CN106935411A - A kind of preparation of Graphene/mesoporous carbon spheres/array polyaniline material - Google Patents
A kind of preparation of Graphene/mesoporous carbon spheres/array polyaniline material Download PDFInfo
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- CN106935411A CN106935411A CN201710280640.6A CN201710280640A CN106935411A CN 106935411 A CN106935411 A CN 106935411A CN 201710280640 A CN201710280640 A CN 201710280640A CN 106935411 A CN106935411 A CN 106935411A
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- graphene
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- mesoporous carbon
- carbon spheres
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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
- H01G11/32—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
- H01G11/48—Conductive polymers
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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 relates to a kind of preparation method of Graphene/mesoporous carbon spheres/array polyaniline material.Comprise the following steps：The preparation of mesoporous silicon oxide, the preparation of mesoporous carbon spheres, the preparation of Graphene/mesoporous carbon spheres/polyaniline.The beneficial effects of the invention are as follows the preparation method novel and unique of Graphene/mesoporous carbon spheres/polyaniline trielement composite material.
Description
Technical field
The present invention relates to a kind of preparation method of Graphene/mesoporous carbon spheres/array polyaniline composite material, belong to material conjunction
Into with electrochemical research field.
Technical background
Electrode material with Graphene as matrix is always the focus of research in recent years, and Graphene has electricity higher
Conductance and specific surface area cause that Graphene has good chemical property, and the shortcoming that Graphene is easily reunited limits its capacitive character
Can, the compound specific surface area for preventing Graphene from electrode material is also add while reunion of Graphene and conducting polymer.It is poly-
There is conductance higher after aniline acid doping, the electronics conduction velocity in charge and discharge process is increased, what polyaniline was produced is
Faraday's electric capacity, is conducive to improving the electric capacity of whole capacitor, and for polyaniline, the addition of Graphene is served well
Fixation, improve polyaniline in charge and discharge process because swelling and shrink cause easily cave in, soluble, stability and
The defects such as charge-discharge cycle difference.The polyaniline of unique ordered structure can provide relatively short ion diffusion path, super
More preferable capacitive property can be shown in level capacitor, aniline aggregation growth on mesoporous carbon spheres is formed the same of array polyaniline
When with Graphene be combined, the polyaniline of ordered structure can also improve capacitive property while preventing Graphene from reuniting.Therefore I
Provide a successful route synthesizing graphite alkene/mesoporous carbon spheres/array polyaniline.
The content of the invention
It is to provide a kind of preparation side of Graphene/mesoporous carbon spheres/array polyaniline composite material that the purpose of the present invention is
Method.
A kind of preparation method of Graphene/mesoporous carbon spheres/array polyaniline composite material of the present invention includes following step
Suddenly：
A, prepare mesoporous silicon dioxide nano particle：By 22.8mL ethanol and CTAB at 60 DEG C
Powder is added in 145.2mL deionized waters and stirs, and after CTAB is completely dissolved, adds ammoniacal liquor and protects
Hold 60 DEG C to continue to stir 30min, 14.6mL tetraethyl orthosilicates be added dropwise, continue to stir 2h at 60 DEG C, suspension is cooled to room temperature,
It is centrifuged 10min under 4000rpm, reclaims solid product and with deionized water and ethanol cyclic washing, dried product is last
6h is calcined in atmosphere；
The preparation of b, mesoporous carbon spheres：Glucose is dissolved in 25mL deionized waters, the silica that will be prepared in step a
Add above-mentioned solution, be stirred vigorously 15min, by mixed solution be transferred in the stainless steel autoclave of 30mL teflon linings and
Heat 4h at 180 DEG C, autoclave is in atmosphere by product filtering and cyclic washing, 60 in distilled water and ethanol after natural cooling
After being dried at DEG C, sample calcines 4h in nitrogen atmosphere in tube furnace, be dispersed in after cooling in 10% hydrofluoric acid solution 24h with
Silica masterplate is removed, with distilled water and ethanol cyclic washing product, last freeze-drying；
The preparation of c, Graphene/mesoporous carbon spheres/array polyaniline composite material：By what is prepared in graphene oxide and b
Mesoporous carbon spheres are added in the ethanol of the 20mL 20% containing 2.28g aniline and hydrochloric acid, are stirred vigorously 1h, by 20mL's 20%
Ethanol is added rapidly in above-mentioned solution, and 0.644g ammonium persulfates are dissolved in 1mL deionized waters and above-mentioned solution is added dropwise over
In, add zinc powder, ultrasonically treated 15min to add 5mL dissolving with hydrochloric acid excess zinc powder after 10h is stirred at 0 DEG C, with excessive water and
Freeze-drying after alcohol flushing.
Further, the amount of CTAB is 3~6g in step a, and ammoniacal liquor is 1~3mL, and calcining heat is
400~600 DEG C.
Further, the amount of glucose is 2~3g in the step b, and the amount of silica is 0.5~1.5g, in tube furnace
Calcining heat is 700~900 DEG C.
Further, the amount of graphene oxide is 3~6mg in the step c, and mesoporous carbon spheres are 0.5~1.5g, and hydrochloric acid is 2
~4mL, zinc powder is 300~600mg.
The beneficial effects of the invention are as follows：The preparation method of Graphene/mesoporous carbon spheres/array polyaniline composite material is novel solely
It is special.
Specific embodiment
Presently in connection with specific embodiment, the present invention will be further described, and following examples are intended to illustrate rather than
Limitation of the invention further.
