CN103560017A - Polypyrrole / graphite felt composite electrode and preparation method thereof - Google Patents
Polypyrrole / graphite felt composite electrode and preparation method thereof Download PDFInfo
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- CN103560017A CN103560017A CN201310527300.0A CN201310527300A CN103560017A CN 103560017 A CN103560017 A CN 103560017A CN 201310527300 A CN201310527300 A CN 201310527300A CN 103560017 A CN103560017 A CN 103560017A
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Abstract
The invention discloses a polypyrrole / graphite felt composite electrode and a preparation method thereof, oxidation pretreatment is conducted on a graphite felt, and the graphite felt is used as a working electrode, a platinum filament is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, a mixing solution of one or more of pyrrole and benzenesulfonic acid, benzene sulfonate or derivatives of the benzene sulfonate is used as an electrolyte, and the polypyrrole / graphite felt composite electrode is prepared through an electrochemistry cyclic voltammetry oxidative polymerization reaction. The polypyrrole / graphite felt composite electrode not only has high energy storage density, but also has good cyclic stability, is simple in preparation technology, and has significant economical and social benefits.
Description
Technical field
The invention belongs to the preparation field of electrode for super capacitor, be specifically related to a kind of polypyrrole/graphite felt combination electrode and preparation method thereof.
Background technology
Polypyrrole, as a kind of important conducting polymer, the current era being taken seriously all the more at renewable resource has huge practical value with advantages such as its good electrochemical reversibility and high environmental stabilities in electrochemical energy storing device.Gardini G P(Gardini G P. Advances in Heterocyclic Chemistry in 1973,1973,15:67-69) synthesized the electric polypyrrole of black powder form.Subsequently, Diaz A F(Diaz A F, Juan I, Castillo J A. Journal of Electroanalytical Chemistry and Interfacial Electrochemistry, 1981, 129:115-132), Yuying G(Yuying G, Lu Z, Hua B, Qi C, Gaoquan S. Journal of Electroanalytical Chemistry, 2006, 597:13-18) with Hyuck L(Hyuck L, Hyeongkeun K, Mi S C, Jaeboong C, Youngkan L. Electrochimica Acta, 2011, 56:7460-7466), Kaiyuan S(Kaiyuan S, Lgor Z. Journal of Power Sources, 2013, the polypyrrole material of 240:42-49) etc. preparing different structure.Research discovery, electric polypyrrole, except having excellent chemical property, also has the advantages such as easily synthetic and environmental friendliness, aspect electrochemical capacitor, is with a wide range of applications.
At present, Platinum material generally can obtain by electrochemical oxidation and chemical oxidization method polymerization.Method is easy, and the polypyrrole material conductivity of preparing is high fast, and electrochemistry capacitance is large.Wang Jie (Wang Jie, Xu Youlong, Chen Xi, Du Xianfeng, Li Xifei.Acta PhySico-Chimica Sinica, 2007,23 (3): 299-304) by electrochemical process, prepare the polypyrrole film of different ions doping, find that PPy-Cl film has good charging and discharging capabilities, when the degree of depth discharges and recharges, still having very little electrochemistry resistance, is 5mVs in sweep speed
-1lower than electric capacity up to 270Fg
-1.Yueping F(Yueping F, Jianwei L, Deok J Y, James P W, Kaan K, Cozge T, Bret N F, Judy W, Jun L. Journal of Power Sources, 2010,195:674-679) method by pulse electrodeposition is coated on polypyrrole on MCNTs electrode, the MWCNT-PPy film that obtains self-supporting, reaches 427Fg than electric capacity
-1.Zhang Aiqin (Zhang Aiqin, Wang Lizhen, Zhang Yong, Shen magic weapon.Battery, 2010,40 (1): 10-12) at low temperatures chemical syntheses doped hydrochloride polypyrrole, in current density, be 8mA/cm
2time, the single electrode of polypyrrole in 1mol/L metabisulfite solution reaches 350.2Fg than electric capacity
-1; When current density is 10mA/cm
2time, the ratio electric capacity of the 100th circulation time is initial value 90.6%.Dubal D P(Dubal D P, Patil S V, Jagadale A D, Lokhande C D. Journal of Alloys and Compounds, 2011,509:8183-8188) starting out the Platinum material that simple two step chemical methods are prepared three-dimensional ball binding structure, is 5mVs in sweep speed
-1lower high specific electric capacity is 533Fg
-1.
