CN105797752A - Fullerene modified graphene/cadmium sulfide catalyst as well as preparation method and application thereof - Google Patents
Fullerene modified graphene/cadmium sulfide catalyst as well as preparation method and application thereof Download PDFInfo
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- CN105797752A CN105797752A CN201610204368.9A CN201610204368A CN105797752A CN 105797752 A CN105797752 A CN 105797752A CN 201610204368 A CN201610204368 A CN 201610204368A CN 105797752 A CN105797752 A CN 105797752A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/02—Preparation of oxygen
- C01B13/0203—Preparation of oxygen from inorganic compounds
- C01B13/0207—Water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
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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
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention relates to a fullerene modified graphene/cadmium sulfide catalyst as well as a preparation method and an application thereof. The fullerene is C60, and the fullerene modified graphene/cadmium sulfide catalyst is represented as C60-rGO/CdS, a mass ratio of graphene to fullerene C60 in the catalyst is 8:(1-8), and a mass ratio of fullerene modified graphene to cadmium sulfide in the catalyst is (0.1-5):100. The catalyst is prepared with a one-step hydrothermal method and is applied to a photolysis reaction of water. Compared with the prior art, the operation is simple, the concept is novel, renewable and clean energy can be prepared through water photolysis, and a new research direction is developed for application of cadmium sulfide in the photocatalysis field.
Description
Technical field
The present invention relates to the technical field of solar energy catalytic decomposition water, be specifically related to the graphite that a kind of fullerene is modified
Alkene/cadmium sulfide catalyst and preparation method and application.
Background technology
21 century, in the face of the most serious energy and environmental problem, scientists is devoted to seek renewable new energy
Source replaces Fossil fuel, and solar energy is as the inexhaustible energy.Therefore, how solar energy is utilized
Producing renewable and clean energy resource and cause the concern of the mankind, preparation low cost, high efficiency photocatalyst have important
Research Significance.Present numerous semi-conducting material obtains the biggest concern, but develops the most available photocatalyst still
So there is a lot of problem.
Cadmium sulfide (CdS) provides new thinking and method as photocatalyst.Cadmium sulfide is a kind of important half
Conductor material, is widely used in the fields such as photoelectricity, chemical sensor, photocatalysis.The energy gap of CdS is about
2.4eV, it is possible to preferably mate with the limit of visible spectrum in solar irradiation, therefore, it is possible to be efficiently absorbed the sun
Can, illustrate the photocatalysis performance of its excellence.But there is the interior of a photoetch sex chromosome mosaicism in CdS photocatalyst
In shortcoming so that CdS is highly unstable as a kind of photocatalyst, significantly hinders its actual application.Extremely
The modern relevant CdS reported application in photocatalytic water, mainly modifies with precious metal surface, increases electronics and passes
Defeated speed, modifies as a example by noble metal platinum by surface, and illumination causes the separation in CdS electronics and hole, light induced electron
Transfer to Pt metal decomposition water liberation of hydrogen, prepare the most again semiconductor composite, utilize level-density parameter to improve light and urge
Change activity.But reaction is relatively costly, and CdS light stability problem is the most significantly improved.
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and provide a kind of low cost, light steady
Graphene/cadmium sulfide catalyst that qualitative good fullerene is modified and preparation method and application.
The purpose of the present invention can be achieved through the following technical solutions:
Technical solution of the present invention one:
Graphene/cadmium sulfide catalyst that a kind of fullerene is modified, described fullerene is C60, fullerene is modified
Graphene/cadmium sulfide catalyst is expressed as C60-rGO/CdS, Graphene and fullerene C in this catalyst60Quality
Ratio is 8:(1-8), the Graphene that in this catalyst, fullerene is modified is (0.1-5) with the mass ratio of cadmium sulfide: 100,
That is, C in this catalyst60The mass ratio of-rGO and CdS is (0.1-5): 100, preferably 2:100.
