CN108766791A - A kind of preparation method of the ultracapacitor based on graphene/polyaniline laminated film - Google Patents
A kind of preparation method of the ultracapacitor based on graphene/polyaniline laminated film Download PDFInfo
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/02—Polyamines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene 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 present invention provides a kind of ultracapacitor and preparation method thereof based on graphene/polyaniline laminated film, belongs to capacitor electrode material and electrochemical energy storage technical field.The present invention includes：Graphene oxide is modified by anilino- is obtained after graphene oxide, aniline monomer reaction；So that the aniline monomer on anilino- modification graphene oxide is polymerize, obtains graphene oxide/polyaniline composite material；Graphene oxide/polyaniline composite material is added in graphene oxide solution, prepares graphene oxide/polyaniline pipe laminated film；Make graphene oxide/polyaniline laminated film that reduction reaction occur, obtains graphene/polyaniline laminated film；Graphene/polyaniline laminated film is assembled, the ultracapacitor based on graphene/polyaniline laminated film is obtained.The present invention makes polyaniline be graft-polymerized on the surface of graphene by amido, realizes that polyaniline and graphene are effectively compound, graphene/polyaniline laminated film has good flexibility.
Description
Technical field
The present invention relates to novel capacitor electrode materials and electrochemical energy storage technical field, and in particular to one kind is based on
The preparation method of the ultracapacitor of graphene/polyaniline laminated film.
Background technology
Tell development and the sharp increase of world population, tellurian resource consumption more and more tighter with economic society
Weight, environmental crisis is extremely urgent, therefore, find the technology of the new energy of clean and effective and energy storage conversion and equipment at
One of the research topic paid high attention to for the whole world.Ultracapacitor has the use of big specific capacitance, high energy density, length
The features such as service life, therefore it is one of important front edge research direction of electrochemical energy field of storage.Its developing trend at present
In miniaturization, flexibility.With portable and wearable electronic equipment fast development, high performance flexibility energy storage device replaces
For traditional hard electronic device, just seeming increasingly has market potential value.Flexible electrode material is wearable super electricity
The core component of container.
There is grapheme material high specific surface area and excellent electric conductivity, special two-dimension plane structure to make it have
More rich microstructure, and graphene itself has good film forming, is the reason for preparing flexible super capacitor electrode
Think one of material.But individually graphene sheet layer is easy to happen reunion stacking, and pure grapheme material only has electric double layer electric
Hold.Polyaniline has conjugated molecule structure and good physical and chemical performance as one of most promising conducting polymer.But
It is that pure polyaniline is insoluble, do not melt, it is difficult to which processing film forming cannot be directly used to construction flexible super capacitor.
It is multiple that a kind of ion liquid modified graphene/polyaniline is disclosed in the patent of Patent No. CN201310643616.6
The preparation method of film is closed, substrate sheet is placed on the polyphenyl aqueous amine by sulfonic group or carboxyl surface modification to the present invention by treated
It is soaked for a period of time in solution, taking-up, which is placed in deionized water, to be soaked for a period of time, and ion liquid modified graphite is put into after dry
Be soaked for a period of time in alkene aqueous dispersions, taking-up is placed on be soaked for a period of time in deionized water after it is dry, repeat above procedure, obtain
To the uniform film of graphene-polyaniline for having regular layer structure.
The polymerisation for carrying out aniline directly on graphene or graphene oxide structure in the prior art, is unfavorable for two
Person is uniformly compound, cannot achieve graphene with polyaniline in the compound of molecular level.
Invention content
To solve, polyaniline pure in the prior art is insoluble, does not melt, it is difficult to which it is flexible to cannot be directly used to construction for processing film forming
The non-uniform technological deficiency that polymerize of ultracapacitor, graphene and aniline, the present invention propose a kind of based on graphene/polyaniline
The preparation method of the ultracapacitor of laminated film, includes the following steps：
（1）Graphene oxide, aniline monomer dispersion are obtained into anilino- in a solvent, after reaction and modify graphene oxide, in oxygen
Anilino- functional group is grafted on graphite alkene；
（2）So that aniline monomer is polymerize using anilino- modification graphene oxide as carrier, graphene oxide/polyaniline is obtained
Composite material；Aniline monomer is graft-polymerized in the surface of graphene oxide containing anilino-, through centrifugation, washing, dries
To graphene oxide/polyaniline pipe composite material；
（3）Graphene oxide/the polyaniline composite material is added in graphene oxide solution, after dispersion, graphite oxide
Alkene/polyaniline composite material filters after disperseing together with graphene oxide again to be conducive to obtain fexible film, what this process used
Solvent can be distilled water, dimethylformamide, chloroform or n-butanol；
（4）Make the graphene oxide/polyaniline laminated film that reduction reaction occur, obtains graphene/polyaniline laminated film；
（5）By step（4）Obtained graphene/polyaniline laminated film is assembled, and is obtained compound based on graphene/polyaniline
The ultracapacitor of film.
