CN104934236A - Method of preparing electroactive molecule grafted graphene doped conductive polymer electrode materials - Google Patents
Method of preparing electroactive molecule grafted graphene doped conductive polymer electrode materials 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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- 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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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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
Provided is a method of preparing electroactive molecule grafted graphene doped conductive polymer electrode materials, comprising: adding a conductive polymer monomer into an electroactive graphene aqueous solution, uniformly mixing and then adding an oxidizing agent, and reacting for 6-24 hours under the stirring condition of -10 DEG C-30 DEG C to obtain electroactive graphene doped conductive polymer electrode materials. The method utilizes the oxygen-containing functional group on the surface of electroactive graphene and electroactive molecules grafted on the surface to perform in-situ doping on a conductive polymer. The anthraquinones electroactive molecules grafted on the graphene surface endow grapheme with good redox activity and dispersity, widen a grapheme potential window, and ensure high conductivity and stability of the conductive polymer after being doped to the conductive polymer. The electroactive molecule grafted graphene doped conductive polymer electrode materials have high energy density and circulating stability as super capacitor electrode materials.
Description
Technical field
The present invention relates to the conductive doped polymer electrode material preparation method of a kind of electric active molecule graft grapheme, belong to electrode of super capacitor Material Field.
Background technology
As the novel energy-storing device of a kind of environmental protection, excellent performance, ultracapacitor has that power density is high, the charging interval is short, the advantage such as long service life and environmentally safe, in various fields extensive application such as national defence, military project, electric automobile, computer, mobile communication.But its energy density (general <10Wh/kg) is still lower, limits the application in a large amount of field of storage.Electrode material is the important component part of ultracapacitor, is the key factor affecting ultracapacitor performance and production cost.Electrode material at present for the preparation of ultracapacitor is mainly divided into carbon, metal oxide, conducting polymer three major types.
High surface carbon electrode material is cheap for manufacturing cost, but the energy density obtained is low; Metal oxide containing precious metals can obtain higher energy density, but material cost is high.Conducting polymer, as polyaniline (PANI), polypyrrole (PPy), polythiophene (PTh) and derivative thereof etc., because of the dynamic process of its charge discharge fast (namely adulterate with go doping process rapid), electric charge can store in whole material volume, and cost comparatively metal oxide containing precious metals is low, thus cause the attention of people, but its cyclical stability difference is the bottleneck that restriction conducting polymer further develops at ultracapacitor and applies.
Therefore conducting polymer/graphene combination electrode material becomes study hotspot in recent years, the compound of conducting polymer and Graphene is realized by in-situ chemical or electrochemical polymerization method usually, possesses good Research foundation [Meng YN, Wang K, Zhang YJ, Wei ZX. Hierarchical porous graphene/polyaniline composite film with superior rate performance for flexible supercapacitors. Adv. Mater., 2103, 25:6985-6990.Kumar NA, Choi HJ, Shin YR, Chang DW, Dai LM, Baek JB. Polyanline-grafted reduced graphene oxide for efficient electrochemical supercapacitors. ACS Nano, 2012, 6:1715-1723. Zhao Y, Liu J, Hu Y, Cheng HH, Hu CG, Jiang CC, et al. Highly compression-tolerant supercapacitor based on polypyrrole-mediated graphene foam electrodes. Adv. Mater., 2013, 25:591-595.].But the raising of combination electrode material cyclical stability depends on the consumption of Graphene, too much Graphene add the reunion that membership causes Graphene, be unfavorable for the raising of its energy density.Therefore, the doulbe-sides' victory how existing basis realizing conducting polymer/graphene combination electrode material cyclical stability and energy density still needs further further investigation.
Summary of the invention
In order to overcome the above problems, the object of this invention is to provide the preparation method of the conductive doped polymer electrode material of a kind of electric active molecule graft grapheme, Anthraquinones electric active molecule is grafted on graphenic surface, give the good redox active of Graphene with dispersed, and widen its potential window, improve its energy density.Secondly, by selecting Graphene to be matrix, give the stably-doped property that Anthraquinones electric active molecule is good, preparation has the conducting polymer of stable doped nanometer, improves its cyclical stability.There is not been reported both at home and abroad for this kind of method.