Technical solution of the present invention two:
The preparation method of Graphene/cadmium sulfide catalyst that above-mentioned fullerene is modified, by the method system of a step hydro-thermal
Standby obtain, specifically include following steps:
(1) by graphene oxide and fullerene C60, it is scattered in organic solvent, supersound process, treats fullerene
C60After being completely dispersed and being sufficiently mixed with graphene oxide, organic solvent is evaporated and volatilizees completely, be subsequently adding second
Alcohol, is centrifuged, washs, dries, and obtains the graphene oxide composite material that fullerene is modified, is expressed as C60-GO；
(2) graphene oxide composite material that step (1) gained fullerene is modified is dissolved in ethylenediamine, adds
Cd(NO3)2·4H2O, is stirring evenly and then adding into thiourea, continues stirring, carries out hydro-thermal reaction, be subsequently cooled to room
Temperature, centrifugation, deionized water and washing with alcohol three times and above after, be dried, obtain fullerene modify graphite
Alkene/cadmium sulfide catalyst C60-rGO/CdS。
Preferably, in step (1), graphene oxide and fullerene C60Weight ratio be 8:(1-8).
Preferably, in step (1), described organic solvent is volatile solvent, selected from toluene etc., and ultrasonic place
Reason time at 10-60min, preferably 30min.
Preferably, in step (1), solvent is evaporated required temperature at 80-130 DEG C, preferably 100-110 DEG C.
Preferably, in step (2), by graphene oxide composite material, the Cd (NO of regulation fullerene modification3)2·4H2O
And the quality of thiourea makes the Graphene that the fullerene that obtains in step (2) modifies with the mass ratio of cadmium sulfide to be
(0.1-5):100.Ethylenediamine in step (2) is used for regulating and controlling CdS pattern, the oxidation stone modified with fullerene
Ink alkene material is not directly dependent upon.
Preferably, in step (2), the condition of described hydro-thermal reaction is: keep 10-15 little at 160-200 DEG C
Time, it is preferably and keeps 12 hours at 180 DEG C.The temperature being dried in step (2) is preferably controlled in 80 DEG C.
Technical solution of the present invention three:
The application of Graphene/cadmium sulfide catalyst that offer fullerene is modified, the Graphene that described fullerene is modified/
Cadmium sulfide catalyst photocatalyst, generates hydrogen and oxygen for photocatalytic water.
First kind of way: Graphene/cadmium sulfide catalyst that described fullerene is modified is used in pure aquatic system,
Under illumination effect, realized the full decomposition of water by the pH value of regulation water.
The second way, Graphene/cadmium sulfide catalyst that described fullerene is modified is for the mixing of water with methanol
In reaction system, under illumination effect, realized the full decomposition of water by the pH value of regulation solution.Described water with
In the hybrid reaction system of methanol, water is 3:1 with the volume ratio of methanol, and methanol is as sacrifice agent.
The regulation of described pH value realizes by adding NaOH, can be very by changing reacting liquid pH value
The valence band of good regulation cadmium sulfide and conduction band positions, it is achieved the full decomposition of water.The scope of pH is at 7-14.Catalyst
Addition and the proportionate relationship of water control between 50mg:80mL to 20mg:60mL.
In the present invention, (by the Graphene of graphene oxide reduction, it is also referred to as with the Graphene that fullerene is modified
Reduced graphene) it is carrier synthesizing cadmium sulfide catalyst..The C of grafting60Molecular cluster is total to due to strong with rGO
Valency interacts and is greatly promoted photo-generated carrier density, and photovoltage responds, meanwhile, and fullerene and stone
The interaction of ink alkene forms nanotip and further improves electron transport ability, and fullerene molecule bunch is as analysis
The avtive spot of hydrogen promotes the generation of photolysis water hydrogen.Superior electron transfer rate is conducive to photo-generated carrier
Separate, improve the efficiency of photochemical catalyzing, improve cadmium sulfide light stability, at 36 hours active testings
Remain to keep preferable activity.Meanwhile, by change reacting liquid pH value can well regulate cadmium sulfide valence band and
Conduction band positions, it is achieved the full decomposition of water.
Compared with prior art, beneficial effects of the present invention is embodied in following several respects:
(1) Graphene/cadmium sulfide catalyst that fullerene is modified, preparation are prepared by the method for a step hydro-thermal
Technique is simple.
