CN107195918B - It is a kind of using graphene-fullerene three-dimensional composite material as the fuel-cell catalyst of carrier and its preparation and application - Google Patents
It is a kind of using graphene-fullerene three-dimensional composite material as the fuel-cell catalyst of carrier and its preparation and application Download PDFInfo
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- CN107195918B CN107195918B CN201710409807.4A CN201710409807A CN107195918B CN 107195918 B CN107195918 B CN 107195918B CN 201710409807 A CN201710409807 A CN 201710409807A CN 107195918 B CN107195918 B CN 107195918B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
- H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
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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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The present invention relates to a kind of using graphene-fullerene three-dimensional composite material as the fuel-cell catalyst of carrier and its preparation and application, under nitrogen protection, Fullerene C20, sarcosine and paraformaldehyde is reacted fullerene synthesis pyrrolidin derivatives in reflux in toluene；The ethanol solution of the fullerene derivate of synthesis and graphene oxide water solution are mixed and stand self assembly, prepares graphene oxide-fullerene three-dimensional self-assembled structures；Using hydrazine hydrate while redox graphene and metal ion are to get using graphene-fullerene three-dimensional composite material as the catalyst of carrier；By the performance of the prepared catalyst Oxidation of Methanol of electrochemical cyclic voltammetry test, it is found that the performance of catalyst prepared by the present invention is significantly increased.Operation of the present invention is simple and fast, and the catalyst prepared is at low cost, catalytic performance is good, has the potential application foreground in direct methanol fuel cell.
Description
Technical field
The invention belongs to fuel cell catalyst materials and its preparation and application fields, in particular to one kind is with graphene-
Fullerene three-dimensional composite material is the fuel-cell catalyst of carrier and its preparation and application.
Background technique
It is a kind of cleaning energy quickly grown in recent years with the fuel cell that direct methanol fuel cell (DMFC) is representative
Source, but the practical popularization and use of DMFC still suffer from severe challenge, wherein the performance difference of catalyst and it is at high cost be two important
Limiting factor.It is currently used raising catalyst catalytic performance and drop by the way that metallic catalyst is loaded to carbon material surface
The effective ways of low cost.
The carbon material for being generally used for catalyst carrier mainly has conductive carbon black, carbon nanotube and graphene, but is received with compound
Rice carbon material, it is less especially with the research of fullerene-based material.Using the special self-assembly property of fullerene, have for preparation big
Composite catalyst carrier material than table product provides possibility.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of using graphene-fullerene three-dimensional composite material as carrier
Fuel-cell catalyst and its preparation and application, the method for the present invention is by being self-assembly of using fullerene and graphene oxide
Three-dimensional structure is catalyst carrier, is prepared for graphene-fulvene compounding material load palladium catalyst by hydro-thermal method, both mentioned
The high performance of catalyst, and reduce catalyst cost.Operating process is simple and quick, has potentially answer in a fuel cell
Use prospect.
Of the invention a kind of using graphene-fullerene three-dimensional composite material as the fuel-cell catalyst of carrier, the combustion
Material battery is urged
Agent is using graphene-fulvene compounding material of three-dimensional structure as the palladium catalyst of carrier.
Of the invention is a kind of using graphene-fullerene three-dimensional composite material as the preparation side of the fuel-cell catalyst of carrier
Method, comprising:
(1) under nitrogen protection, by fullerene 60, paraformaldehyde and sarcosine in reflux in toluene, reaction temperature is
100-120 DEG C, reaction time 12-16h, separating-purifying obtains fulleropyrrolidine derivative；Wherein Fullerene C20, poly
The mass ratio of formaldehyde and sarcosine is 2:0.5~1.5:3~6；
(2) fulleropyrrolidine derivative solution is mixed and is stood with graphene oxide solution, self assembly is carried out, by shape
At precipitation and centrifugal separation, obtain graphene oxide-fullerene three-dimensional self-assembled structures composite material；
(3) it disperses above-mentioned graphene oxide-fullerene three-dimensional self-assembled structures compound material ultrasound in aqueous solution, adds
Enter palladium chloride aqueous solution sonic oscillation again, be then transferred to hydrothermal reaction kettle, hydrazine hydrate is added, keeps the temperature 3-5h at 95 DEG C, is centrifuged
Separation is to get using graphene-fullerene three-dimensional composite material as the fuel-cell catalyst of carrier.