At present, polypyrrole, high specific capacitance simple and easy to get with it, high-energy-density are applied on electrode material for super capacitor.But its cycle life is low, affected greatly its practical application, still need further strengthening research.
Summary of the invention
The object of the present invention is to provide a kind of polypyrrole/graphite felt combination electrode and preparation method thereof, this combination electrode not only has higher energy storage density, and has excellent cyclical stability; Preparation technology is simple, possesses significant economic and social benefit.
For achieving the above object, the present invention adopts following technical scheme:
/ graphite felt combination electrode is usingd oxidation pre-treatment graphite felt as a carrier, usings substituted benzenesulfonic acid radical ion Doped polypyrrole as electrode operation material.
Preparation method comprises the following steps:
(1) pyrroles is mixed with one or more in benzene sulfonic acid, benzene sulfonate or derivatives thereof, make mixed solution;
(2) using pre-oxidation treatment graphite felt as work electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, and the mixed solution of step (1) preparation, as electrolyte, utilizes electrochemistry cyclic voltammetric oxidative polymerization to prepare polypyrrole/graphite felt combination electrode.
Described benzene sulfonic acid, benzene sulfonate or derivatives thereof comprise: benzene sulfonic acid, benzene sulfonate, p-methyl benzenesulfonic acid, toluenesulfonate, to 120,000 oxygen base benzene sulfonic acids, to 120,000 oxygen base benzene sulfonates, aminobenzenesulfonic acid, amino phenyl sulfonyl hydrochlorate, nitrobenzene-sulfonic acid, nitrobenzene-sulfonic acid salt.
Concrete steps are as follows:
(1) one or more in benzene sulfonic acid, benzene sulfonate or derivatives thereof are dissolved in the deionized water of 100mL, making benzene sulfonic acid radical ion concentration is the solution of 0.05 ~ 0.3 mol/L, add pyrroles, the mol ratio that makes pyrroles and benzene sulfonic acid radical ion is 2 ~ 0.5:1, ultrasonic 10 ~ 40 min, obtain mixed solution;
(2) adopt three-electrode system, with oxidation pre-treatment graphite felt, (mulberry business is refined for Li Xiaogang, Huang Kelong, Tan Ning, Liu Suqin, Chen Liquan, Catalysis of graphite felt electrode treated with electrochemical oxidation VO
2+/ VO
2 +the catalytic activity functional material that electricity is right, 2006, 37(7): 1084-1086) as work electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the mixed solution that step (1) makes is as electrolyte, utilize electrochemistry cyclic voltammetric oxidative polymerization, voltage scan range 0.0V ~ 1.5V, sweep speed 10 ~ 100mV/s, scan round 20 ~ 60 circles, take out work electrode, with ethanol and deionized water, repeatedly rinse, vacuumize obtains usining oxidation pre-treatment graphite felt as carrier, using the combination electrode of substituted benzenesulfonic acid radical ion Doped polypyrrole as electrode operation material, be high energy storage density polypyrrole/graphite felt combination electrode.
Remarkable advantage of the present invention is: high energy storage density polypyrrole/graphite felt combination electrode prepared by the present invention is mainly applicable to prepare ultracapacitor.Preparation method of the present invention is simple, prepared high energy storage density polypyrrole/graphite felt combination electrode is when charging and discharging currents density is respectively 1g/A, 2g/A, 4g/A and 10g/A, than electric capacity respectively up to 658F/g, 577F/g, 520F/g and 472F/g, discharge and recharge after 1000 times, than capacitance fade, be less than 1%.
