CN108607593A - Niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalyst of cadmium sulfide nano-particles modification and application - Google Patents
Niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalyst of cadmium sulfide nano-particles modification and application Download PDFInfo
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- CN108607593A CN108607593A CN201810388355.0A CN201810388355A CN108607593A CN 108607593 A CN108607593 A CN 108607593A CN 201810388355 A CN201810388355 A CN 201810388355A CN 108607593 A CN108607593 A CN 108607593A
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- niobium pentoxide
- nitrogen
- cadmium sulfide
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- doped graphene
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- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 66
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 title claims abstract description 63
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 title claims abstract description 58
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 50
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 230000004048 modification Effects 0.000 title claims abstract description 43
- 238000012986 modification Methods 0.000 title claims abstract description 43
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims description 32
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 28
- 239000001257 hydrogen Substances 0.000 claims description 28
- 229910052739 hydrogen Inorganic materials 0.000 claims description 28
- 230000001699 photocatalysis Effects 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 16
- 150000001875 compounds Chemical class 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 13
- 238000007146 photocatalysis Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 claims description 9
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 9
- 229910001868 water Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 claims description 6
- 239000012046 mixed solvent Substances 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- SGJUCMOYVKXLDY-UHFFFAOYSA-N acetic acid;cadmium Chemical compound [Cd].CC(O)=O.CC(O)=O SGJUCMOYVKXLDY-UHFFFAOYSA-N 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical class CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- 150000003384 small molecules Chemical group 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 11
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 description 17
- 239000000243 solution Substances 0.000 description 9
- 239000010955 niobium Substances 0.000 description 8
- 229910052758 niobium Inorganic materials 0.000 description 8
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 229910052724 xenon Inorganic materials 0.000 description 7
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 125000002353 D-glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 101100373011 Drosophila melanogaster wapl gene Proteins 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003483 aging Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000005915 ammonolysis reaction Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 210000004483 pasc Anatomy 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 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
- B01J27/24—Nitrogen compounds
-
- 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—
-
- 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
- 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
-
- 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
-
- 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 discloses a kind of niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalysts of cadmium sulfide nano-particles modification and application.With nitrogen-doped graphene for carrier and electron acceptor with multilevel hierarchy photochemical catalyst, the niobium pentoxide nano stick of cadmium sulfide nano-particles modification is that the light of photochemical catalyst captures body and electron transit mediator, the catalyst has many advantages, such as that photoresponse range is wide, catalytic activity is high, stability is good, catalytic reaction condition is simple, and service life is long.
Description
The invention belongs to niobium pentoxide nano stick/nitrogen-doped graphenes of entitled cadmium sulfide nano-particles modification
Composite photo-catalyst, preparation method and application are patent on January 26th, 2016 application No. is the 201610050573.4, applying date
The divisional application of application belongs to product and its application obscure portions.
Technical field
The present invention relates to a kind of novel semi-conductor-graphenes preparing hydrogen for catalytic decomposition water reaction under visible light
Composite photo-catalyst, and in particular to a kind of niobium pentoxide nano stick/nitrogen-doped graphene of cadmium sulfide nano-particles modification is multiple
Closing light catalyst and photocatalysis hydrogen production application.
Background technology
Hydrogen Energy have the characteristics that cleaning, it is efficient, environmental-friendly, be a kind of ideal secondary energy sources.Currently, large-scale industrial
The main method of hydrogen manufacturing has water-gas, electrolysis water, ammonolysis craft method, active metal to be reacted with acid, highly basic and aluminium or pasc reaction, methanol
The methods of cracking process.Conventional hydrogen preparation method has the characteristics that technical maturity, simple.But severe reaction conditions set production
It is standby to require height, and need to consume mass energy, production cost is higher.Certain methods have waste water, waste residue to generate, and have centainly to environment
It influences.In addition, only converting fossil energy to Hydrogen Energy using fossil fuel hydrogen manufacturing, energy shortage can not be solved and environment is dirty
Dye problem.