Embodiment one：
The preparation method of Graphene/mesoporous carbon spheres/array polyaniline material, comprises the following steps：
(1) 22.8mL ethanol and 5.73g CTAB powder are added to 145.2mL and are gone at 60 DEG C
In ionized water and stir, after CTAB is completely dissolved, 1.25mL ammoniacal liquor is added in mixture, protect
After holding 60 DEG C of continuation stirring 30min, 14.6mL tetraethyl orthosilicates are added dropwise, continue to stir 2h at 60 DEG C, suspension is cooled to room
Temperature, is centrifuged 10min under 4000rpm, reclaims solid product and with deionized water and ethanol cyclic washing, and dried product is most
6h is calcined in atmosphere at 550 DEG C afterwards, obtains mesoporous silicon oxide.
(2) 2.25g glucose is dissolved in 25mL deionized waters, is subsequently adding the titanium dioxide prepared in 1g steps (1)
Silicon, after 15min is stirred vigorously, mixed solution is transferred in the stainless steel autoclave of 30mL teflon linings and at 180 DEG C
Lower heating 4h, autoclave is in atmosphere after natural cooling by product filtering and the cyclic washing in distilled water and ethanol, at 60 DEG C
After drying, sample calcines 4h in the nitrogen atmosphere in tube furnace at 750 DEG C, is taken out after cooling and is immersed in 10% hydrofluoric acid solution
To remove silica masterplate, with distilled water and ethanol cyclic washing product, last freeze-drying, mesoporous carbon is prepared within 24 hours
Ball.
(3) the mesoporous carbon spheres 1g prepared in graphene oxide 4mg and (2) is added to and contains 2.8g aniline and 3.3mL
In the ethanol of the 20mL 20% of hydrochloric acid, 1h is stirred vigorously, the ethanol of 20mL 20% is added rapidly in above-mentioned solution, will
0.644g ammonium persulfates are dissolved in 3mL deionized waters and are added dropwise in above-mentioned solution, and 500mg is added after stirring 10h at 0 DEG C
Zinc powder, ultrasonically treated 15min adds 5mL dissolving with hydrochloric acid excess zinc powder, with freeze-drying after excessive water and alcohol flushing, prepares
Go out Graphene/mesoporous carbon spheres/array polyaniline.
Claims (4)
1. a kind of preparation method of Graphene/mesoporous carbon spheres/array polyaniline composite material, it is characterised in that：Step is as follows：
A, prepare mesoporous silicon dioxide nano particle：By 22.8mL ethanol and CTAB powder at 60 DEG C
It is added in 145.2mL deionized waters and stirs, after CTAB is completely dissolved, adds ammoniacal liquor and holding 60
DEG C continue stir 30min, be added dropwise 14.6mL tetraethyl orthosilicates, 60 DEG C continue stir 2h, suspension is cooled to room temperature,
It is centrifuged 10min under 4000rpm, reclaims solid product and with deionized water and ethanol cyclic washing, dried product finally exists
6h is calcined in air；
The preparation of b, mesoporous carbon spheres：Glucose is dissolved in 25mL deionized waters, the silica that will be prepared in step a is added
Above-mentioned solution, is stirred vigorously 15min, and mixed solution is transferred in the stainless steel autoclave of 30mL teflon linings and 180
Heat 4h at DEG C, autoclave is in atmosphere by product filtering and the cyclic washing in distilled water and ethanol, 60 DEG C after natural cooling
After lower drying, sample calcines 4h in nitrogen atmosphere in tube furnace, and 24h is to remove during 10% hydrofluoric acid solution is dispersed in after cooling
Silica masterplate is removed, with distilled water and ethanol cyclic washing product, last freeze-drying；
The preparation of c, Graphene/mesoporous carbon spheres/array polyaniline composite material：It is mesoporous by what is prepared in graphene oxide and b
Carbon ball is added in the ethanol of the 20mL 20% containing 2.28g aniline and hydrochloric acid, is stirred vigorously 1h, by the ethanol of 20mL 20%
It is added rapidly in above-mentioned solution, 0.644g ammonium persulfates is dissolved in 1mL deionized waters and are added dropwise in above-mentioned solution,
Zinc powder, ultrasonically treated 15min is added to add 5mL dissolving with hydrochloric acid excess zinc powder, rushed with excessive water and ethanol after 10h is stirred at 0 DEG C
Wash rear freeze-drying.
2. a kind of preparation method of Graphene/mesoporous carbon spheres/array polyaniline composite material according to claim 1, it is special
Levying is：CTAB is 3~6g in the step a, and ammoniacal liquor is 1~3mL, and calcining heat is 400~600
℃。
3. a kind of preparation method of Graphene/mesoporous carbon spheres/array polyaniline composite material according to claim 1, it is special
Levying is：The amount of glucose is 2~3g in the step b, and the amount of silica is 0.5~1.5g, and calcining heat is in tube furnace
700~900 DEG C.
4. a kind of preparation method of Graphene/mesoporous carbon spheres/array polyaniline composite material according to claim 1, it is special
Levying is：The amount of graphene oxide is 3~6mg in the step c, and mesoporous carbon spheres are 0.5~1.5g, and hydrochloric acid is 2~4mL, zinc powder
It is 300~600mg.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109065896A (en) * | 2018-08-15 | 2018-12-21 | 山东建筑大学 | The nanometer-material-modified anode of microbial fuel cell preparation method of mesoporous silicon oxide/polypyrrole |
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