CN110176363A - The preparation method of porous carbon load nano material of manganese dioxide - Google Patents
The preparation method of porous carbon load nano material of manganese dioxide Download PDFInfo
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- CN110176363A CN110176363A CN201910395977.0A CN201910395977A CN110176363A CN 110176363 A CN110176363 A CN 110176363A CN 201910395977 A CN201910395977 A CN 201910395977A CN 110176363 A CN110176363 A CN 110176363A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
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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 kind of preparation methods of porous carbon load nano material of manganese dioxide.Porous carbon and potassium permanganate are 1:4~1:16 grinding by the method in mass ratio, are dispersed in water, and are added after the concentrated sulfuric acid is uniformly mixed, and heating in water bath for reaction obtains porous carbon load nano material of manganese dioxide.The method of the present invention is simple and easy to do, and the physical property of the nano material of synthesis is relatively stable, and specific capacitance has preferable chemical property up to 337F/g, as super capacitor material.
Description
Technical field
The invention belongs to electrode material preparation technical fields, are related to a kind of system of porous carbon load nano material of manganese dioxide
Preparation Method.
Background technique
Supercapacitor has many advantages, such as that high-energy density, high power density and charging are fast, focuses in energy market performance
The effect wanted.In supercapacitor, fake capacitance can be obtained since quick redox reaction can occur than electric double layer electricity
Hold higher capacitance and energy density.Comprehensively consider environment friendly, cost-effectiveness and natural abundance, manganese dioxide becomes
By the material of favor in electrode material for super capacitor.In general, the supporting substrate of manganese dioxide uses graphene or carbon nanometer
Pipe, but their synthesis technology is comparatively laborious and cannot be mass produced, cost is also higher.
Currently, the method for synthesis manganese dioxide composite material is mainly oxidation-reduction method, electrodeposition process, hydro-thermal method and water-bath
Method.Chinese patent application CN108922790A is mixed using manganese dioxide/nitrogen that oxidation-reduction method has synthesized a kind of sodium ion insertion
Miscellaneous porous carbon composite, this method obtains porous carbon firstly the need of synthesis carbon matrix precursor, then high-temperature calcination, finally by longer
The redox reaction synthetic composite material of time, this method is longer experimental period, complex steps, the material capacitor of synthesis compared with
It is low, only 217F/g.Chinese patent application CN105390697A, in porous supported on carbon surface manganese dioxide, is somebody's turn to do using electrodeposition process
Method energy consumption is higher, and the condition for needing to regulate and control is more, such as reaction system pH, current density, temperature, constant current or pulse electrolysis
The parameters such as time need accuracy controlling.Chinese patent application CN102664277A uses hydro-thermal method, but hydro-thermal method requires high temperature
And it takes a long time；In addition immersion method is additionally used, but needs that MnCl is added in the synthesis process2·4H2O, and manganese is as a huge sum of money
Belong to, there is certain harm to environment.
Summary of the invention
The purpose of the present invention is to provide it is a kind of it is simple and easy, received with the porous carbon load manganese dioxide compared with high specific capacitance
The preparation method of rice material.
Realize that the technical solution of the object of the invention is as follows:
The preparation method of porous carbon load nano material of manganese dioxide, the specific steps are as follows:
It is 1:4~1:16 by the mass ratio of porous carbon and potassium permanganate, grinds, add after porous carbon and potassium permanganate are mixed
Water is stirred to after being uniformly dispersed, and 98% concentrated sulfuric acid is added, continues to be uniformly mixed, is placed in water-bath heating stirring at 80~90 DEG C
Reaction successively uses water, ethyl alcohol centrifuge washing to neutrality after reaction, is dried to obtain porous carbon load manganese dioxide nano material
Material.
Preferably, the mass ratio of the porous carbon and potassium permanganate is 1:8~1:16.
Preferably, the time added water and stirred is 10~30min.
Preferably, the volume ratio of 98% concentrated sulfuric acid and water is 1:4000~6:4000, more preferably 3:4000.
Preferably, the heating water bath time is 1~2h.
Preferably, the drying temperature is 50~100 DEG C.
Compared with prior art, the invention has the following advantages that the method for the present invention is simple and easy, process is simple, time-consuming short,
Without high-temperature process, nanocomposite physico-chemical property obtained is stablized, and specific capacitance reaches 337F/g, has good electrification
Performance is learned, large scale preparation is suitable for.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of 1 material prepared of embodiment.
Fig. 2 is 1 material prepared (a) cyclic voltammetry curve of embodiment, (b) charging and discharging curve figure.
Fig. 3 is 2 material prepared (a) cyclic voltammetry curve of embodiment, (b) charging and discharging curve figure.
Fig. 4 is 3 material prepared (a) cyclic voltammetry curve of embodiment, (b) charging and discharging curve figure.
Fig. 5 is 4 material prepared (a) cyclic voltammetry curve of embodiment, (b) charging and discharging curve figure.
Fig. 6 is 5 material prepared (a) cyclic voltammetry curve of embodiment, (b) charging and discharging curve figure.