Photocatalytic hydrogen production by water decomposition method has shown that wide application prospect in terms of solving environmental pollution and energy crisis,
By the common concern of domestic and international researcher.Photochemical catalyzing hydrogen making be convert solar energy into it is storable, at any time
The optimal path of available chemical energy.Photocatalytic hydrogen production by water decomposition has reaction condition mild, and non-secondary pollution, equipment is simple,
The advantages that small investment.It is that sunlight, semiconductor valence band are absorbed by catalyst using semiconductor as catalyst photolysis water hydrogen principle
Electronics is excited to conduction band, and the effect of conduction band electron water occurs reduction reaction, generates hydrogen；Hole in semiconductor valence band then with water
Oxidation reaction occurs, generates oxygen.Therefore, suitable photochemical catalyzing catalyst should have it is appropriate lead, valence band location（It leads
Band current potential should be than hydrogen electrode current potential E (H+/H2) slightly negative, and valence band current potential then should be than oxygen electrode current potential E (O2/H2O) slightly just）.Except this
Except, photolytic hydrogen production catalyst also needs to meet band gap appropriate（Sunlight can be absorbed）, high stability, do not generate light corruption
Erosion, the conditions such as cheap.
Niobium based photocatalyst has that stability is good, the characteristics such as nontoxic, is that a kind of great semiconductor light for having development potentiality is urged
Agent.But due to Nb2O5Energy band greater band gap (~ 3.1 eV), it is low to the utilization rate of sunlight.Meanwhile light induced electron and photoproduction
Hole is easy to compound, and quantum efficiency is relatively low, thus its photocatalytic activity is relatively low.By partly leading for niobium base semiconductor and other narrow band gaps
Bluk recombination, which forms heterojunction structure, can expand its photoresponse range, reduce compound, the Jin Erti of light induced electron and electron hole
Highlight catalytic active.
Invention content
The present invention provides a kind of niobium pentoxide nano stick/nitrogen-doped graphene of cadmium sulfide nano-particles modification is compound
The preparation method of photochemical catalyst.With nitrogen-doped graphene for carrier and electron acceptor with multilevel hierarchy photochemical catalyst, sulphur
The niobium pentoxide nano stick of cadmium Nanoparticle Modified is that the light of photochemical catalyst captures body and electron transit mediator, catalyst tool
There is the advantages that photoresponse range is wide, catalytic activity is high, stability is good, catalytic reaction condition is simple, and service life is long.
To achieve the above object of the invention, the technical solution adopted by the present invention is：The five of a kind of cadmium sulfide nano-particles modification
The preparation method for aoxidizing two niobium nanometer rods/nitrogen-doped graphene composite photo-catalyst, includes the following steps：
（1）Niobium pentoxide nano stick（NbR）Preparation
Niobium pentoxide nano stick is synthesized using the method for hydro-thermal.
By niobic acid ultrasonic disperse in the mixed solvent, mixed liquor is stirred to get；Then mixed liquor is put into polytetrafluoro inner sleeve
In autoclave, after 100~200 DEG C are aged 20~40 hours, consolidated successively through suction filtration, deionized water washing, drying
Body；Then by solid in Muffle furnace, with the rate of 5~20 DEG C/min by room temperature to 400~700 DEG C, then heat preservation roasting
It is down to room temperature naturally after burning 2~10 hours, NbR is made；
（2）The niobium pentoxide nano stick composite semiconductor of cadmium sulfide nano-particles modification（NbR/CdS）Preparation
Niobium pentoxide nano stick is dispersed in alcohols solvent, after ultrasonic disperse, cadmium ion agent for capturing is added；It is then refluxed for anti-
It answers 2~5 hours postcoolings to room temperature, then acetic acid cadmium solution is added dropwise, stir 50~75 minutes；Then Na is added2S solution；Stirring
After 50~75 minutes, mixture is obtained；Mixture is placed in polytetrafluoro inner sleeve autoclave, is reacted at 150~200 DEG C
20~30 hours；Then reaction solution successively through filter, deionized water washing, dry cadmium sulfide nano-particles modification five oxidations
Two niobium nanometer rods（NbR/CdS）；
（3）Niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalyst of cadmium sulfide nano-particles modification（NbR/CdS/
NGR）Preparation
The niobium pentoxide nano stick NbR/CdS and N doping stone for the cadmium sulfide nano-particles modification that above-mentioned steps are prepared
Ultrasonic reaction 1~3 hour after black alkene suspension and deionized water mixing；It is then centrifuged for handling, obtained solid is through deionized water
After washing, drying, niobium pentoxide nano stick/nitrogen-doped graphene composite photocatalyst of cadmium sulfide nano-particles modification is obtained
Agent；The niobium pentoxide nano stick of the cadmium sulfide nano-particles modification, the matter of nitrogen-doped graphene suspension and deionized water
Amount is than being 1: 0.01-0.06: 30-50.
