CN106925298A - A kind of fullerene/cadmium sulfide nano composite photo-catalyst and preparation method thereof - Google Patents
A kind of fullerene/cadmium sulfide nano composite photo-catalyst and preparation method thereof Download PDFInfo
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- CN106925298A CN106925298A CN201710121766.9A CN201710121766A CN106925298A CN 106925298 A CN106925298 A CN 106925298A CN 201710121766 A CN201710121766 A CN 201710121766A CN 106925298 A CN106925298 A CN 106925298A
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- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 103
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 94
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 54
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 47
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 239000002159 nanocrystal Substances 0.000 claims abstract description 8
- AUIZLSZEDUYGDE-UHFFFAOYSA-L cadmium(2+);diacetate;dihydrate Chemical compound O.O.[Cd+2].CC([O-])=O.CC([O-])=O AUIZLSZEDUYGDE-UHFFFAOYSA-L 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 15
- 239000001257 hydrogen Substances 0.000 abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 15
- 239000003054 catalyst Substances 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 12
- 238000007146 photocatalysis Methods 0.000 abstract description 12
- 229910052793 cadmium Inorganic materials 0.000 abstract description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 235000018417 cysteine Nutrition 0.000 abstract 1
- 150000001945 cysteines Chemical class 0.000 abstract 1
- 238000004073 vulcanization Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000004577 artificial photosynthesis Methods 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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 provides a kind of fullerene/cadmium sulfide nano composite photo-catalyst and preparation method thereof.The photochemical catalyst is fullerene C60Uniform fold is formed in CdS nanocrystal surfaces, fullerene C60It is 0.4~8 with the mass ratio of CdS:100.First by Cadmium diacetate dihydrate and L cysteines addition deionized water, mixed solution is made, its mass ratio is 1.33:1.22~3.66:20~30；Again by fullerene C60Add in mixed solution, carry out hydro-thermal reaction；It is vacuum dried after hydrothermal product is washed again, fullerene/cadmium sulfide nano composite photo-catalyst is obtained.Fullerene is evenly coated at CdS nanocrystal surface and is tightly combined in catalyst of the present invention, drastically increase the separating rate of photo-generated carrier in cadmium sulfide, effectively enhance the photocatalytic activity and stability of cadmium sulfide photochemical catalyst, and preparation process is simple, photocatalytic activity and cyclical stability are superior to existing vulcanization cadmium material, are with a wide range of applications in terms of photocatalysis Decomposition aquatic products hydrogen and pollutant process.
Description
Technical field
The present invention is that, on nano material, more particularly to one kind contaminates for photocatalysis Decomposition aquatic products hydrogen and photocatalytic degradation
The nano composite photo-catalyst of material.
Background technology
Since 21 century, energy shortage has become human survival and development is faced two with problem of environmental pollution
Big key issue.For many years, people are devoted to finding suitable regenerative resource and pollutant process method.In numerous solutions
Certainly in method, semiconductor light-catalyst is due to can effectively utilize solar energy, it is considered to be one kind can solve simultaneously the energy and
The effective ways of environmental problem, and obtained the extensive concern of researcher.In past four ten years, have one by one
Many semi-conducting materials are found to can be used for photocatalyst, and make some progress, but develop conscientiously available
Photochemical catalyst is still present many problems.
In numerous semiconductor light-catalysts, cadmium sulfide (CdS), can be with due to low energy gap (2.4eV)
The preferable visible light part that must be absorbed in sunshine, all shows very excellent photocatalytic under sunshine or visible ray
Energy.Additionally, CdS also has, resource distribution is wide, and price is low, prepares the advantage such as simple.Therefore CdS is used as a kind of important semiconductor
Material, has been employed for a variety of fields, such as photoelectricity, solar cell, chemical sensor and photochemical catalyst.So
And, CdS base optic catalytic materials there is also that such as photocatalytic activity is poor, conversion quantum efficiency is low and photoetch problem is inherent lacks
Fall into.Under sunlight, the sulphion in CdS is easy to aoxidize to form elemental sulfur by photohole, causes its photocatalysis
Active step-down and bad stability, seriously limit its practical application.Therefore, how to solve these problems is to improve CdS
The key of photocatalytic activity.At present, except the method such as traditional doping, compound, selection modifies to improve CdS's with carbon material
Photocatalysis performance has become recent study hotspot.People are by by carbon such as agraphitic carbon, graphene oxide or CNTs
Material and CdS are compound to prepare nano composite material, using carbon material good conductivity, specific surface area is big the advantages of improving CdS's
Photocatalytic activity.Fullerene C60As a kind of new allotrope of carbon, because unique big π bond structures of non-localizedization are caused
It has excellent electron affinity, with abundant chemical reactivity.Therefore, fullerene C60In solar cell and
Widely paid attention in the fields such as artificial photosynthesis.In addition, based on its excellent Electronic Transport of Two Benzene, fullerene C60Can be with
Effectively improve TiO2、g-C3N4With the separating rate of photo-generated carrier in the photochemical catalyst such as ZnO, so as to improve their catalysis live
Property.However, it is reported that, seldom have been reported that fullerene C at present60The catalysis activity to improve CdS photochemical catalysts compound with CdS.