Embodiment
Embodiment 1
(1) preparation of pyrroles and the p-methyl benzenesulfonic acid aqueous solution: take 0.01 mol p-methyl benzenesulfonic acid, be dissolved in the deionized water of 100 mL, prepare the p-methyl benzenesulfonic acid aqueous solution of 0.1 mol/L; The pyrroles that to take with p-methyl benzenesulfonic acid radical ion mol ratio be 1.5:1 is as in the above-mentioned aqueous solution, and ultrasonic 30 min obtain the aqueous solution of pyrroles and p-methyl benzenesulfonic acid.
(2) preparation of polypyrrole/graphite felt combination electrode: adopt three-electrode system, using oxidation pre-treatment graphite felt as work electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the aqueous solution that step (1) makes is as electrolyte, utilize electrochemistry cyclic voltammetric oxidative polymerization, voltage scan range 0.0V ~ 1.5V, sweep speed 50mV/s, scan round 40 circles, take out work electrode, with ethanol and deionized water, repeatedly rinse, vacuumize obtains usining oxidation pre-treatment graphite felt as carrier, using the combination electrode of p-methyl benzenesulfonic acid radical ion Doped polypyrrole as electrode operation material, be described high energy storage density polypyrrole/graphite felt combination electrode.
Polypyrrole/graphite felt combination electrode prepared by said method is being usingd 0.5 mol/L aqueous sulfuric acid as electrolyte, record this combination electrode when charging and discharging currents density is respectively 1g/A, 2g/A, 4g/A and 10g/A, than electric capacity respectively up to 658F/g, 577F/g, 520F/g and 472F/g, discharge and recharge after 1000 times, than capacitance fade to 99.14% of initial value.
Embodiment 2
(1) preparation of pyrroles and p-methyl benzenesulfonic acid sodium water solution: take 0.01 mol paratoluenesulfonic acid sodium salt, be dissolved in the deionized water of 100 mL, prepare the p-methyl benzenesulfonic acid sodium water solution of 0.1 mol/L; The pyrroles that to take with p-methyl benzenesulfonic acid radical ion mol ratio be 1.5:1 is as in the above-mentioned aqueous solution, and ultrasonic 30 min obtain the aqueous solution of pyrroles and paratoluenesulfonic acid sodium salt.
(2) preparation of polypyrrole/graphite felt combination electrode: adopt three-electrode system, using oxidation pre-treatment graphite felt as work electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the aqueous solution that step (1) makes is as electrolyte, utilize electrochemistry cyclic voltammetric oxidative polymerization, voltage scan range 0.0V ~ 1.5V, sweep speed 50mV/s, scan round 40 circles, take out work electrode, with ethanol and deionized water, repeatedly rinse, vacuumize obtains usining oxidation pre-treatment graphite felt as carrier, using the combination electrode of p-methyl benzenesulfonic acid radical ion Doped polypyrrole as electrode operation material, be described high energy storage density polypyrrole/graphite felt combination electrode.
Polypyrrole/graphite felt combination electrode prepared by said method is being usingd 0.5 mol/L aqueous sulfuric acid as electrolyte, record this combination electrode when charging and discharging currents density is respectively 1g/A, 2g/A, 4g/A and 10g/A, than electric capacity respectively up to 461F/g, 415F/g, 392F/g and 368F/g, discharge and recharge after 1000 times, than capacitance fade to 99.27% of initial value.