In above-mentioned technical proposal, step（1）In, the mass ratio of niobic acid and mixed solvent is 1: 50~3000；Mixed solvent
For the mixture of ethyl alcohol and water；The volume ratio of ethyl alcohol and water is preferably 1: 1；Mixing time is 20~50 minutes；In Muffle furnace, rise
Warm rate is 10 DEG C/min, and roasting time is 5 hours.The present invention has reaction can be in height using polytetrafluoro inner sleeve autoclave
It is carried out under temperature, high pressure（When with aqueous medium, reaction pressure is up to 2.1MPa）, but not introduce impurity.Accurately control heating rate
The perfect NbR of crystal form can be obtained with roasting time.
In above-mentioned technical proposal, step（2）In, the alcohols solvent be small molecule alcohol solvent, as methanol, isopropanol,
Ethyl alcohol, propyl alcohol etc., preferred alcohol；The time of ultrasonic disperse is 50~75 minutes, preferably 60 minutes；The cadmium ion agent for capturing is
3- aminopropyl triethoxysilanes（APTES）, it is D-Glucose, one or more in polyethylene glycol, polyethylene glycol is preferably poly-
Ethylene glycol 400；Reflux time is 3 hours；A concentration of 4 mg/mL of acetic acid cadmium solution；Na2A concentration of the 25 of S solution
mg/mL；Mixture is placed in polytetrafluoro inner sleeve autoclave, is reacted 20~25 hours at 160~180 DEG C；Drying condition
It is dried in vacuo for 70~80 DEG C.
In above-mentioned technical proposal, step（2）In, the niobium pentoxide nano stick, cadmium ion agent for capturing, cadmium acetate,
Na2The molar ratio of S is（1.5~2）∶（4~4.5）∶（0.5~1）∶（0.8~1.2）.
In above-mentioned technical proposal, step（3）In, the N doping amount of nitrogen-doped graphene is 1~5 atm%；N doping graphite
A concentration of 0.1 mg/mL of alkene suspension；The ultrasonic reaction time is 1.5~2.5 hours；Centrifugal treating technique is 1800~2200
Rev/min, centrifugation time are 25~40 minutes；Drying condition is to be dried in vacuo at 70~80 DEG C.
In the present invention, after reaction, reaction solution obtains filter cake, filter cake heats baking after deionized water by filtering
It is dry, to obtain corresponding solid product.
The present invention further discloses the niobium pentaoxides of the cadmium sulfide nano-particles prepared according to the above method modification to receive
Rice stick/nitrogen-doped graphene composite photo-catalyst；Wherein a length of 0.5~1.0 μm of niobium pentoxide nano stick, a diameter of 90~
130 nm；The grain size of cadmium sulfide is 5~20 nm.Niobium pentoxide nano stick with suitable draw ratio, is conducive to light induced electron
Orientation transmit, it is possible to reduce the probability of recombination of light induced electron and hole, improve light quantum utilization ratio.Meanwhile cadmium sulfide with
NbR compound tenses with suitable draw ratio, the CdS nano particle diameters generated on NbR are moderate, are evenly distributed on NbR, thus
The features such as composite semiconductor material photocatalytic activity is higher.
The composite catalyst of the present invention not only has very high photocatalytic activity under ultraviolet-visible light irradiation, visible
Also there is preferable activity under light irradiation；And stability is good, and higher photocatalytic activity can be still kept after reacting for a long time；Cause
The present invention further discloses niobium pentoxide nano stick/nitrogen-doped graphene that above-mentioned cadmium sulfide nano-particles are modified is compound for this
Application of the photochemical catalyst in photocatalysis hydrogen production；Further, the niobium pentaoxide of cadmium sulfide nano-particles of the invention modification
Nanometer rods/nitrogen-doped graphene composite photo-catalyst at normal temperatures and pressures, photocatalysis hydrogen production reaction can be carried out under visible light.
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
1）The present invention successfully solves the problems, such as that existing niobium pentaoxide activity itself is low, can effectively expand niobium pentaoxide
Photoresponse range, not only ultraviolet-visible light irradiation under have very high photocatalytic activity, under visible light illumination also have compared with
Good activity.
2）The present invention is compound with niobium pentaoxide by cadmium sulfide, compound is partly led to combine to be formed compared with low band gap and high band gap
Body changes Nb2O5Structure extends the absorption region to incident light, can make full use of visible light, improve its photocatalytic activity,
To improve photoresponse range and photocatalysis performance.