In the step (1) separating-purifying be used in be silicagel column, wherein eluant, eluent be toluene/ethanol (volume ratio
For 10:1).
The structural formula of fulleropyrrolidine derivative is in the step (1)Wherein n=1~7.
The solvent of fulleropyrrolidine derivative solution is ethyl alcohol in the step (2)；The solvent of graphene oxide solution
For water, solution concentration is 0.5mg/ml.
Graphene oxide is to utilize Hummers method graphite oxide powder preparation gained in the step (2).
The mass ratio of graphene oxide and fulleropyrrolidine derivative is 1:0.5~1 in step (2).
Time of repose is 2~6h in the step (2).
Palladium chloride aqueous solution sonic oscillation 20-35min again is added in the step (3).
In step (3) in water by graphene oxide-fullerene three-dimensional composite material ultrasonic disperse, it is water-soluble that palladium chloride is added dropwise
Liquid again sonic oscillation disperse 30 minutes after, be transferred to hydrothermal reaction kettle, with hydrazine hydrate simultaneously redox graphene and palladium ion,
Prepare graphene-fulvene compounding material load palladium catalyst.
The mass ratio of Metal Palladium and carrier is 1:4 in step (3).
What step (3) obtained is the fuel-cell catalyst of carrier for urging using graphene-fullerene three-dimensional composite material
Change the performance test of Oxidation of Methanol: specifically: the electrochemical workstation that electrocatalysis characteristic test utilizes is CHI 660D, work electricity
Extremely glass-carbon electrode is platinum electrode to electrode, and reference electrode is saturated calomel electrode (SCE), and electrolyte is 1.0M CH3OH+
1.0M NaOH solution, potential scanning speed 50mV/s, electric potential scanning range are -1~0.2V.
By the performance of the prepared catalyst Oxidation of Methanol of electrochemical cyclic voltammetry test, present invention system is found
The performance of standby catalyst is significantly increased.Operation of the present invention is simple and fast, and the catalyst prepared is at low cost, catalytic performance
It is good, there is the potential application foreground in direct methanol fuel cell.
Of the invention is a kind of using graphene-fullerene three-dimensional composite material as the application of the fuel-cell catalyst of carrier,
Using graphene-application of the fullerene three-dimensional composite material as the fuel-cell catalyst of carrier in methanol fuel cell.
One kind of the invention prepares 3-D nano, structure graphene-fullerene composite wood with fullerene and graphene self assembly
The preparation method of material and its fuel-cell catalyst as carrier, gained catalyst performance is excellent, in direct methanol fuel electricity
There is important application prospect in pond.
Beneficial effect
That (1) the present invention overcomes general carbon material carrier specific surface areas is smaller, catalyst synthesis is complicated and catalytic performance is poor,
The disadvantages of at high cost；
(2) present invention incorporates fullerene-graphene three-dimensional structures of bigger serface as carrier and easy hydro-thermal
Reaction prepares metal catalytic agent method, is prepared for novel fuel-cell catalyst；
(3) preparation method of the present invention is simple and quick, the catalyst performance of preparation is good；
(4) graphene prepared by the present invention-fullerene three-dimensional composite material load palladium catalyst is compared with simple graphene
There is higher catalytic activity for the palladium catalyst of carrier, there is potential application foreground in direct methanol fuel cell.
Detailed description of the invention
Fig. 1 (a) is graphene oxide-fullerene three-dimensional self-assembled structures scanning electron microscope (SEM) photograph, is (b) graphene-fowler
The transmission electron microscope picture of alkene three-dimensional composite material loaded palladium catalyst；
Fig. 2 is palladium catalyst on different carriers to anodic oxidation of methanol cyclic voltammetry curve, and wherein carrier is distinguished
It is respectively the graphene and fulvene compounding material of RGO:C60=1:0.5 and 1:1 for pure graphene (RGO) or mass ratio；
Fig. 3 is chronoa mperometric plot of the palladium catalyst on different carriers to anodic oxidation of methanol.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
The oscillator device that the present invention uses is KQ-3200 type ultrasonic cleaner；Drying equipment is dry for DZF-6051 vacuum
Dry case；Scanning electron microscope (SEM) is S-4800；Transmission electron microscope (TEM) is JEM-2100F；Electro-chemical test equipment is CHI 660D
Electrochemical workstation.