Embodiment 3
(1) preparation of pyrroles and p-methyl benzenesulfonic acid and paratoluenesulfonic acid sodium salt mixture aqueous solution: take 0.005 mol p-methyl benzenesulfonic acid and 0.005 mol paratoluenesulfonic acid sodium salt, be dissolved in the deionized water of 100 mL, preparing p-methyl benzenesulfonic acid radical ion concentration is the aqueous solution of 0.1 mol/L; The pyrroles that to take with p-methyl benzenesulfonic acid radical ion mol ratio be 1.5:1 is as in the above-mentioned aqueous solution, and ultrasonic 30 min obtain the aqueous solution of pyrroles and p-methyl benzenesulfonic acid and paratoluenesulfonic acid sodium salt mixture.
(2) preparation of polypyrrole/graphite felt combination electrode: adopt three-electrode system, using oxidation pre-treatment graphite felt as work electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the aqueous solution that step (1) makes is as electrolyte, utilize electrochemistry cyclic voltammetric oxidative polymerization, voltage scan range 0.0V ~ 1.5V, sweep speed 50mV/s, scan round 40 circles, take out work electrode, with ethanol and deionized water, repeatedly rinse, vacuumize obtains usining oxidation pre-treatment graphite felt as carrier, using the combination electrode of p-methyl benzenesulfonic acid radical ion Doped polypyrrole as electrode operation material, be described high energy storage density polypyrrole/graphite felt combination electrode.
Polypyrrole/graphite felt combination electrode prepared by said method is being usingd 0.5 mol/L aqueous sulfuric acid as electrolyte, record this combination electrode when charging and discharging currents density is respectively 1g/A, 2g/A, 4g/A and 10g/A, than electric capacity respectively up to 624F/g, 559F/g, 515F/g and 466F/g, discharge and recharge after 1000 times, than capacitance fade to 99.18% of initial value.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. polypyrrole/graphite felt combination electrode, is characterized in that: using oxidation pre-treatment graphite felt as carrier, using substituted benzenesulfonic acid radical ion Doped polypyrrole as electrode operation material.
2. a method of preparing polypyrrole/graphite felt combination electrode as claimed in claim 1, is characterized in that: comprise the following steps:
(1) pyrroles is mixed with one or more in benzene sulfonic acid, benzene sulfonate or derivatives thereof, make mixed solution;
(2) using pre-oxidation treatment graphite felt as work electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, and the mixed solution of step (1) preparation, as electrolyte, utilizes electrochemistry cyclic voltammetric oxidative polymerization to prepare polypyrrole/graphite felt combination electrode.
3. the preparation method of polypyrrole/graphite felt combination electrode according to claim 2, is characterized in that: described benzene sulfonic acid, benzene sulfonate or derivatives thereof comprise: benzene sulfonic acid, benzene sulfonate, p-methyl benzenesulfonic acid, toluenesulfonate, to 120,000 oxygen base benzene sulfonic acids, to 120,000 oxygen base benzene sulfonates, aminobenzenesulfonic acid, amino phenyl sulfonyl hydrochlorate, nitrobenzene-sulfonic acid, nitrobenzene-sulfonic acid salt.
4. the preparation method of polypyrrole/graphite felt combination electrode according to claim 2, is characterized in that: concrete steps are as follows:
(1) one or more in benzene sulfonic acid, benzene sulfonate or derivatives thereof are dissolved in the deionized water of 100mL, making benzene sulfonic acid radical ion concentration is the solution of 0.05 ~ 0.3 mol/L, add pyrroles, the mol ratio that makes pyrroles and benzene sulfonic acid radical ion is 2 ~ 0.5:1, ultrasonic 10 ~ 40 min, obtain mixed solution;
(2) adopt three-electrode system, using oxidation pre-treatment graphite felt as work electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the mixed solution that step (1) makes is as electrolyte, utilize electrochemistry cyclic voltammetric oxidative polymerization, voltage scan range 0.0V ~ 1.5V, sweep speed 10 ~ 100mV/s, scan round 20 ~ 60 circles, take out work electrode, with ethanol and deionized water, repeatedly rinse, vacuumize obtains usining oxidation pre-treatment graphite felt as carrier, using the combination electrode of substituted benzenesulfonic acid radical ion Doped polypyrrole as electrode operation material, be high energy storage density polypyrrole/graphite felt combination electrode.