Fig. 7 is 6 material prepared (a) cyclic voltammetry curve of embodiment, (b) charging and discharging curve figure.
Fig. 8 is 1 material prepared (a) cyclic voltammetry curve of comparative example, (b) charging and discharging curve figure.
Fig. 9 is 2 material prepared (a) cyclic voltammetry curve of comparative example, (b) charging and discharging curve figure.
Figure 10 is the scanning electron microscope (SEM) photograph of 3 material prepared of comparative example.
Figure 11 is 4 material prepared (a) cyclic voltammetry curve of comparative example, (b) charging and discharging curve figure.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
The preparation of porous carbon of the invention can with bibliography [Marta Sevilla and Antonio B.Fuertes,
Direct Synthesis of Highly PorousInterconnected Carbon Nanosheetsand Their
Application as High-Performance Supercapacitors, Acs Nano, 2014,5,5069-5078.],
Specifically:
After the grinding of 2g potassium citrate, it is placed in tube furnace, under the protection of inert nitrogen gas, with the liter of 3 DEG C/min
Warm rate is warming up to 750 DEG C of calcining 2h, and after natural cooling, product is taken out, with hydrochloric acid and water washing centrifugation removal impurity and
It is dried in baking oven, obtains porous carbon materials.
Embodiment 1
In mass ratio it is 1:8 grinding by porous carbon and potassium permanganate, is scattered in 20ml deionized water and stirs 30min,
After adding 15uL concentrated sulfuric acid stirring 2h, heating water bath and 2h is stirred at 80 DEG C, with deionized water, ethyl alcohol centrifuge washing into
Property, 60 DEG C of vacuum oven drying are placed in, the nano material of porous carbon load manganese dioxide is obtained.
Embodiment 2
In mass ratio it is 1:4 grinding by porous carbon and potassium permanganate, is scattered in 20ml deionized water and stirs 30min,
After adding 15uL concentrated sulfuric acid stirring 2h, heating water bath and 2h is stirred at 80 DEG C, with deionized water, ethyl alcohol centrifuge washing into
Property, 60 DEG C of vacuum oven drying are placed in, a kind of nano material of porous carbon load manganese dioxide is obtained.
Embodiment 3
In mass ratio it is 1:16 grinding by porous carbon and potassium permanganate, is scattered in 20ml deionized water and stirs 30min,
After adding 15uL concentrated sulfuric acid stirring 2h, heating water bath and 2h is stirred at 80 DEG C, with deionized water, ethyl alcohol centrifuge washing into
Property, 60 DEG C of vacuum oven drying are placed in, the nano material of porous carbon load manganese dioxide is obtained.
Embodiment 4
In mass ratio it is 1:8 grinding by porous carbon and potassium permanganate, is scattered in 20ml deionized water and stirs 30min,
After adding 5uL concentrated sulfuric acid stirring 2h, heating water bath and DEG C stirring 2h at 80 DEG C, with deionized water, ethyl alcohol centrifuge washing into
Property, 60 DEG C of vacuum oven drying are placed in, the nano material of porous carbon load manganese dioxide is obtained.
Embodiment 5
In mass ratio it is 1:8 grinding by porous carbon and potassium permanganate, is scattered in 20ml deionized water and stirs 30min,
After adding 30uL concentrated sulfuric acid stirring 2h, heating water bath and 2h is stirred at 80 DEG C, with deionized water, ethyl alcohol centrifuge washing into
Property, 60 DEG C of vacuum oven drying are placed in, the nano material of porous carbon load manganese dioxide is obtained.
Embodiment 6
In mass ratio it is 1:8 grinding by porous carbon and potassium permanganate, is scattered in 20ml deionized water and stirs 30min,
After adding 15uL concentrated sulfuric acid stirring 2h, heating water bath and 2h is stirred at 90 DEG C, with deionized water, ethyl alcohol centrifuge washing into
Property, 60 DEG C of vacuum oven drying are placed in, the nano material of porous carbon load manganese dioxide is obtained.
Comparative example 1
In mass ratio it is 1:2 grinding by porous carbon and potassium permanganate, is scattered in 20ml deionized water and stirs 30min,
After adding 15uL concentrated sulfuric acid stirring 2h, heating water bath and 2h is stirred at 80 DEG C, with deionized water, ethyl alcohol centrifuge washing into
Property, 60 DEG C of vacuum oven drying are placed in, the nano material of porous carbon load manganese dioxide is obtained.
Comparative example 2
In mass ratio it is 1:8 grinding by porous carbon and potassium permanganate, is scattered in 20ml deionized water and stirs 30min,
After adding 60uL concentrated sulfuric acid stirring 2h, heating water bath and 2h is stirred at 80 DEG C, with deionized water, ethyl alcohol centrifuge washing into
Property, 60 DEG C of vacuum oven drying are placed in, the nano material of porous carbon load manganese dioxide is obtained.
Comparative example 3
In mass ratio it is 1:8 grinding by porous carbon and potassium permanganate, is scattered in 20ml deionized water and stirs 30min,
Heating water bath and 2h is stirred at 80 DEG C, with deionized water, ethyl alcohol centrifuge washing to neutrality, is placed in 60 DEG C of vacuum oven drying,
Obtain product.