Embodiment 1
The synthesis of fulleropyrrolidine derivative.
In 100ml round-bottomed flask, be added the paranitrobenzaldehyde of C60,36mg of 72mg, the sarcosine of 180mg and
The toluene of 45ml, nitrogen protection lower 115 DEG C of back flow reactions 14 hours, filtrate was concentrated cold filtration with vacuum rotary evaporator
By silica gel chromatography, eluant, eluent is toluene/ethanol (10:1).Products therefrom is characterized by MALDI-TOF-MS, is being divided
Son amount is to observe serial mass spectra peak at 834~1119, corresponds respectively to 2-7 pyrrolidinyl substituent group.
Embodiment 2
The preparation of graphene oxide-fullerene three-dimensional self-assembled structures.
By the ethanol solution of 20ml graphene oxide water solution (0.5mg/ml) and 10 milliliters of fulleropyrrolidine derivatives
(0.5mg/ml) ultrasound mixes for 5 minutes, stands 4 hours；Water ultrasonic disperse will be used again after the precipitation and centrifugal separation of formation, is directly dripped
It is added on clean silicon wafer, using S-4800 scanning electron microscope observation, graphene oxide-fullerene three-dimensional self-assembled structures can be obtained
(Fig. 1 a).
Embodiment 3
The preparation of graphene-fullerene three-dimensional composite material loaded palladium catalyst.
By 20mg graphene oxide-fullerene three-dimensional composite material ultrasonic disperse in 20ml aqueous, 2ml palladium chloride is added
Aqueous solution (2mg/ml) is 30 minutes ultrasonic again, is transferred in hydrothermal reaction kettle, reacts 4 at 95 DEG C after the hydrazine hydrate of 80 μ l is added
Hour.It cools down and is centrifugated, after precipitating distillation washing three times, it is small to be placed in a vacuum drying oven at 40~50 DEG C dry 24
When to get graphene-fullerene three-dimensional composite material loaded palladium catalyst.It is characterized by TEM, it is seen that catalyst nano
Grain is dispersed in graphene-fullerene three-dimensional composite material surface (Fig. 1 b).
Embodiment 4
The test of graphene-fullerene three-dimensional composite material loaded palladium catalyst electrocatalysis characteristic.
Made graphene-fullerene three-dimensional composite material loaded palladium catalyst 2mg is dispersed in 1ml ethyl alcohol, ultrasound vibration
It after swinging 30 minutes, pipettes 5 μ l and drips on the glass-carbon electrode polished smooth, after infrared lamp drying, then be added dropwise 5 μ l's 0.5%
Nafion solution obtains working electrode.Made working electrode is placed on 1.0M CH3In OH+1.0M NaOH mixed solution, with
Platinum electrode is to electrode, and with saturated calomel electrode (SCE) for reference electrode, the cyclic voltammetric for testing anodic oxidation of methanol is bent
Line and chronoa mperometric plot.The result shows that the present invention is when palladium load capacity is identical with graphene and fulleropyrrolidine derivative
Synthesized three-dimensional composite material loaded palladium catalyst has best catalytic activity (figure to methanol oxidation when mass ratio 1:0.5
And stability (Fig. 3) 2).Wherein it can be seen that with graphene and when fullerene mass ratio RGO:C60=1:0.5 it is synthesized three
The palladium catalyst of the more simple graphene of palladium catalyst catalytic activity (RGO) load of dimension composite material load improves about 1.5 times,
And highest current density is still kept after continuous discharge 3000 seconds, show high stability.But with graphene and fowler
The performance of Pd catalyst decline of synthesized three-dimensional composite material load when alkene mass ratio RGO:C60=1:1 is due to high concentration
Fullerene reduce caused by carrier material electric conductivity.It can be seen that compound suitable fullerene can increase graphene load in graphene
The specific surface area of body material, to improve the electro catalytic activity of metallic catalyst.