Therefore, new fullerene/cadmium sulfide nano composite material of the exploitation with high catalytic activity and high stability is to CdS photocatalysis materials
The development of material is significant.
The content of the invention
The purpose of the present invention, is directed to current cadmium sulfide base optic catalytic material and has that photocatalytic activity is low and photoetch is led
The latent defects such as the cyclical stability difference of cause, there is provided a kind of fullerene/cadmium sulfide nano by the preparation of the step of hydro-thermal method one is multiple
Closing light catalyst and preparation method thereof.
Technical scheme is as follows：
(1) by Cadmium diacetate dihydrate and Cys addition deionized water, dispersed mixing is obtained after stirring
Solution；Cadmium diacetate dihydrate and Cys and the mass ratio of deionized water are 1.33 in mixed solution:1.22~3.66:20
~30；
(2) by fullerene C60It is added in mixed solution obtained in step (1), fullerene C is obtained after stirring60Uniform point
Scattered mixed solution, then carries out hydro-thermal reaction；Wherein fullerene C60With the matter of the cadmium sulfide generated in step (1) mixed solution
Amount is than being 0.4~8:100；
(3) by the hydrothermal product of step (2), using deionized water and ethanol, alternately the removal of impurity is gone in washing, then by product
Vacuum drying obtains fullerene/cadmium sulfide nano composite photo-catalyst.
The mixing speed of step (1) mixed solution is 300~400r/min, and mixing time is 1~2h.
Step (2) C containing fullerene60The mixing speed of mixed solution be 300-400r/min, mixing time is
0.5-1h。
The temperature of step (3) hydro-thermal reaction is 160-220 DEG C, and hydro-thermal soaking time is 5-12h, then natural cooling
To room temperature.
The step (3) is alternately washed using deionized water and ethanol, is repeated 6~10 times；Vacuum drying temperature is 50-
100 DEG C, vacuum drying time is 8-12h.
In fullerene of the present invention/cadmium sulfide nano composite photo-catalyst, CdS nanocrystal has size small
The characteristics of (30-80nm), therefore photoelectron-transfer distance in illumination shortens, and is conducive to the generation of reaction.In fullerene/sulphur
Fullerene C in cadmium nano composite photo-catalyst60Uniform fold can effectively derive light induced electron on CdS nanocrystal surface
Promote the carrying out of light-catalyzed reaction, improve the photocatalytic activity of cadmium sulfide；Simultaneously as fullerene C60Excellent electron affinity
The separating rate of photo-generated carrier in cadmium sulfide can be effectively improved, so as to further enhance its cyclical stability.
Compared with prior art, the present invention has following clear advantage：
1) fullerene/cadmium sulfide nano composite photo-catalyst excellent performance in actual applications in the present invention, compared with bright sulfur
Greatly improved in terms of photocatalytic activity and cyclical stability for cadmium.
2) there is the fullerene/cadmium sulfide nano composite photo-catalyst in the present invention fullerene to coat CdS nanocrystal
Special construction, is advantageous to the separation in light induced electron and hole in light-catalyzed reaction, can effectively improve photochemical catalyst
Photocatalytic activity.
3) present invention uses hydro-thermal method, and a step is obtained fullerene/cadmium sulfide nano composite photo-catalyst, with preparation technology
Simple advantage.