3）The present invention changes simultaneously semiconductor topography, and semiconductor is prepared into nano bar-shape structure, can not only obtain ratio
The catalysis material that surface area is big and crystallinity is high, and light induced electron and electron hole can be reduced in the photocatalytic process
It is compound, effectively improve photocatalytic activity.
4）In composite photo-catalyst disclosed by the invention, graphene has larger specific surface area, can be used as catalyst
Excellent carrier, by semiconductor light-catalyst and graphene it is compound after, the good electric conductivity of graphene is conducive to light induced electron and sky
Cave detaches in time, can further increase the photocatalytic activity of catalyst.
5）Preparation method disclosed by the invention is simple, and obtained composite catalyst stability is good, long-time light-catalyzed reaction
Higher catalytic activity can be still kept afterwards.
6）Niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalyst of cadmium sulfide nano-particles modification of the present invention
Catalyzing manufacturing of hydrogen condition requires that simply, catalyzing manufacturing of hydrogen reaction can be carried out at normal temperatures and pressures, has higher urge under visible light
Change activity.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of niobium pentoxide nano stick in embodiment one；
Fig. 2 is the scanning electron microscope (SEM) photograph for the niobium pentoxide nano stick that cadmium sulfide nano-particles are modified in embodiment one；
Fig. 3 is that niobium pentoxide nano stick/nitrogen-doped graphene complex light that cadmium sulfide nano-particles are modified in embodiment one is urged
The scanning electron microscope (SEM) photograph of agent.
Specific implementation mode
Embodiment one
1）Niobium pentoxide nano stick（NbR）Preparation
The niobic acid ultrasonic disperse of 0.5 g is weighed to 200 mL ethyl alcohol/deionized water (1:1) in, 30 min of stirring obtain mixed liquor；
Gained mixed liquor is put into band polytetrafluoro inner sleeve autoclave after 180 DEG C are aged 38 hours, through filtering, deionization washing
It washs, dries.Obtained solid is warming up to 600 DEG C in Muffle furnace with the rate of 10 DEG C/min, and room is down to naturally after being kept for 5 hours
NbR is made in temperature；
2）The niobium pentoxide nano stick composite semiconductor of cadmium sulfide nano-particles modification（NbR/CdS）Preparation
It weighs 0.5 g NbR to be dispersed in 100 mL absolute ethyl alcohols, the 3- ammonia of 4.2 mmol is added after 1.0 hours in ultrasonic agitation
Propyl-triethoxysilicane（APTES）As Cd ion capturing agents, flows back 3.0 hours in 70 DEG C, be slowly added to after being cooled to room temperature
35 mL cadmium acetates (4 mg mL-1) solution, it stirs 1.0 hours, adds 3 mL Na2S solution (25 mg mL-1).Stirring
After reaction 1.0 hours, gained mixed liquor is placed in band polytetrafluoro inner sleeve autoclave and is reacted 24 hours in 180 DEG C.It is down to
It after room temperature, filters, obtained solid obtains five oxidations of cadmium sulfide nano-particles modification through deionized water washing, 70 DEG C of vacuum drying
Two niobium nanometer rods composite semiconductors（NbR/CdS）；
3）Niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalyst of cadmium sulfide nano-particles modification（NbR/CdS/
NGR）Preparation
NbR/CdS composite semiconductors, the NGR that above-mentioned steps are prepared（0.1 mg mL-1, 5 atm% of N doping amount）It suspends
Liquid and deionized water in mass ratio 1:0.02:After the mixing of 40 ratios, after being handled 2 hours using ultrasonic wave added in-situ reaction, from
The heart, obtained solid are washed through deionized water, are dried in vacuo at 70 DEG C, and five oxidations two of product cadmium sulfide nano-particles modification are obtained
Niobium nanometer rods/nitrogen-doped graphene composite photo-catalyst.
Attached drawing 1 is the scanning electron microscope (SEM) photograph of above-mentioned niobium pentoxide nano stick；Niobium pentoxide nano stick is about 0.5-1.0 μ
M, about 100 nm of stick diameter.
Attached drawing 2 is the scanning electron microscope (SEM) photograph of the niobium pentaoxide composite semiconductor of above-mentioned cadmium sulfide nano-particles modification；Five oxygen
Change two niobium nanometer rods and is about 0.5-1.0 μm, about 110 nm of stick diameter；Cadmium sulfide nano-particles are evenly distributed in five oxidations two
In niobium nanometer rods, grain size is about 10 nm.