(2) present invention fullerene grapheme modified/cadmium sulfide catalyst, low cost, and there is good stablizing
Property.
(3) covalent effect that fullerene molecule bunch is strong with Graphene promotes the migration of light induced electron, liberation of hydrogen further
Site is the nanotip that fullerene molecule bunch is formed, and can improve photocatalytic water greatly by regulation reacting liquid pH value
Efficiency.
(4) catalyst of the present invention is simple to operate in application process, process environmental protection, has sustainability.
Accompanying drawing explanation
Fig. 1 is the X-ray diffracting spectrum of catalyst of the present invention；
Fig. 2 is C60The projection electromicroscopic photograph of the Graphene modified；
Fig. 3 is C60The projection electromicroscopic photograph of-rGO/CdS composite；
Fig. 4 is C60The photoelectric current collection of illustrative plates of-rGO/CdS composite photo-catalyst and CdS；
Fig. 5 is C60-rGO/CdS composite photo-catalyst and the impedance spectrum of CdS；
Fig. 6 is C60-rGO/CdS composite photo-catalyst photolysis water hydrogen activity figure.
Detailed description of the invention
Elaborating embodiments of the invention below, the present embodiment enters under premised on technical solution of the present invention
Row is implemented, and gives detailed embodiment and concrete operating process, but under protection scope of the present invention is not limited to
The embodiment stated.
Embodiment 1
Graphene/cadmium sulfide catalyst that a kind of fullerene is modified, in the present embodiment, fullerene is C60, fowler
Graphene/cadmium sulfide catalyst that alkene is modified is expressed as C60-rGO/CdS, Graphene and fullerene in this catalyst
C60Mass ratio be 8:1, in this catalyst, the mass ratio of Graphene and cadmium sulfide that fullerene is modified is 2:100.
The preparation method of Graphene/cadmium sulfide catalyst that the present embodiment fullerene is modified, comprises the following steps:
(1) 80mg GO and 20mg C is taken60It is distributed in the toluene solution of 100mL, ultrasonic 30min,
Treat C60After being completely dispersed and being sufficiently mixed with GO, above-mentioned solution is evaporated at 110 DEG C, makes toluene wave completely
Send out, after being centrifuged with ethanol, wash, dry the most again, i.e. obtain C60The GO material modified, is abbreviated as
C20-GO, 20 represent C60Milligram number；
(2) 8.56g Cd (NO is taken3)2·4H2O joins 40mL containing above-mentioned prepared whole C20-GO's
In ethylenediamine solvent, after stirring, then in solution, add 4.20g thiourea, continue stirring 0.5h,
Again above-mentioned solution is transferred in 50mL water heating kettle, after keeping 12h under the conditions of 180 DEG C, naturally cool to room
Temperature, after respectively washing three times with deionized water and ethanol by centrifugation, is vacuum dried 12h at 80 DEG C, can obtain
C60The catalyst of the CdS Nanorods Catalyst of the reduction GO load modified, is abbreviated as C20-rGO/CdS, 20
Represent C60Milligram number.
Cadmium sulfide (CdS) is carried on Graphene (rGO) and fullerene (C respectively60On), it is denoted as rGO-CdS respectively
And C60-CdS, and to C20-rGO/CdS, CdS, rGO-CdS and C60-CdS carries out X-ray diffraction respectively,
The result obtained is as shown in Figure 1.From figure 1 it appears that hexagonal phase all can be loaded on different carriers
CdS nanometer rods, i.e. embodiment 1 gained C20-rGO/CdS success is CdS-loaded.
The C that said method is obtained20-rGO/CdS and C60-rGO carries out electron-microscope scanning, and the electron-microscope scanning obtained shines
Sheet is distinguished the most as shown in Figure 2 and Figure 3, it can be seen that C60Molecular cluster is formed on reduced graphene surface, simultaneously
CdS nanometer rods successfully loads to C20-rGO surface.