Claims (8)
1. a kind of using graphene-fullerene three-dimensional composite material as the preparation method of the fuel-cell catalyst of carrier, comprising:
(1) under nitrogen protection, by Fullerene C20, paraformaldehyde and sarcosine in reflux in toluene, reaction temperature 100-
120 DEG C, reaction time 12-16h, separating-purifying obtains fulleropyrrolidine derivative；Wherein Fullerene C20, paraformaldehyde
Mass ratio with sarcosine is 2:0.5~1.5:3~6；
(2) fulleropyrrolidine derivative solution is mixed and is stood with graphene oxide solution, be centrifuged, obtain graphite oxide
Alkene-fullerene three-dimensional self-assembled structures composite material；
(3) it disperses above-mentioned graphene oxide-fullerene three-dimensional self-assembled structures compound material ultrasound in aqueous solution, chlorine is added
Change aqueous palladium sonic oscillation again, be then transferred to hydrothermal reaction kettle, hydrazine hydrate is added, keep the temperature 3-5h at 95 DEG C, centrifugation to get
Using graphene-fullerene three-dimensional composite material as the fuel-cell catalyst of carrier.
2. according to claim 1 a kind of using graphene-fullerene three-dimensional composite material as the fuel cell catalyst of carrier
The preparation method of agent, it is characterised in that: used in separating-purifying be silicagel column in the step (1), wherein eluant, eluent is first
The volume ratio of benzene/ethyl alcohol, toluene and ethyl alcohol is 10:1.
3. according to claim 1 a kind of using graphene-fullerene three-dimensional composite material as the fuel cell catalyst of carrier
The preparation method of agent, it is characterised in that: the structural formula of fulleropyrrolidine derivative is in the step (1)Its
Middle n=1~7.
4. according to claim 1 a kind of using graphene-fullerene three-dimensional composite material as the fuel cell catalyst of carrier
The preparation method of agent, it is characterised in that: the solvent of fulleropyrrolidine derivative solution is ethyl alcohol in the step (2)；Oxidation
The solvent of graphene solution is water, and solution concentration is 0.5mg/ml.
5. according to claim 1 a kind of using graphene-fullerene three-dimensional composite material as the fuel cell catalyst of carrier
The preparation method of agent, it is characterised in that: the mass ratio of graphene oxide and fulleropyrrolidine derivative is 1 in step (2):
0.5~1.
6. according to claim 1 a kind of using graphene-fullerene three-dimensional composite material as the fuel cell catalyst of carrier
The preparation method of agent, it is characterised in that: time of repose is 2~6h in the step (2).
7. according to claim 1 a kind of using graphene-fullerene three-dimensional composite material as the fuel cell catalyst of carrier
The preparation method of agent, it is characterised in that: palladium chloride aqueous solution sonic oscillation 20-35min again is added in the step (3).
8. according to claim 1 a kind of using graphene-fullerene three-dimensional composite material as the fuel cell catalyst of carrier
The preparation method of agent, it is characterised in that: the mass ratio of Metal Palladium and carrier is 1:4 in step (3).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108232211B (en) * | 2018-03-09 | 2020-07-24 | 浙江大学 | Self-doped fullerene fixed palladium nano electro-catalyst and preparation method and application thereof |
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| CN107831208B (en) * | 2017-09-27 | 2019-06-25 | 重庆医科大学 | The preparation method and detection method of nanocomposite, SDM electrochemistry aptamer sensor |
| CN109728312B (en) * | 2018-12-11 | 2020-11-27 | 浙江大学 | Preparation and application of graphene-fullerene ammonium iodide salt composite carrier and Pd catalytic electrode loaded by graphene-fullerene ammonium iodide salt composite carrier |
| CN109994745B (en) * | 2019-04-03 | 2022-03-04 | 东华大学 | Fullerene grafted graphene material supported palladium catalyst and preparation and application thereof |
| CN113889630B (en) * | 2021-09-29 | 2022-09-13 | 陕西科技大学 | Preparation method of composite structure oxygen reduction electrocatalyst for fuel cell cathode |
| CN115418124B (en) * | 2022-09-21 | 2024-01-12 | 无锡极电光能科技有限公司 | Cross-linked passivation type fullerene coating, perovskite battery and preparation method of perovskite battery |
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