CN103390511A - Preparation method for graphene oxide/polypyrrole composite material of lamellar microstructure - Google Patents
Preparation method for graphene oxide/polypyrrole composite material of lamellar microstructure Download PDFInfo
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Abstract
The invention provides a preparation method for graphene oxide/polypyrrole composite material of a lamellar microstructure. The preparation method comprises the following steps: adding organic sulfoacid into graphene oxide dilute solution, stirring the solution, separating and mixing the solution through ultrasonic wave, adding pyrrole monomer, stirring uniformly and adding oxidizing agent, and reacting for 12 to 24 hours under ice bath condition, so as to obtain the graphene oxide/polypyrrole composite material of the lamellar microstructure. According to the method provided by the invention, the graphene oxide/polypyrrole composite material of the lamellar microstructure is prepared through the induction of the electronegativity functional group on the graphene oxide surface, and the lamellar microstructure is suitable for improving ion/electron transfer capability of composite materials, and further improving specific capacity of the composite materials. The prepared composite material can obtain higher conductivity and specific capacitance, and is suitable for serving as super capacitor electrode materials.
Description
Technical field
The present invention relates to conducting polymer composite material, specifically, be to utilize the stannic oxide/graphene nano sheet to induce the graphene oxide/Pt/Polypyrrole composite material for preparing the lamella micro-structural by the method for in-situ polymerization, this composite material can be applicable to electrode material for super capacitor.
Background technology
Along with technological progress and the industry development of new energy field, energy storage technology more and more is subject to each side and payes attention to, and becomes the key link that solves the Future New Energy Source industry development.Ultracapacitor is a kind of novel energy-storing device between battery and traditional capacitor, has both advantages concurrently, has that power density is high, energy density is high, the charging interval is short, an advantage such as long service life and environmentally safe.As the novel energy-storing device of a kind of environmental protection, excellent performance, ultracapacitor is in various fields extensive application such as national defence, military project, electric automobile, computer, mobile communication.
Has the ideal electrode material that is considered to ultracapacitor than the conducting polymer of bigger serface, the conducting polymer that is applicable to this type of capacitor has: polypyrrole, polyaniline, polythiophene and derivative thereof, wherein, the conductivity of polypyrrole Yin Qigao, interesting redox property, environmental stability and can become in recent years study hotspot by advantages such as chemistry or electrochemical method are easy to prepare.Graphite oxide be a kind of can delamination be the two-dimensional layer material of graphene oxide in height polar solvent medium (for example water) under the effect of mechanical energy.Anchor is at mono-layer graphite oxide alkene sheet surface sp
3Great amount of hydroxy group on the hydridization carbon atom and epoxide group and be positioned at graphene oxide sheet edge sp
2Carboxyl and carbonyl functional groups a large amount of on the hydridization carbon atom make graphene oxide be easy to be scattered in water.Simultaneously, these oxygen-containing functional groups make graphene oxide sheet produce strong the interaction and to form oxidized graphite composite material with little polar molecule or polymer.
at present, the research of graphene oxide/Pt/Polypyrrole composite material mainly concentrates on raising [the Zhang LL of conductivity of composite material energy, Zhao S, Tian XN, Zhao XS.Layered graphene oxide nanostructures with sandwiched conducting polymers as supercapacitor electrodes.Langmuir, 2010, 26 (22): 17624-17628.Han YQ, Lu Y.Preparation and characterization of graphite oxide/polypyrrole composites.Carbon, 2007, 45:2394-2399.Han YQ, LuY.Characterization and electrical properties of conductive polymer/colloidal graphite oxide nanocomposites.Composite.Sci.Technol., 2009, 69:1231-1237.], the report that seldom relevant for this composite material, than electric capacity, improves.Our previous research work shows that rate of charge has certain influence [Han YQ to the chemical property of graphene oxide/Pt/Polypyrrole composite material, Ding B, Zhang XG.Effect of feeding ratios on the structure and electrochemical performance of graphite oxide/polypyrrole nanocomposites.Chinese Sci.Bulletin, 2011,56:2846.], but the ratio electric capacity of graphene oxide/Pt/Polypyrrole composite material still remains to be improved.
Summary of the invention
The invention provides a kind of preparation method of graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural, the electronegativity functional group that utilizes the graphene oxide surface induces the graphene oxide for preparing the lamella micro-structural/polypyrrole nano composite material by in-situ polymerization, the composite material that is prepared by this method has the microstructure of sheet and higher conductivity, and this kind method there is not yet report both at home and abroad.Preparation method of the present invention is simple, prepared composite material have when the electrode material for super capacitor higher conductivity with than electric capacity.