In order to realize above-mentioned goal of the invention, the technical solution used in the present invention is as follows:
A preparation method for the conductive doped polymer electrode material of electric active molecule graft grapheme, its characterization step is as follows:
(1) by soluble in water for Anthraquinones electric active molecule graft grapheme, stir and utilize ultrasonic wave to disperse to form solution; Described Anthraquinones electric active molecule is 1-amino anthraquinones; 1; 4-diamino-anthraquinone; 2; 6-diamino-anthraquinone, 1-amino anthraquinones-5-sulfonate, 1-amino anthraquinones-2-sulfonate; one in 1-amino anthraquinones-2-formates, the concentration of Anthraquinones electric active molecule graft grapheme is 0.01g/L-1g/L;
(2) conducting polymer monomer is added in above-mentioned solution, stir and utilize ultrasonic wave to disperse forming reactions system, the conducting polymer monomer adopted is aniline, m-phenylene diamine (MPD), pyrroles, 3, one in 4-ethylenedioxy thiophene, the mass ratio of Anthraquinones electric active molecule graft grapheme and conducting polymer monomer is: 1:1-1:99.
(3) be dissolved in the water by oxidant and make solution, the disposable reaction system adding step (2) and formed, mixes, and the mol ratio of conducting polymer monomer and oxidant is 1:1-1:8.Described oxidant is ammonium persulfate, potassium peroxydisulfate or anhydrous ferric trichloride;
(4) react 6-24h at stirring condition in-10-30 DEG C, product deionized water cleans repeatedly, and in vacuum drying chamber inner drying, bake out temperature is 60 DEG C, and drying time is 24h, obtains the conductive doped polymer electrode material of electroactive Graphene.
The present invention is directed to the problem that energy density is low and cyclical stability is poor that current electrode material for super capacitor exists, the doping advantage of the electro-chemical activity that combined anthraquinone class electric active molecule graft grapheme is good and conducting polymer uniqueness, the conductive doped polymer composites of electroactive Graphene prepared, can be used as electrode material for super capacitor.
Good effect of the present invention is as follows:
1, utilize the hydrogen bond between the Anthraquinones electric active molecule oxy radical of graphenic surface institute grafting (such as formula (I): 1-amino anthraquinones-5-sodium sulfonate graft grapheme) and conducting polymer monomer and π-π to interact to realize the effect of doping to conducting polymer and induced growth, the Graphene of Anthraquinones electric active molecule grafting can also provide electron channel for conducting polymer while as electric active molecule matrix, can realize the controlled synthesis of the conducting polymer of stable doped nanometer, such design has no bibliographical information both at home and abroad.
formula (I)
The conductive doped polymer of electroactive Graphene of what 2, prepared by the present invention have redox active has higher energy density, and keep good cyclical stability, as electrode material for super capacitor, there is excellent chemical property, be with a wide range of applications.
3, the present invention adopts one-step method to carry out home position polymerization reaction, and equipment is simple, processing ease, easily expands large-scale production.
Embodiment
Below by way of specific embodiment, foregoing of the present invention is described in further detail.But this should be interpreted as content of the present invention is only limitted to following example.
The preparation method of the conductive doped polymer electrode material of embodiment 1 one kinds of electric active molecule graft graphemes, step is as follows:
(1) by 1mg 1-amino anthraquinones graft grapheme, (preparation method is see Wu Q, Sun YQ, Bai H, Shi GQ. High-performance supercapacitor electrodes based on graphene hydrogels modified with 2-aminoanthraquinone moieties. Phys. Chem. Chem. Phys., 2011, 13:11193-11198. disclosed herein is the preparation method of 1-amino anthraquinones graft grapheme, implement 2-6 method not open, but openly method is identical therewith for basic preparation principle, only have the difference of reaction time and temperature) be dissolved in 100mL water, stir and utilize ultrasonic wave to disperse to form Anthraquinones electric active molecule graft grapheme (electroactive Graphene) solution that concentration is 0.01g/L, for subsequent use.
(2) by 99mg(1.0645mmol) aniline (purchased from Chemical Reagent Co., Ltd., Sinopharm Group) adds in above-mentioned dispersion liquid, and stir and utilize ultrasonic wave to disperse forming reactions system (1:99).
(3) by 0.2429g(1.0645mmol) ammonium persulfate (purchased from Chemical Reagent Co., Ltd., Sinopharm Group) is dissolved in the water and makes solution, and the disposable reaction system adding step (2) and formed, mixes.
(4) react 24h at stirring condition in-10 DEG C, product deionized water cleans repeatedly, and in vacuum drying chamber inner drying, bake out temperature is 60 DEG C, and drying time is 24h, obtains the conductive doped polymer electrode material of electroactive Graphene.
The preparation method of the conductive doped polymer electrode material of embodiment 2. 1 kinds of electric active molecule graft graphemes, its place different from embodiment 1 is that 1mg 1-amino anthraquinones graft grapheme becomes 5mg 1,4-diamino-anthraquinone graft grapheme, 99mg(1.0645mmol) aniline becomes 0.35g(5.2239mmol) pyrroles, 0.2429g(1.0645mmol) ammonium persulfate becomes 1.6946g(10.4477mmol) ,-10 DEG C of reaction 24h become stirring condition in 0 DEG C of reaction 18h.