Graphene and graphene oxide are all inorganic material, and polyaniline is organic material, if directly have graphene or
In the presence of person's graphene oxide, the polymerisation of aniline is carried out, it is uniformly compound to be unfavorable for the two.And in advance in graphene oxide table
After face is grafted anilino-, anilino- can react for aniline polymerization provides carrier scion grafting site, realizes that graphene exists with polyaniline
Molecular level it is compound.
Wherein, step（1）The graphene oxide, aniline monomer weight ratio be 1:1-1.5.Reaction temperature is 100-
110 DEG C, the reaction time is 12-36 hours.If the weight ratio of graphene oxide, aniline monomer is 1:1,1:1.3,1:1.5；Reaction
Temperature can be 100 DEG C, 105 DEG C, 110 DEG C；Reaction time can be 12h, 18h, 36h.
To ensure that polymerisation can be carried out fully, step（2）Middle addition oxidant and aniline, step（2）Middle anilino-
Modify graphene oxide, aniline, oxidant mass ratio be 1:1-2.5:3-10.If the ratio of three can be 1:2:6.Oxidation
Agent can be one or more in ammonium persulfate, ferric sulfate, iron chloride, ferric nitrate, if oxidant is ammonium persulfate.
Reduction reaction is important process, the reducing agent of reduction reaction be hydrochloric acid/potassium iodide mixed solution, hydrochloric acid/
One or both of sodium iodide mixed solution, reaction time of reduction reaction is 4~for 24 hours.
Step（5）Described in the electrolyte that uses of assembling be PVA/H2SO4Solid electrolyte, PVA/Na2SO4Solid-state electricity
Solve one or both of matter.
Polyaniline of the present invention is graft-polymerized on the surface of graphene by amido, realizes that polyaniline and graphene are effectively compound,
Reduce the aggregation of graphene；Graphene oxide/polyaniline composite material filters advantageous after disperseing together with graphene oxide again
In obtaining fexible film；The graphene/polyaniline laminated film obtained after reduction still maintains good flexibility, therefore is based on stone
The ultracapacitor of black alkene/polyaniline laminated film has bending restorability well.
Specific implementation mode
In order to better understand the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
Embodiment 1：
（1）The p-phenylenediamine of 0.1g graphene oxides, 0.1g is dispersed in the dimethylformamide of 150mL, 18 are reacted at 100 DEG C
Hour, obtain the graphene oxide containing anilino- functional group after centrifugation, washing, drying；
（2）The 0.1g graphene oxides for containing anilino- are dispersed in the hydrochloric acid of pH=1 of 10mL, be separately added into 0.1g aniline,
0.3g ammonium persulfates react 18 hours at 4 DEG C, and graphene oxide/polyaniline composite material is obtained after centrifugation, washing, drying；
（3）Graphene oxide/polyaniline composite material of 0.05g is added to graphene oxide solution（Solvent is distilled water, dense
Degree is 3mg/mL, volume 20mL）In, it is filtered after ultrasonic disperse 2h, obtains graphene oxide/polyaniline laminated film；
（4）Graphene oxide/polyaniline laminated film is immersed in hydrochloric acid/potassium iodide mixed solution, is obtained after reduction reaction 15h
Graphene/polyaniline laminated film；
（5）By two panels step（4）Obtained graphene/polyaniline laminated film, by PVA+H2SO4Solid electrolyte uniformly coats
Among two panels film, assembling obtains the ultracapacitor based on graphene/polyaniline laminated film.