Brief description of the drawings
Fig. 1 is C in the embodiment of the present invention 1~460/ CdS nano composite photo-catalysts and pure fullerene C60With pure CdS's
X-ray diffractogram；
Fig. 2 is C in the embodiment of the present invention 160The transmission electron microscope photo of/CdS nano composite photo-catalysts；
Fig. 3 is C in the embodiment of the present invention 160The high power transmission electron microscope photo of/CdS nano composite photo-catalysts；
Fig. 4 is C in the embodiment of the present invention 1~460The Photocatalyzed Hydrogen Production speed of/CdS nano composite photo-catalysts and pure CdS
Comparison diagram；0.4C in figure60/CdS、0.8C60/CdS、4C60/CdS、8C60/ CdS represent respectively embodiment 1 in the present invention, 2,3,
The product prepared in 4；
Fig. 5 is C in the embodiment of the present invention 160The Photocatalyzed Hydrogen Production cyclical stability figure of/CdS nano composite photo-catalysts.
Fig. 6 is C in the embodiment of the present invention 1~460The photocatalysis of/CdS nano composite photo-catalysts and pure CdS to rhodamine B
Degradation efficiency comparison chart；
0.4C in Fig. 660/CdS、0.8C60/CdS、4C60/CdS、8C60/ CdS represent respectively embodiment 1 in the present invention, 2,
3rd, the product prepared in 4；
Fig. 7 is C in the embodiment of the present invention 160The photocatalytic degradation circulation of/CdS nano composite photo-catalysts to rhodamine B is steady
Qualitative figure.
Specific embodiment
The present invention is raw materials used to be chemically pure reagent, and specific embodiment is as follows；
Embodiment 1
(1) 1.33g Cadmium diacetate dihydrates and 1.22g Cys are added in 20ml deionized waters, with 400r/
The fullerene C of 3mg is added after min stirrings 1h60, continue to stir 0.5h with 400r/min, obtain fullerene C60Dispersed is mixed
Close solution.
(2) mixed solution obtained in step (1) is transferred in 30ml ptfe autoclaves, baking oven is put into after sealing
In in 200 DEG C of hydro-thermal reaction 10h.
(3) hydrothermal product is alternately washed using deionized water and ethanol, is repeated 6 times to go the removal of impurity, 70 DEG C of vacuum are done
C is obtained after dry 10h60/ CdS nano composite photo-catalysts.
Fig. 1 is C prepared in embodiment 160/ CdS nano composite photo-catalysts and pure CdS is nanocrystalline and fullerene
C60XRD spectrum, it can be seen that prepared product is by hexagonal phase CdS and Emission in Cubic fullerene C60Composition, wherein CdS
It is nanocrystalline with excellent crystallinity, fullerene C60Introducing do not influence the crystallinity of CdS.
Fig. 2 and Fig. 3 is the C of preparation in embodiment 160The transmission electron microscope photo and its high power of/CdS nano composite photo-catalysts
Transmission photo.Prepared product has polygonized structure as can see from Figure 2, and its size range is 30~80nm.From Fig. 3
In it can be seen that have one layer of uniform amorphous layer (at dotted line) in single CdS nanocrystal surfaces, thickness is about 1nm, is to adsorb
In the fullerene C on its surface60Molecule, illustrates there is preferable interface binding power therebetween.
Be further demonstrate by above-mentioned sign collection of illustrative plates, C can be obtained using preparation method provided by the present invention60/ CdS receives
Rice composite photo-catalyst.
The C that will be prepared in the present embodiment 160/ CdS nano composite photo-catalysts are applied in Photocatalyzed Hydrogen Production reaction.Specifically
Experimental technique is as follows：
The C that will be prepared in 25mg embodiments 160/ CdS nano composite photo-catalysts ultrasonic disperse is in 50ml lactic acid aqueous solutions
In (comprising 45ml deionized waters and 5ml lactic acid), then suspension is transferred in Pyrex glass three-neck flask, added
The platinum acid chloride solution of 0.08mL 0.1M, by photoreduction met hod catalyst surface in-situ deposition 1wt% Pt co-catalysts.So
Lead to argon gas 30 minutes afterwards by air emptying in bottle.Then, under conditions of closing and stirring, (300W xenon lamps are carried to open light source
420nm optical filters), hydrogen content in reaction system was detected with gas chromatograph every 30 minutes, then calculate average product hydrogen speed
Rate, is per hour measurement unit with mM every gram.The C that will be prepared in the present embodiment 160/ CdS nano composite photo-catalyst applications
In Photocatalyzed Hydrogen Production reaction, its hydrogen-producing speed and cycle stability are shown in Fig. 4 and Fig. 5 respectively.Be can see from the two figures,
As fullerene C60C when content is the 0.4% of cadmium sulfide quality60/ CdS nano composite photo-catalysts show excellent photocatalysis
Activity, its Photocatalyzed Hydrogen Production speed is 2.3 times of pure CdS, and the hydrogen-producing speed after being circulated by three times can still keep.