The preparation method of the conductive doped polymer electrode material of embodiment 3. 1 kinds of electric active molecule graft graphemes, its place different from embodiment 1 is that 1mg 1-amino anthraquinones graft grapheme becomes 10mg 2,6-diamino-anthraquinone graft grapheme, 99mg(1.0645mmol) aniline becomes 0.5g(4.6296mmol) m-phenylene diamine (MPD), 0.2429g(1.0645mmol) ammonium persulfate becomes 5.0055g(18.5184mmol) potassium peroxydisulfate ,-10 DEG C of reaction 24h become stirring condition in 10 DEG C of reaction 18h.
The preparation method of the conductive doped polymer electrode material of embodiment 4. 1 kinds of electric active molecule graft graphemes, its place different from embodiment 1 is that 1mg 1-amino anthraquinones graft grapheme becomes 40mg 1-amino anthraquinones-5-sulfonate graft grapheme, 99mg(1.0645mmol) aniline becomes 1.2g(8.44mmol) 3,4-ethylenedioxy thiophene, 0.2429g(1.0645mmol) ammonium persulfate becomes 6.8448g(42.2mmol) anhydrous ferric trichloride, 10 DEG C of reaction 24h become stirring condition in 20 DEG C of reaction 12h.
The preparation method of the conductive doped polymer electrode material of embodiment 5. 1 kinds of electric active molecule graft graphemes, its place different from embodiment 1 is that 1mg 1-amino anthraquinones graft grapheme becomes 70mg 1-amino anthraquinones-2-sulfonate graft grapheme, the quality of aniline is from 99mg(1.0645mmol) become 0.7g(7.5269mmol), the quality of ammonium persulfate is from 0.2429g(1.0645mmol) become 12.0235g(52.6883mmol) ,-10 DEG C of reaction 24h become stirring condition in 25 DEG C of reaction 8 h.
The preparation method of the conductive doped polymer electrode material of embodiment 6. 1 kinds of electric active molecule graft graphemes, its place different from embodiment 1 is that 1mg 1-amino anthraquinones graft grapheme becomes 100mg 1-amino anthraquinones-2-formates graft grapheme, the quality of aniline is from 99mg(1.0645mmol) become 0.1g(1.0753mmol), the quality of ammonium persulfate is from 0.2429g(1.0645mmol) become 1.9630g(8.6021mmol) ,-10 DEG C of reaction 24h become stirring condition in 30 DEG C of reaction 6h.
Embodiment 1-6 prepares shown in the performance parameter chart 1 of composite material, and in table 1, reference examples is the conductive polymer electrodes material property parameter of electric active molecule graft grapheme of not adulterating:
Table 1
Claims (8)
1. a preparation method for the conductive doped polymer electrode material of electric active molecule graft grapheme, is characterized in that step is as follows:
By soluble in water for the Graphene of electric active molecule grafting, stir and utilize ultrasonic wave to disperse to form solution, for subsequent use;
Conducting polymer monomer is added in above-mentioned solution, stirs and utilize ultrasonic wave to disperse forming reactions system, for subsequent use;
Be dissolved in the water by oxidant and make solution, the disposable reaction system adding step (2) and formed, mixes;
(4) react 6-24h at stirring condition in-10-30 DEG C, product deionized water cleans repeatedly, and in vacuum drying chamber inner drying, obtains the conductive doped polymer electrode material of electroactive Graphene.
2. the preparation method of the conductive doped polymer electrode material of electric active molecule graft grapheme according to claim 1, it is characterized in that described electric active molecule is 1-amino anthraquinones, 1,4-diamino-anthraquinone, 2,6-diamino-anthraquinone, 1-amino anthraquinones-5-sulfonate, 1-amino anthraquinones-2-sulfonate, the one in 1-amino anthraquinones-2-formates.
3. the preparation method of the conductive doped polymer electrode material of electric active molecule graft grapheme according to claim 1, it is characterized in that the conducting polymer monomer adopted in step (2) is the one in aniline, m-phenylene diamine (MPD), pyrroles, 3,4-ethylene dioxythiophene.
4. the preparation method of the conductive doped polymer electrode material of electric active molecule graft grapheme according to claim 1, is characterized in that the oxidant adopted in step (3) is the one of ammonium persulfate, potassium peroxydisulfate, anhydrous ferric trichloride.
5. the preparation method of the conductive doped polymer electrode material of electric active molecule graft grapheme according to claim 1, is characterized in that the concentration of electric active molecule graft grapheme solution in step (1) is 0.01-1g/L.