With 0.5M Na2SO4Solution is electrolyte, obtains with 420nm LED monochromatic light for test of light source
C20The photoelectric current of-rGO/CdS catalyst and impedance diagram, the most as shown in Figure 4 and Figure 5.It can be seen that it is rich
The graphene oxide strangling alkene modification is that carrier can be greatly improved photocurrent response intensity, increases electron transfer rate.
The C that above-mentioned steps obtains20-rGO/CdS catalyst, is applied in the photolysis of water, specifically comprises the following steps that
With 60mL water, 20mL water methanol (sacrifice agent) as reaction system, with NaOH regulation pH value of solution extremely
7, take 50mg catalyst, logical high-purity N2By air emptying；Airtight, stirring under conditions of, with 4
420nmLED lamp is test of light source photocatalytic water activity, and as shown in Figure 6, from Fig. 6, our acquired results can
Go out, C20-rGO/CdS catalyst has the stability of extraordinary photo catalytic reduction water hydrogen manufacturing, reacts 36 hours
Preferably activity can be kept.
Embodiment 2
Using the preparation method roughly the same with embodiment 1, difference is C60Addition become 10mg,
The graphene oxide that the fullerene of gained is modified is C10-GO, the C of gained60The reduced graphene load modified
CdS Nanorods Catalyst is C10-rGO/CdS。
Embodiment 3
Using the preparation method roughly the same with embodiment 1, difference is C60Addition become 30mg,
The graphene oxide that the fullerene of gained is modified is C30-GO, the C of gained60The reduced graphene load modified
CdS Nanorods Catalyst is C30-rGO/CdS。
Embodiment 4
Using the preparation method roughly the same with embodiment 1, difference is C60Addition become 40mg,
The graphene oxide that the fullerene of gained is modified is C40-GO, the C of gained60The reduced graphene load modified
CdS Nanorods Catalyst is C40-rGO/CdS。
Embodiment 5
Using the preparation method roughly the same with embodiment 1, difference is C60Addition become 50mg,
The graphene oxide that the fullerene of gained is modified is C50-GO, the C of gained60The reduced graphene load modified
CdS Nanorods Catalyst is C50-rGO/CdS。
Embodiment 6
Using the preparation method roughly the same with embodiment 1, difference is C60Addition become 80mg,
The graphene oxide that the fullerene of gained is modified is C80-GO, the C of gained60The reduced graphene load modified
CdS Nanorods Catalyst is C80-rGO/CdS。
Embodiment 7
C is obtained by embodiment 1 step20-rGO/CdS, is applied in the photolysis of water, step and enforcement
Example 1 is roughly the same, and difference is with NaOH regulation pH value of solution to 8, detects photolytic activity.At pH=8
Under conditions of, in active testing, hydrogen does not produces.
Embodiment 8
C is obtained by embodiment 1 step20-rGO/CdS, is applied in the photolysis of water, step and enforcement
Example 1 is roughly the same, and difference is with NaOH regulation pH value of solution to 9, detects photolytic activity.At pH=9
Under conditions of, in active testing, hydrogen does not produces.
Embodiment 9
C is obtained by embodiment 1 step20-rGO/CdS, is applied in the photolysis of water, step and enforcement
Example 1 is roughly the same, and difference is with NaOH regulation pH value of solution to 10, detects photolytic activity.At pH=10
Under conditions of, in active testing, hydrogen does not produces.
Embodiment 10
C is obtained by embodiment 1 step20-rGO/CdS, is applied in the photolysis of water, step and enforcement
Example 1 is roughly the same, and difference is with NaOH regulation pH value of solution to 14, detects photolytic activity.At pH=14
Under conditions of, active testing hydrogen gas rate is 127.2 μm ol*h-1*g-1。
Claims (10)
1. Graphene/cadmium sulfide catalyst that a fullerene is modified, it is characterised in that described fullerene is
C60, Graphene/cadmium sulfide catalyst that fullerene is modified is expressed as C60-rGO/CdS, Graphene in this catalyst
With fullerene C60Mass ratio be 8:(1-8), the matter of Graphene and cadmium sulfide that fullerene is modified in this catalyst
Amount ratio is (0.1-5): 100.