Technical scheme of the present invention is as follows:
A kind of preparation method of graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural, step is as follows:
(1) organic sulfonic acid is added in graphene oxide solution, stirs and utilize ultrasonic wave to disperse to make its mixing, after continuing to stir under condition of ice bath, standby, the concentration of graphene oxide solution is 0.1-0.5mg/mL, better scope is 0.2-0.4mg/mL.Organic acid is any in 1,5-naphthalenedisulfonic acid, sulfanilic acid, α-naphthalenesulfonicacid, beta-naphthalenesulfonic-acid, and the temperature of ice bath is controlled at 0-5 ℃;
(2) pyrrole monomer is injected in the mixture of step (1), stirs and form reaction system, standby.Graphene oxide and pyrroles's mass ratio is 1:10-1:30, and organic sulfonic acid and pyrroles's mol ratio is 1:4-1:1; The pyrroles is before use through heavily steaming;
(3) oxidant is dissolved in the water and makes solution, the reaction system that adds fast step (2) to form, mix, under condition of ice bath after stirring reaction 12-24h, the product that obtains is cleaned repeatedly with deionized water, and, in the vacuum drying chamber inner drying, obtain the graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural.Bake out temperature is 60 ℃, and drying time is 24h; Oxidant is any in ammonium persulfate, potassium peroxydisulfate, anhydrous ferric trichloride, Fe(NO3)39H2O, and the mol ratio of pyrroles and oxidant is 1:1-1:2.
The invention has the advantages that:
1, adopt the electronegativity functional group on graphene oxide surface to induce the graphene oxide/Pt/Polypyrrole composite material for preparing the lamella micro-structural to there is not yet report in document at home and abroad.
2, adopt one-step method to carry out home position polymerization reaction, equipment is simple, processing ease, easily enlarges large-scale production.
3, the prepared graphene oxide/Pt/Polypyrrole composite material of the present invention has excellent chemical property as electrode material for super capacitor, is with a wide range of applications.
Description of drawings
Fig. 1 is the SEM photo that the embodiment of the present invention 1 prepares graphene oxide and graphene oxide/Pt/Polypyrrole composite material, left figure amplifies the graphene oxide SEM photo of 8000 times, right figure is the SEM photo that amplifies the graphene oxide/Pt/Polypyrrole composite material of 25000 times, adopt JSM-5610 type ESEM (Japanese JEOL company) to test, sample is gold,platinized before test.By the SEM image as seen, graphene oxide presents the lamella micro-structural of accordion.In contrast thereto, induce the graphene oxide/Pt/Polypyrrole composite material for preparing to demonstrate the overlapping structure of sub-micron stratiform by graphene oxide, lamella size 200-300nm.
Fig. 2 .. be the embodiment of the present invention 1 preparation graphene oxide (curve a) with the cyclic voltammetry curve (electrolyte: 1M H of graphene oxide/Pt/Polypyrrole composite material (curve b)
2SO
4, sweep speed=10mV/s).As seen from Figure 2, the CV curve shape of the graphene oxide/Pt/Polypyrrole composite material of embodiment 1 preparation is compared with graphene oxide more near rectangle, shows desirable electrochemical capacitance characteristic.Compare with graphene oxide, composite material CV area under the curve and cyclic voltammetric response current are more much bigger than graphene oxide, and this shows the more much larger than capacity ratio graphene oxide of composite material
Fig. 3 .. be the embodiment of the present invention 1 preparation graphene oxide (curve a) with the charging and discharging curve (electrolyte: 1M H of graphene oxide/polypyrrole conducing composite material (curve b)
2SO
4, current density=1A/g).As can be seen from Figure 3, embodiment 1 prepare the ratio electric capacity of graphene oxide and composite material can basis:
Calculate, wherein C
mFor than electric capacity, I is discharging current, and △ t is discharge time, and m is the quality of active material, and △ V is the voltage drop in discharge process, and the ratio electric capacity that calculates the graphene oxide of embodiment 1 preparation is 9F/g, and the ratio electric capacity of composite material can reach 319F/g.
Embodiment
Below by specific embodiment, foregoing of the present invention is described in further detail.But this should be interpreted as that content of the present invention only limits to following example.