The C that will be prepared in the present embodiment 160/ CdS nano composite photo-catalysts are applied in photocatalytic degradation reaction.Specifically
Experimental technique is as follows：
The C that will be prepared in 20mg embodiments 160/ CdS nano composite photo-catalysts ultrasonic disperse is 10mg/L in 20ml concentration
Rhodamine B solution in, then suspension is transferred in quartz reactor, stir and secretly adsorb 30 minutes with reach absorption put down
Weighing apparatus.Light source (300W xenon lamps carry 420nm optical filters) is opened, solution was detected with ultraviolet-uisible spectrophotometer every 10 minutes
The absorbance of middle rhodamine B, so as to be calculated the disposal efficiency at each time point.The C that will be prepared in the present embodiment 160/
CdS nano composite photo-catalysts are applied in photocatalytic degradation reaction, and its degradation efficiency and cycle stability are shown in Fig. 6 and Tu respectively
7.Be can see from the two figures, the C prepared in embodiment 160/ CdS nano composite photo-catalysts were by the light of 40 minutes
Degradation efficiency according to after can reach 96.7%, and the degradation efficiency after being circulated by three times can still reach 94.6%, with non-
Often good cyclical stability.
Embodiment 2：
Specific preparation method is roughly the same with embodiment 1, and difference is fullerene C60Addition be changed into 6mg, so
C is obtained afterwards60/ CdS nano composite photo-catalysts.Prepared C in embodiment 260/ CdS nano composite photo-catalysts according to reality
Identical method tests its photocatalysis performance in applying example 1, its Photocatalyzed Hydrogen Production speed and photocatalytic degradation efficiency see respectively Fig. 4 and
Fig. 6.
Embodiment 3：
Specific preparation method is roughly the same with embodiment 1, and difference is fullerene C60Addition be changed into 30mg, so
C is obtained afterwards60/ CdS nano composite photo-catalysts.Prepared C in embodiment 360/ CdS nano composite photo-catalysts according to reality
Identical method tests its photocatalysis performance in applying example 1, its Photocatalyzed Hydrogen Production speed and photocatalytic degradation efficiency see respectively Fig. 4 and
Fig. 6.
Embodiment 4：
Specific preparation method is roughly the same with embodiment 1, and difference is fullerene C60Addition be changed into 60mg, so
C is obtained afterwards60/ CdS nano composite photo-catalysts.Prepared C in embodiment 460/ CdS nano composite photo-catalysts according to reality
Identical method tests its photocatalysis performance in applying example 1, its Photocatalyzed Hydrogen Production speed and photocatalytic degradation efficiency see respectively Fig. 4 and
Fig. 6.
In Fig. 4 and Fig. 6,0.4C60/CdS、0.8C60/CdS、4C60/CdS、8C60/ CdS is implemented in representing the present invention respectively
The product prepared in example 1,2,3,4.Be can see from Fig. 4 and Fig. 6, fullerene C60Modification improve CdS photocatalysis live
Property.As fullerene C60C when content is the 0.4% of CdS mass60/ CdS nano composite photo-catalysts show highest photocatalysis
Activity, its Photocatalyzed Hydrogen Production speed and rate of photocatalytic oxidation are respectively 2.3 times and 1.5 times of pure CdS.
The method of the embodiment of the present invention, is described by preferred embodiment, and person skilled substantially can be not
Depart from and methods and techniques described herein route is modified or reconfigured in present invention, spirit and scope, come real
Now final technology of preparing.In particular, all similar replacements and change for a person skilled in the art
It is it will be apparent that they are considered as being included in spirit of the invention, scope and content.