2. the preparation method of Graphene/cadmium sulfide catalyst that fullerene as claimed in claim 1 is modified, it is special
Levy and be, prepared by the method for a step hydro-thermal, specifically include following steps:
(1) by graphene oxide and fullerene C60, it is scattered in organic solvent, supersound process, treats fullerene
C60After being completely dispersed and being sufficiently mixed with graphene oxide, organic solvent is evaporated and volatilizees completely, be subsequently adding second
Alcohol, is centrifuged, washs, dries, and obtains the graphene oxide composite material that fullerene is modified, is expressed as C60-GO；
(2) graphene oxide composite material that step (1) gained fullerene is modified is dissolved in ethylenediamine, adds
Cd(NO3)2·4H2O, is stirring evenly and then adding into thiourea, continues stirring, carries out hydro-thermal reaction, be subsequently cooled to room
Temperature, centrifugation, deionized water and washing with alcohol three times and above after, be dried, obtain fullerene modify graphite
Alkene/cadmium sulfide catalyst C60-rGO/CdS。
The preparation method of Graphene/cadmium sulfide catalyst that a kind of fullerene the most according to claim 2 is modified,
It is characterized in that, in step (1), graphene oxide and fullerene C60Weight ratio be 8:(1-8).
The preparation method of Graphene/cadmium sulfide catalyst that a kind of fullerene the most according to claim 2 is modified,
It is characterized in that, in step (1), described organic solvent is volatile solvent, selected from toluene.
The preparation method of Graphene/cadmium sulfide catalyst that a kind of fullerene the most according to claim 2 is modified,
It is characterized in that, in step (2), by graphene oxide composite material, the Cd (NO of regulation fullerene modification3)2·4H2O
And the quality of thiourea makes the Graphene that the fullerene that obtains in step (2) modifies with the mass ratio of cadmium sulfide to be
(0.1-5):100。
The preparation method of Graphene/cadmium sulfide catalyst that a kind of fullerene the most according to claim 2 is modified,
It is characterized in that, in step (2), the condition of described hydro-thermal reaction is: keep 10-15 little at 160-200 DEG C
Time.
7. an application for Graphene/cadmium sulfide catalyst that fullerene as claimed in claim 1 is modified, it is special
Levy and be, Graphene/cadmium sulfide catalyst photocatalyst that described fullerene is modified, aquatic for photodissociation
Become hydrogen and oxygen.
The application of Graphene/cadmium sulfide catalyst that a kind of fullerene the most according to claim 7 is modified, its
Being characterised by, Graphene/cadmium sulfide catalyst that described fullerene is modified is in pure aquatic system, by regulation
The pH value of water realizes the full decomposition of water.
The application of Graphene/cadmium sulfide catalyst that a kind of fullerene the most according to claim 7 is modified, its
Being characterised by, Graphene/cadmium sulfide catalyst that described fullerene is modified is for the hybrid reaction body of water with methanol
In system, realized the full decomposition of water by the pH value of regulation solution.
The application of Graphene/cadmium sulfide catalyst that a kind of fullerene the most according to claim 7 is modified,
It is characterized in that, the addition of catalyst and the proportionate relationship of water control at 50mg:80mL to 20mg:60mL
Between.
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| CN108273527A (en) * | 2018-03-30 | 2018-07-13 | 台州学院 | FeSe/CdS nano composite photo-catalysts and preparation method |
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| CN114534746A (en) * | 2022-02-28 | 2022-05-27 | 浙江理工大学 | Photocatalytic hydrogen production system based on heterojunction photocatalyst and formaldehyde aqueous solution |
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| CN108273527A (en) * | 2018-03-30 | 2018-07-13 | 台州学院 | FeSe/CdS nano composite photo-catalysts and preparation method |
| CN111686761A (en) * | 2020-05-20 | 2020-09-22 | 华南理工大学 | Cu/CdS/graphene composite photocatalyst and preparation method and application thereof |
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| CN114644320A (en) * | 2022-03-18 | 2022-06-21 | 浙江理工大学 | Photocatalytic hydrogen production system and application thereof |
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