparation method of the present invention, prepared material in performance with
The present invention compares decline substantially.
Finally it should be noted that：Obviously, above-described embodiment is only intended to clearly illustrate example of the present invention, and simultaneously
The non-restriction to embodiment.For those of ordinary skill in the field, can also do on the basis of the above description
Go out change or the variation of other multi-forms.There is no need to be exhaustive to all of embodiment.And thus drawn
Obvious change that Shen goes out or change among still in protection scope of the present invention.
Claims (9)
1. a kind of preparation method of tubulose manganese dioxide/polyaniline/graphene composite material is it is characterised in that methods described bag
Include following steps：
1) polyethyleneimine and potassium permanganate are added in deionized water, stir, Deca additive synthesis adjust reactant
It is pH value, Hydrothermal Synthesiss are realized fully reacting；
2) reactant is washed with deionized, sucking filtration, then with absolute ethanol washing, sucking filtration, be vacuum dried, obtain tubulose dioxy
Change manganese；
3) tubulose manganese dioxide is added in acid solution with aniline and stir, after fully reacting, be filtrated to get filter cake；
4) filter cake is washed with dilute hydrochloric acid, then deionized water is washed till filtrate neutrality, finally uses absolute ethanol washing, is dried, obtains
To tubulose manganese dioxide/polyaniline composite material；
5) tubulose manganese dioxide/polyaniline composite material is added in graphene oxide dispersion, is fully reacted, filter
Obtain filter cake；
6) by filter cake heat drying and reduce, that is, obtain tubulose manganese dioxide/polyaniline/graphene combination electrode material.
2. a kind of preparation method of tubulose manganese dioxide/polyaniline/graphene composite material as claimed in claim 1, it is special
Levy and be, step 1）The consumption of middle polyethyleneimine is the 1-20wt% of deionized water, and the consumption of potassium permanganate is deionized water
1-20wt%.
3. a kind of preparation method of tubulose manganese dioxide/polyaniline/graphene composite material as claimed in claim 1, it is special
Levy and be, step 1）Described in additive synthesis be one of ammonia, sodium hydroxide, potassium hydroxide, Lithium hydrate, synthesis helps
Agent set-up procedure 1）The pH value of reaction system is 7-9.
4. a kind of preparation method of tubulose manganese dioxide/polyaniline/graphene composite material as claimed in claim 1, it is special
Levy and be, step 1）The temperature of middle Hydrothermal Synthesiss is 80 ~ 160 DEG C, and the time of Hydrothermal Synthesiss is 6 ~ 12h.
5. a kind of preparation method of tubulose manganese dioxide/polyaniline/graphene composite material as claimed in claim 1, it is special
Levy and be, step 2）In be washed with deionized, sucking filtration 2 times, then with absolute ethanol washing, sucking filtration 2 times, at 100-200 DEG C
Vacuum drying 12h.
6. a kind of preparation method of tubulose manganese dioxide/polyaniline/graphene composite material as claimed in claim 1, it is special
Levy and be, step 3）Middle aniline is 0.01-0.5 with the mass ratio of tubulose manganese dioxide:1, acid solution is hydrochloric acid, sulphuric acid, phosphorus
One of acid, perchloric acid, reaction temperature is 5-10 DEG C, and the response time is 6-12h.
7. a kind of preparation method of tubulose manganese dioxide/polyaniline/graphene composite material as claimed in claim 1, it is special
Levy and be, step 4）The temperature of middle drying is 100 ~ 300 DEG C.
8. a kind of preparation method of tubulose manganese dioxide/polyaniline/graphene composite material as claimed in claim 1, it is special
Levy and be, step 5）The concentration of middle graphene oxide dispersion is 0.5-10mg/ml, graphene oxide and tubulose manganese dioxide
Mass ratio is 2-5:10, reaction temperature is 40-50 DEG C, and the response time is 10-12h.
9. a kind of preparation method of tubulose manganese dioxide/polyaniline/graphene composite material as claimed in claim 1, it is special
Levy and be, step 6）The temperature of middle dry reduction is 100-200 DEG C.
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| CN117334886A (en) * | 2023-12-01 | 2024-01-02 | 广东容钠新能源科技有限公司 | Preparation method and application of polyaniline in-situ coated hard carbon material |
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| CN106449148B (en) | 2018-01-30 |
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