Embodiment 1
A kind of preparation method of graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural comprises the following steps:
(1) with 1,5-naphthalenedisulfonic acid (134.5mg, 0.3731mmol, available from Chemical Reagent Co., Ltd., Sinopharm Group) (preparation method is referring to Hummers W S, Offeman R E.Preparation of graphite oxide.J Am Chem Soc, 1958 to add the graphene oxide of 100mL0.1mg/mL, in weak solution 80:1339), stir and utilize ultrasonic wave to disperse to make it to mix after continue to stir in ice bath after, standby
(2) 100mg pyrrole monomer (1.4925mmol, available from German Aldrich) is injected in said mixture, stirs and form reaction system, standby.(concentration ratio of graphene oxide and pyrrole monomer is 1:10).
(3) with 340.6mg(1.4925mmol) ammonium persulfate (available from Chemical Reagent Co., Ltd., Sinopharm Group) is dissolved in 5mL water and makes solution, and the reaction system that adds fast step (2) to form, mix.
(4) under stirring condition under 0-5 ℃ the reaction 12h after, the product that obtains is cleaned repeatedly with deionized water, and, in the vacuum drying chamber inner drying, obtains the graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural.Bake out temperature is 60 ℃, and drying time is 24h.
Embodiment 2
Embodiment 2 difference from Example 1 are 1 in step (1), 5-naphthalenedisulfonic acid (134.5mg, 0.3731mmol) become sulfanilic acid (381mg, 2.2388mmol), 0.1mg/mL graphene oxide become the graphene oxide of 0.2mg/mL, 100mg pyrrole monomer (1.4925mmol) in step (2) becomes 300mg pyrrole monomer (4.4776mmol), the 340.6mg(1.4925mmol in step (3)) ammonium persulfate becomes 1.21g(4.4776mmol) potassium peroxydisulfate.
Embodiment 3
Embodiment 3 difference from Example 1 are step (1) 1,5-naphthalenedisulfonic acid (134.5mg, 0.3731mmol) become α-naphthalenesulfonicacid (1.8651g, 8.9552mmol), 0.1mg/mL graphene oxide become the graphene oxide of 0.3mg/mL, 100mg pyrrole monomer (1.4925mmol) in step (2) becomes 600mg pyrrole monomer (8.9552mmol), 340.6mg(1.4925mmol in step (3)) ammonium persulfate becomes 2.905g(17.9104mmol) anhydrous ferric trichloride, the reaction 12h in step (4) becomes 18h.
Embodiment 4
embodiment 4 difference from Example 1 are 1 in step (1), 5-naphthalenedisulfonic acid (134.5mg, 0.3731mmol) become beta-naphthalenesulfonic-acid (2.091g, 7.4627mmol), 100mL0.1mg/mL graphene oxide become the graphene oxide of 50mL0.4mg/mL, in step (2), 100mg pyrrole monomer (1.4925mmol) becomes 500mg pyrrole monomer (7.4627mmol), in step (3) with 340.6mg(1.4925mmol) ammonium persulfate becomes 6.0298g(14.9254mmol) anhydrous ferric trichloride, reaction 12h in step (4) becomes 18h.
Embodiment 5
embodiment 5 difference from Example 1 are the 5-naphthalenedisulfonic acid (134.5mg in step (1), 0.3731mmol) become 1, 5-naphthalenedisulfonic acid (8.0677g, 2.2388mmol), 100mL0.1mg/mL graphene oxide become the graphene oxide of 40mL0.5mg/mL, 100mg pyrrole monomer (1.4925mmol) in step (2) becomes 600mg pyrrole monomer (8.9552mmol), in step (3) with 340.6mg(1.4925mmol) ammonium persulfate becomes 3.618g(8.9552mmol) Fe(NO3)39H2O, reaction 12h in step (4) becomes 24h.
Shown in the performance parameter chart 1 of the graphene oxide/Pt/Polypyrrole composite material of the lamella micro-structural that embodiment 1-5 prepares:
Table 1
Claims (9)
1. the preparation method of the graphene oxide/Pt/Polypyrrole composite material of a lamella micro-structural is characterized in that step is as follows:
(1) organic sulfonic acid is added in the weak solution of graphene oxide, stir and utilize ultrasonic wave to disperse to make it to mix after continue to stir under condition of ice bath after, standby;
(2) pyrrole monomer is injected in said mixture, stirs and form reaction system, standby;
(3) oxidant is dissolved in the water and makes solution, the reaction system that adds fast step (2) to form, mix; Stirring reaction 12-24h under condition of ice bath, clean the product that obtains repeatedly with deionized water, and, in the vacuum drying chamber inner drying, obtain the graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural.
2. the preparation method of the graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural according to claim 1, it is characterized in that: the described organic sulfonic acid of step (1) is: 1,5-naphthalenedisulfonic acid, sulfanilic acid, α-naphthalenesulfonicacid, any in beta-naphthalenesulfonic-acid.