Comparative example 4
In mass ratio it is 1:8 grinding by porous carbon and potassium permanganate, is scattered in 20ml deionized water and stirs 30min,
After adding 15uL concentrated sulfuric acid stirring 2h, heating water bath and 2h is stirred at 70 DEG C, with deionized water, ethyl alcohol centrifuge washing into
Property, 60 DEG C of vacuum oven drying are placed in, a kind of nano material of porous carbon load manganese dioxide is obtained.
Fig. 1 is the scanning electron microscope (SEM) photograph of 1 material prepared of embodiment, and as can be seen from the figure porous carbon load manganese dioxide is protected
Vesicular texture is held, and manganese dioxide thin slice is crosslinked mutually, aperture is about 0.9 nanometer, and wall thickness is about 200 nanometers.
Fig. 2 is 1 material prepared (a) cyclic voltammetry curve of embodiment, (b) charging and discharging curve figure, it was found from curve
The specific capacitance of 1 material prepared of embodiment is 337F/g, specific capacitance with higher.
Fig. 3 is 2 material prepared (a) cyclic voltammetry curve of embodiment, (b) charging and discharging curve figure, it was found from curve
The specific capacitance of 2 material prepared of embodiment is 169.6F/g.
Fig. 4 is 3 material prepared (a) cyclic voltammetry curve of embodiment, (b) charging and discharging curve figure, it was found from curve
The specific capacitance of 3 material prepared of embodiment is 232.6F/g, specific capacitance with higher.
Fig. 5 is 4 material prepared (a) cyclic voltammetry curve of embodiment, (b) charging and discharging curve figure, it was found from curve
The specific capacitance of 4 material prepared of embodiment is 166.4F/g.
Fig. 6 is 5 material prepared (a) cyclic voltammetry curve of embodiment, (b) charging and discharging curve figure, it was found from curve
The specific capacitance of 5 material prepared of embodiment is 152.2F/g.
Fig. 7 is 6 material prepared (a) cyclic voltammetry curve of embodiment, (b) charging and discharging curve figure, it was found from curve
The specific capacitance of 6 material prepared of embodiment is 293F/g, specific capacitance with higher.
Fig. 8 is 1 material prepared (a) cyclic voltammetry curve of comparative example, (b) charging and discharging curve figure, it was found from curve
The specific capacitance of 1 material prepared of comparative example is 84.6F/g, has low specific capacitance.
Fig. 9 is 2 material prepared (a) cyclic voltammetry curve of comparative example, (b) charging and discharging curve figure, it was found from curve
The specific capacitance of 2 material prepared of comparative example is 126F/g, has low specific capacitance.
Figure 10 is the scanning electron microscope (SEM) photograph of 3 material prepared of comparative example, it can be seen that porous carbon surface is substantially without titanium dioxide
The presence of manganese nanometer sheet, it was demonstrated that the addition of the concentrated sulfuric acid is to the compound critically important of material.
Figure 11 is 4 material prepared (a) cyclic voltammetry curve of comparative example, (b) charging and discharging curve figure, it was found from curve
The specific capacitance of 4 material prepared of comparative example is 170F/g, has low specific capacitance.
Claims (7)
1. the preparation method of porous carbon load nano material of manganese dioxide, which is characterized in that specific step is as follows:
It is 1:4~1:16 by the mass ratio of porous carbon and potassium permanganate, is ground after porous carbon and potassium permanganate are mixed, water is added to stir
It mixes to after being uniformly dispersed, 98% concentrated sulfuric acid is added, continues to be uniformly mixed, it is anti-to be placed in water-bath heating stirring at 80~90 DEG C
It answers, after reaction, successively uses water, ethyl alcohol centrifuge washing to neutrality, be dried to obtain porous carbon load nano material of manganese dioxide.
2. preparation method according to claim 1, which is characterized in that the mass ratio of the porous carbon and potassium permanganate is
1:8~1:16.
3. according to claim 1 or the preparation method, which is characterized in that the time added water and stirred is 10~
30min。
4. preparation method according to claim 1 or 2, which is characterized in that the volume ratio of 98% concentrated sulfuric acid and water
For 1:4000~6:4000.
5. preparation method according to claim 1 or 2, which is characterized in that the volume ratio of 98% concentrated sulfuric acid and water
For 3:4000.
6. preparation method according to claim 1 or 2, which is characterized in that the heating water bath time is 1~2h.
7. preparation method according to claim 1 or 2, which is characterized in that the drying temperature is 50~100 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111554515A (en) * | 2020-05-11 | 2020-08-18 | 周小飞 | MnO (MnO)2Supercapacitor electrode material for modifying biomass porous carbon and preparation method thereof |
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| CN102568855A (en) * | 2012-03-12 | 2012-07-11 | 重庆大学 | Carbon material-loading manganese dioxide nanowire array composite and method for producing same |
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Application publication date: 20190827 |