Claims (8)
1. a kind of fullerene/cadmium sulfide nano composite photo-catalyst, is fullerene C60Uniform fold is in CdS nanocrystal surface shapes
Into being expressed as C60/CdS；The fullerene C60It is 0.4~8 with the mass ratio of CdS:100.
2. a kind of fullerene/cadmium sulfide nano composite photo-catalyst according to claim 1, it is characterised in that the richness
Strangle alkene C60It is 0.4 with the mass ratio of CdS:100.
3. a kind of fullerene/cadmium sulfide nano composite photo-catalyst according to claim 1, it is characterised in that described multiple
The nanocrystalline sizes of CdS in condensation material are 30~80nm；Fullerene C60CdS nanocrystal surface is evenly coated at, its thickness 1
~3nm.
4. a kind of preparation method of fullerene/cadmium sulfide nano composite photo-catalyst of claim 1, straight by one step hydro thermal method
Preparation is connect, is comprised the following steps that：
(1) by Cadmium diacetate dihydrate and Cys addition deionized water, dispersed mixed solution is obtained after stirring；
Cadmium diacetate dihydrate and Cys and the mass ratio of deionized water are 1.33 in mixed solution:1.22~3.66:20~30；
(2) by fullerene C60It is added in mixed solution obtained in step (1), fullerene C is obtained after stirring60Dispersed is mixed
Solution is closed, hydro-thermal reaction is then carried out；Wherein fullerene C60It is with the mass ratio of cadmium sulfide generated in step (1) mixed solution
0.4~8:100.
(3) by the hydrothermal product of step (2), using deionized water and ethanol, alternately the removal of impurity is gone in washing, then by product vacuum
It is dried to obtain fullerene/cadmium sulfide nano composite photo-catalyst.
5. a kind of preparation method of fullerene/cadmium sulfide nano composite photo-catalyst according to claim 4, its feature exists
In the mixing speed of step (1) mixed solution is 300~400r/min, and mixing time is 1~2h.
6. a kind of preparation method of fullerene/cadmium sulfide nano composite photo-catalyst according to claim 4, its feature exists
In step (2) C containing fullerene60Mixed solution mixing speed be 300~400r/min, mixing time be 0.5~
1h。
7. a kind of preparation method of fullerene/cadmium sulfide nano composite photo-catalyst according to claim 4, its feature exists
In the temperature of step (3) hydro-thermal reaction is 160~220 DEG C, and hydro-thermal soaking time is 5~12h, is then naturally cooled to
Room temperature.
8. a kind of preparation method of fullerene/cadmium sulfide nano composite photo-catalyst according to claim 4, its feature exists
In the step (3) is alternately washed using deionized water and ethanol, is repeated 6~10 times；Vacuum drying temperature is 50~100 DEG C,
Vacuum drying time is 8~12h.
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| CN107983413A (en) * | 2017-12-12 | 2018-05-04 | 成都育芽科技有限公司 | A kind of fullerene composite photo-catalyst for environmental pollution improvement |
| CN111517372A (en) * | 2020-05-11 | 2020-08-11 | 山西医科大学 | Fullerene coated Fe3O4Composite nano material and preparation method thereof |
| CN113019397A (en) * | 2021-03-16 | 2021-06-25 | 南京信息工程大学 | Preparation method of photocatalyst |
| CN113926487A (en) * | 2021-09-14 | 2022-01-14 | 杭州师范大学 | Fullerol/palladium nano composite photocatalyst and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107983413A (en) * | 2017-12-12 | 2018-05-04 | 成都育芽科技有限公司 | A kind of fullerene composite photo-catalyst for environmental pollution improvement |
| CN107983413B (en) * | 2017-12-12 | 2020-12-04 | 金鹏飞 | Fullerene composite photocatalyst for environmental pollution treatment |
| CN111517372A (en) * | 2020-05-11 | 2020-08-11 | 山西医科大学 | Fullerene coated Fe3O4Composite nano material and preparation method thereof |
| CN113019397A (en) * | 2021-03-16 | 2021-06-25 | 南京信息工程大学 | Preparation method of photocatalyst |
| CN113926487A (en) * | 2021-09-14 | 2022-01-14 | 杭州师范大学 | Fullerol/palladium nano composite photocatalyst and preparation method and application thereof |
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