3. the preparation method of the graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural according to claim 1, it is characterized in that: the described oxidant of step (3) is: any in ammonium persulfate, potassium peroxydisulfate, anhydrous ferric trichloride, Fe(NO3)39H2O.
4. the preparation method of the graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural according to claim 1, is characterized in that the pyrroles of step (2) is before use through heavily steaming.
5. the preparation method of the graphene oxide/Pt/Polypyrrole composite material of the described micro-structural of lamella according to claim 1, is characterized in that the temperature of the ice bath of step (1), (3) is controlled at 5 ℃ of 0-.
6. the preparation method of the graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural according to claim 1, is characterized in that the concentration of graphene oxide weak solution in step (1) is 0.1-0.5mg/mL.
7. the preparation method of the graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural according to claim 1, is characterized in that in step (2), the mass ratio of graphene oxide and pyrroles is 1:10-1:30, and organic sulfonic acid and pyrroles's mol ratio is 1:4-1:1.
8. the preparation method of the graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural according to claim 1, is characterized in that in step (3), pyrroles's and oxidant mol ratio is 1:1-1:2.
9. the preparation method of the graphene oxide/Pt/Polypyrrole composite material of lamella micro-structural according to claim 1, the bake out temperature that it is characterized in that step (4) is 60 ℃, drying time is 24h.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103887076A (en) * | 2014-01-21 | 2014-06-25 | 华侨大学 | Water system asymmetric super capacitor and preparation method thereof |
| CN104934236A (en) * | 2015-04-30 | 2015-09-23 | 河海大学 | Method of preparing electroactive molecule grafted graphene doped conductive polymer electrode materials |
| CN105244190A (en) * | 2015-10-21 | 2016-01-13 | 山东科技大学 | Preparation method of graphene/carbon nano tube co-reinforced conducting polymer hydrogel |
| CN107090586A (en) * | 2017-04-13 | 2017-08-25 | 上海应用技术大学 | A kind of FeS2RGO composites, preparation method and applications |
| CN107698914A (en) * | 2017-11-08 | 2018-02-16 | 山东科技大学 | A kind of preparation method of flexible memory conductive polymer composite aquogel |
| CN109888183A (en) * | 2019-04-02 | 2019-06-14 | 上海理工大学 | A kind of preparation method and application of organic inorganic hybridization film |
| CN110041739A (en) * | 2019-04-02 | 2019-07-23 | 砥创(苏州)新材料科技有限公司 | A kind of efficient corrosion resisting oversize graphene aqueous slurry and preparation method thereof |
| CN112908728A (en) * | 2021-01-15 | 2021-06-04 | 河南大学 | Double-anion doped polypyrrole electrode slice, preparation method thereof and super capacitor |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103887076A (en) * | 2014-01-21 | 2014-06-25 | 华侨大学 | Water system asymmetric super capacitor and preparation method thereof |
| CN104934236A (en) * | 2015-04-30 | 2015-09-23 | 河海大学 | Method of preparing electroactive molecule grafted graphene doped conductive polymer electrode materials |
| CN105244190A (en) * | 2015-10-21 | 2016-01-13 | 山东科技大学 | Preparation method of graphene/carbon nano tube co-reinforced conducting polymer hydrogel |
| CN107090586A (en) * | 2017-04-13 | 2017-08-25 | 上海应用技术大学 | A kind of FeS2RGO composites, preparation method and applications |
| CN107698914A (en) * | 2017-11-08 | 2018-02-16 | 山东科技大学 | A kind of preparation method of flexible memory conductive polymer composite aquogel |
| CN109888183A (en) * | 2019-04-02 | 2019-06-14 | 上海理工大学 | A kind of preparation method and application of organic inorganic hybridization film |
| CN110041739A (en) * | 2019-04-02 | 2019-07-23 | 砥创(苏州)新材料科技有限公司 | A kind of efficient corrosion resisting oversize graphene aqueous slurry and preparation method thereof |
| CN110041739B (en) * | 2019-04-02 | 2021-11-26 | 砥创(苏州)新材料科技有限公司 | Oversized graphene aqueous slurry for efficient corrosion prevention and preparation method thereof |
| CN112908728A (en) * | 2021-01-15 | 2021-06-04 | 河南大学 | Double-anion doped polypyrrole electrode slice, preparation method thereof and super capacitor |
| CN112908728B (en) * | 2021-01-15 | 2021-10-26 | 河南大学 | Double-anion doped polypyrrole electrode slice, preparation method thereof and super capacitor |
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