6. the preparation method of the conductive doped polymer electrode material of electric active molecule graft grapheme according to claim 1, is characterized in that the mass ratio of electric active molecule graft grapheme and conducting polymer monomer in step (2) is 1:1-1:99.
7. the preparation method of the conductive doped polymer electrode material of electric active molecule graft grapheme according to claim 1, is characterized in that the mol ratio of conducting polymer monomer and initator in step (3) is 1:1-1:8.
8. the preparation method of the conductive doped polymer electrode material of electric active molecule graft grapheme according to claim 1, it is characterized in that the bake out temperature of step (4) is 60 DEG C, drying time is 24h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105244189A (en) * | 2015-10-21 | 2016-01-13 | 山东科技大学 | Preparation method of carbon nano tube reinforced conducting polymer hydrogel |
| CN105388200A (en) * | 2015-10-16 | 2016-03-09 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing sensor used for organic phosphorus pesticide detection |
| CN105551820A (en) * | 2016-03-01 | 2016-05-04 | 聊城大学 | Supercapacitor electrode material and preparation method thereof |
| CN106504910A (en) * | 2016-10-25 | 2017-03-15 | 河海大学 | A kind of anthraquinone molecular cograft carbon/conducting polymer composite material and preparation method thereof |
| CN108428556A (en) * | 2018-03-19 | 2018-08-21 | 华南理工大学 | A kind of graphene/metal anthraquinone complex/carbon/polyaniline super capacitor electrode material and preparation method thereof |
| CN109489540A (en) * | 2018-10-22 | 2019-03-19 | 西南石油大学 | A method of conductive fiber strain sensing performance is improved using non-covalent bond is modified |
| EP3514223A1 (en) * | 2018-01-17 | 2019-07-24 | Eppendorf AG | Multisensor for a bioreactor, bioreactor, method for producing a multi-sensor and for measuring parameters |
| CN110246703A (en) * | 2019-05-21 | 2019-09-17 | 浙江工业大学 | Functional graphene oxide/poly- (3,4- ethene dioxythiophene) composite material and preparation method |
| CN112186173A (en) * | 2020-09-21 | 2021-01-05 | 湖南艾华集团股份有限公司 | Negative electrode with high rate performance, preparation method and lithium ion battery |
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| CN105388200B (en) * | 2015-10-16 | 2018-02-09 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of transducer production method for detection of organic phosphorus pesticide |
| CN105244189A (en) * | 2015-10-21 | 2016-01-13 | 山东科技大学 | Preparation method of carbon nano tube reinforced conducting polymer hydrogel |
| CN105551820B (en) * | 2016-03-01 | 2018-04-10 | 聊城大学 | A kind of electrode material for super capacitor and preparation method thereof |
| CN105551820A (en) * | 2016-03-01 | 2016-05-04 | 聊城大学 | Supercapacitor electrode material and preparation method thereof |
| CN106504910A (en) * | 2016-10-25 | 2017-03-15 | 河海大学 | A kind of anthraquinone molecular cograft carbon/conducting polymer composite material and preparation method thereof |
| CN106504910B (en) * | 2016-10-25 | 2018-03-09 | 河海大学 | A kind of anthraquinone molecular cograft carbon/conducting polymer composite material and preparation method thereof |
| EP3514223A1 (en) * | 2018-01-17 | 2019-07-24 | Eppendorf AG | Multisensor for a bioreactor, bioreactor, method for producing a multi-sensor and for measuring parameters |
| WO2019141466A1 (en) * | 2018-01-17 | 2019-07-25 | Eppendorf Ag | Mutli sensor for a bioreactor, bioreactor, method for producing a multi sensor, and for measuring parameters |
| CN108428556A (en) * | 2018-03-19 | 2018-08-21 | 华南理工大学 | A kind of graphene/metal anthraquinone complex/carbon/polyaniline super capacitor electrode material and preparation method thereof |
| CN109489540A (en) * | 2018-10-22 | 2019-03-19 | 西南石油大学 | A method of conductive fiber strain sensing performance is improved using non-covalent bond is modified |
| CN110246703A (en) * | 2019-05-21 | 2019-09-17 | 浙江工业大学 | Functional graphene oxide/poly- (3,4- ethene dioxythiophene) composite material and preparation method |
| CN110246703B (en) * | 2019-05-21 | 2021-05-11 | 浙江工业大学 | Functionalized graphene oxide/poly (3, 4-ethylenedioxythiophene) composite material and preparation method thereof |
| CN112186173A (en) * | 2020-09-21 | 2021-01-05 | 湖南艾华集团股份有限公司 | Negative electrode with high rate performance, preparation method and lithium ion battery |
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Application publication date: 20150923 |