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Cited By (8)
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| CN104237350A (en) * | 2014-10-09 | 2014-12-24 | 无锡百灵传感技术有限公司 | Electrochemical sensor based on magnetic nano-particle modified electrodes |
| CN106206059A (en) * | 2016-09-22 | 2016-12-07 | 福州大学 | NiCo2s4the preparation method and application of/graphite felt combination electrode material |
| CN106356203A (en) * | 2016-10-31 | 2017-01-25 | 福州大学 | Nickel cobaltate nano-sheet/graphite felt composite material and preparation and application thereof |
| CN106486296A (en) * | 2016-11-22 | 2017-03-08 | 福州大学 | A kind of preparation method of nitrogen/nickel cobalt codope graphite felt electrode material |
| CN108550469A (en) * | 2018-04-20 | 2018-09-18 | 南京邮电大学 | A kind of preparation method and application of metalloporphyrin frame/polypyrrole composite and flexible electrode |
| WO2019073487A1 (en) * | 2017-10-12 | 2019-04-18 | Amara Raja Batteries Limited | An electrode for lead acid battery assembly and its method of preparation |
| CN111115769A (en) * | 2019-12-27 | 2020-05-08 | 自然资源部天津海水淡化与综合利用研究所 | One-step electrosynthesis graphene composite electrode by using electrochemical method and method |
| CN112201486A (en) * | 2020-10-13 | 2021-01-08 | 福州大学 | Preparation method of poly (3, 4-ethylenedioxythiophene)/graphite felt flexible electrode material |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104237350A (en) * | 2014-10-09 | 2014-12-24 | 无锡百灵传感技术有限公司 | Electrochemical sensor based on magnetic nano-particle modified electrodes |
| CN104237350B (en) * | 2014-10-09 | 2016-08-24 | 无锡百灵传感技术有限公司 | A kind of electrochemical sensor based on magnetic nano-particle modified electrode |
| CN106206059A (en) * | 2016-09-22 | 2016-12-07 | 福州大学 | NiCo2s4the preparation method and application of/graphite felt combination electrode material |
| CN106206059B (en) * | 2016-09-22 | 2018-07-20 | 福州大学 | NiCo2S4The preparation method and application of/graphite felt combination electrode material |
| CN106356203A (en) * | 2016-10-31 | 2017-01-25 | 福州大学 | Nickel cobaltate nano-sheet/graphite felt composite material and preparation and application thereof |
| CN106356203B (en) * | 2016-10-31 | 2019-02-22 | 福州大学 | A kind of cobalt acid nickel nano film/graphite felt composite material and its preparation and application |
| CN106486296A (en) * | 2016-11-22 | 2017-03-08 | 福州大学 | A kind of preparation method of nitrogen/nickel cobalt codope graphite felt electrode material |
| WO2019073487A1 (en) * | 2017-10-12 | 2019-04-18 | Amara Raja Batteries Limited | An electrode for lead acid battery assembly and its method of preparation |
| CN108550469A (en) * | 2018-04-20 | 2018-09-18 | 南京邮电大学 | A kind of preparation method and application of metalloporphyrin frame/polypyrrole composite and flexible electrode |
| CN111115769A (en) * | 2019-12-27 | 2020-05-08 | 自然资源部天津海水淡化与综合利用研究所 | One-step electrosynthesis graphene composite electrode by using electrochemical method and method |
| CN111115769B (en) * | 2019-12-27 | 2022-06-10 | 自然资源部天津海水淡化与综合利用研究所 | One-step electrosynthesis graphene composite electrode by using electrochemical method and method |
| CN112201486A (en) * | 2020-10-13 | 2021-01-08 | 福州大学 | Preparation method of poly (3, 4-ethylenedioxythiophene)/graphite felt flexible electrode material |
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