Embodiment 2：
（1）The p-phenylenediamine of 0.15g graphene oxides, 0.225g is dispersed in the dimethylformamide of 200mL, it is anti-at 105 DEG C
It answers 24 hours, the graphene oxide containing anilino- is obtained after centrifugation, washing, drying；
（2）The 0.2g graphene oxides for containing anilino- are dispersed in the hydrochloric acid of pH=1 of 15mL, 0.5g aniline, 2g are separately added into
Ferric sulfate reacts 24 hours at 0 DEG C, and graphene oxide/polyaniline composite material is obtained after centrifugation, washing, drying；
（3）Graphene oxide/polyaniline composite material of 0.1g is added to graphene oxide solution（Solvent is chloroform, concentration
For 1mg/mL, volume 20mL）In, it is filtered after ultrasonic disperse 4h, obtains graphene oxide/polyaniline laminated film；
（4）Graphene oxide/polyaniline laminated film is immersed in hydrochloric acid/sodium iodide mixed solution, is obtained after reduction reaction 8h
Graphene/polyaniline laminated film；
（5）By two panels step（4）Obtained graphene/polyaniline laminated film, by PVA+H2SO4Solid electrolyte uniformly coats
Among two panels film, assembling obtains the ultracapacitor based on graphene/polyaniline laminated film.
Embodiment 3：
（1）The p-phenylenediamine of 0.35g graphene oxides, 0.4g is dispersed in the dimethylformamide of 350mL, is reacted at 105 DEG C
30 hours, the graphene oxide containing anilino- is obtained after centrifugation, washing, drying；
（2）The 0.15g graphene oxides for containing anilino- are dispersed in the hydrochloric acid of pH=1 of 20mL, be separately added into 0.3g aniline,
1.5g iron chloride reacts 36 hours at 0 DEG C, and graphene oxide/polyaniline composite material is obtained after centrifugation, washing, drying；
（3）Graphene oxide/polyaniline composite material of 0.12g is added to graphene oxide solution（Solvent is dimethyl methyl
Amide, a concentration of 4mg/mL, volume 30mL）In, it is filtered after ultrasonic disperse 6h, it is multiple to obtain graphene oxide/polyaniline
Close film；
（4）Graphene oxide/polyaniline laminated film is immersed in hydrochloric acid/potassium iodide mixed solution, is obtained after reduction reaction 10h
Graphene/polyaniline laminated film；
（5）By two panels step（4）Obtained graphene/polyaniline laminated film, by PVA+Na2SO4Solid electrolyte uniformly applies
It overlays among two panels film, assembling obtains the ultracapacitor based on graphene/polyaniline laminated film.
Embodiment 4：
（1）The p-phenylenediamine of 0.45g graphene oxides, 0.5g is dispersed in the dimethylformamide of 500mL, is reacted at 110 DEG C
32 hours, the graphene oxide containing anilino- is obtained after centrifugation, washing, drying；
（2）The 0.2g graphene oxides for containing anilino- are dispersed in the hydrochloric acid of pH=1 of 18mL, be separately added into 0.1g aniline,
0.9g ferric nitrates react 24 hours at 4 DEG C, and graphene oxide/polyaniline composite material is obtained after centrifugation, washing, drying；
（3）Graphene oxide/polyaniline composite material of 0.15g is added to graphene oxide solution（Solvent is n-butanol, dense
Degree is 4mg/mL, volume 40mL）In, it is filtered after ultrasonic disperse 8h, obtains graphene oxide/polyaniline laminated film；
（4）Graphene oxide/polyaniline laminated film is immersed in hydrochloric acid/sodium iodide mixed solution, is obtained after reduction reaction 4h
Graphene/polyaniline laminated film；
（5）By two panels step（4）Obtained graphene/polyaniline laminated film, by PVA+Na2SO4Solid electrolyte uniformly applies
It overlays among two panels film, assembling obtains the ultracapacitor based on graphene/polyaniline laminated film.
Embodiment 5：
（1）The p-phenylenediamine of 0.2g graphene oxides, 0.3g is dispersed in the n,N-Dimethylformamide of 300mL, it is anti-at 100 DEG C
It answers 36 hours, the graphene oxide containing anilino- is obtained after centrifugation, washing, drying；
（2）The 0.25g graphene oxides for containing anilino- are dispersed in the hydrochloric acid of pH=1 of 18mL, be separately added into 0.3g aniline,
0.8g ammonium persulfates react 28 hours at 4 DEG C, and graphene oxide/polyaniline composite material is obtained after centrifugation, washing, drying；
（3）Graphene oxide/polyaniline composite material of 0.18g is added to graphene oxide solution（Solvent is distilled water, dense
Degree is 10mg/mL, volume 30mL）In, it is filtered after ultrasonic disperse 10h, obtains graphene oxide/polyaniline THIN COMPOSITE
Film；
（4）Graphene oxide/polyaniline laminated film is immersed in hydrochloric acid/potassium iodide mixed solution, is obtained after reduction reaction 22h
Graphene/polyaniline laminated film；
（5）By two panels step（4）Obtained graphene/polyaniline laminated film, PVA+H2SO4 solid electrolytes are uniformly coated
Among two panels film, assembling obtains the ultracapacitor based on graphene/polyaniline laminated film.
Ultracapacitor based on graphene/polyaniline laminated film made from Example 1-5 carries out chemical property
Test experiments.It was found that this ultracapacitor can be arbitrarily bent, and bending has little effect its chemical property.It recycles volt
Peace curve is rectangular and area is larger, time-measuring electric potential curve symmetric, and the specific capacitance under 1A/g current densities is 126F/g, is
Ideal flexible super capacitor.
Polyaniline of the present invention is graft-polymerized on the surface of graphene by amido, realizes that polyaniline and graphene are effectively compound,
Reduce the aggregation of graphene；Graphene oxide/polyaniline composite material filters advantageous after disperseing together with graphene oxide again
In obtaining fexible film；The graphene/polyaniline laminated film obtained after reduction still maintains good flexibility, therefore is based on stone
The ultracapacitor of black alkene/polyaniline laminated film has bending recoverability well.
The present invention is not limited to above-mentioned specific embodiment, and the invention may be variously modified and varied.Every foundation
The technical spirit of the present invention should be included in the present invention to embodiment of above any modification, equivalent replacement, improvement and so on
Protection domain.
Claims (7)
1. a kind of preparation method of the ultracapacitor based on graphene/polyaniline laminated film, which is characterized in that including with
Lower step：
（1）Graphene oxide, aniline monomer dispersion are obtained into anilino- in a solvent, after reaction and modify graphene oxide；
（2）So that aniline monomer is polymerize using anilino- modification graphene oxide as carrier, graphene oxide/polyaniline is obtained
Composite material；
（3）Graphene oxide/the polyaniline composite material is added in graphene oxide solution, after dispersion, is aoxidized
Graphene/polyaniline pipe laminated film；
（4）Make the graphene oxide/polyaniline laminated film that reduction reaction occur, obtains graphene/polyaniline laminated film；
（5）By step（4）Obtained graphene/polyaniline laminated film is assembled, and is obtained compound based on graphene/polyaniline
The ultracapacitor of film.
2. preparation method according to claim 1, which is characterized in that step（1）The graphene oxide, aniline monomer
Weight ratio is 1:1-1.5.
3. preparation method according to claim 1, which is characterized in that step（2）Middle addition oxidant and aniline, step
（2）Middle anilino- modification graphene oxide, aniline, oxidant mass ratio be 1:1-2.5:3-10.
4. preparation method according to claim 3, which is characterized in that the oxidant is ammonium persulfate, ferric sulfate, chlorination
It is one or more in iron, ferric nitrate.
5. preparation method according to claim 1, which is characterized in that step（4）The reducing agent of the reduction reaction is salt
One or both of acid/potassium iodide mixed solution, hydrochloric acid/sodium iodide mixed solution.
6. preparation method according to claim 5, which is characterized in that the reaction time of the reduction reaction be 4~for 24 hours.
7. preparation method according to claim 6, which is characterized in that step（5）Described in the electrolyte that uses of assembling
It is PVA/H2SO4Solid electrolyte, PVA/Na2SO4One or both of solid electrolyte.
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| CN109456478A (en) * | 2018-10-22 | 2019-03-12 | 东华大学 | A kind of preparation method of graphene/polyaniline binary absorbing material |
| CN110289176A (en) * | 2019-02-25 | 2019-09-27 | 常州大学 | A kind of preparation method for the polyaniline grafted redox graphene/multi-wall carbon nano-tube composite material can be used for electrochemical energy storage |
| CN113628896A (en) * | 2021-08-13 | 2021-11-09 | 深圳市汉嵙新材料技术有限公司 | Preparation method of graphene flexible electrode composite membrane |
| CN115206689A (en) * | 2022-07-07 | 2022-10-18 | 浙江理工大学 | Graphene modified material and preparation method thereof |
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