Attached drawing 3 is that niobium pentoxide nano stick/nitrogen-doped graphene complex light of above-mentioned cadmium sulfide nano-particles modification is urged
The scanning electron microscope (SEM) photograph of agent, cadmium sulfide/niobium pentoxide nano stick are evenly distributed on nitrogen-doped graphene surface.
4）Photochemical catalyzing is reacted
The above-mentioned catalyst of 0.25 mg and 70 mL contain 0.35 M Na2S and 0.25 M Na2SO3Aqueous solution mixing, ultrasound stirs
After mixing 0.5 hour, it is added into photo catalysis reactor.It it is 25 DEG C in reaction temperature, it is seen that light（150 W xenon lamps, λ>400 nm）
The lower catalysis reaction of irradiation 8 hours, hydrogen output is 800 μm of ol g-1。
Embodiment two
By in embodiment one, step（1）180 DEG C of ageings are changed to 150 DEG C for 38 hours and are aged 30 hours, step（2）In band polytetrafluoro
It is changed in polytetrafluoro inner sleeve autoclave within 24 hours in 180 DEG C of reactions in inner sleeve autoclave, reacts 20 at 160 DEG C
Hour；Obtain niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalyst of product cadmium sulfide nano-particles modification.
The above-mentioned catalyst of 0.25 mg and 70 mL contain 0.35 M Na2S and 0.25 M Na2SO3Aqueous solution mixing, surpass
After sound stirs 0.5 hour, it is added into photo catalysis reactor.It it is 25 DEG C in reaction temperature, in visible light（150 W xenon lamps, λ>
400 nm）The lower catalysis reaction of irradiation 8 hours, hydrogen output is 605 μm of ol g-1。
Embodiment three
Niobium pentoxide nano stick（NbR）, cadmium sulfide nano-particles modification niobium pentoxide nano stick composite semiconductor（NbR/
CdS）Preparation method it is identical as embodiment one.But when preparing composite semiconductor catalyst, NbR/CdS composite semiconductors, nitrogen
Doped graphene NGR suspension（0.1 mg mL-1, 5 atm% of N doping amount）With deionized water in mass ratio 1:0.01:40 ratio
Example mixing, preparation process and condition are identical as embodiment one, and the niobium pentaoxide for obtaining the modification of product cadmium sulfide nano-particles is received
Rice stick/nitrogen-doped graphene composite photo-catalyst.
The above-mentioned catalyst of 0.25 mg and 70 mL contain 0.35 M Na2S and 0.25 M Na2SO3Aqueous solution mixing, surpass
After sound stirs 0.5 hour, it is added into photo catalysis reactor.It it is 25 DEG C in reaction temperature, in visible light（150 W xenon lamps, λ>
400 nm）The lower catalysis reaction of irradiation 8 hours, hydrogen output is 550 μm of ol g-1。
Example IV
The mass ratio of NbR and CdS in one second step of embodiment is changed to 1:0.1, obtain the modification of product cadmium sulfide nano-particles
Niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalyst.
The above-mentioned catalyst of 0.25 mg and 70 mL contain 0.35 M Na2S and 0.25 M Na2SO3Aqueous solution mixing, surpass
After sound stirs 0.5 hour, it is added into photo catalysis reactor.It it is 25 DEG C in reaction temperature, in visible light（150 W xenon lamps, λ>
400 nm）The lower catalysis reaction of irradiation 8 hours, hydrogen output is 495 μm of ol g-1。
Embodiment five
Cd ion capturing agents in one second step of embodiment are changed to D-Glucose, the mass ratio of NbR and CdS are changed to 1:0.3, other
Preparation condition is identical as embodiment one, obtains niobium pentoxide nano stick/N doping stone of product cadmium sulfide nano-particles modification
Black alkene composite photo-catalyst.
The above-mentioned catalyst of 0.25 mg and 70 mL contain 0.35 M Na2S and 0.25 M Na2SO3Aqueous solution mixing, surpass
After sound stirs 0.5 hour, it is added into photo catalysis reactor.It it is 25 DEG C in reaction temperature, in visible light（150 W xenon lamps, λ>
400 nm）The lower catalysis reaction of irradiation 8 hours, hydrogen output is 521 μm of ol g-1。
Embodiment six
Using the niobium pentoxide nano stick/nitrogen-doped graphene complex light for the cadmium sulfide nano-particles modification that embodiment one obtains
Catalyst.0.25 mg catalyst and 70 mL contain 0.35 M Na2S and 0.25 M Na2SO3Aqueous solution mixing, ultrasonic agitation
After 0.5 hour, it is added into photo catalysis reactor.It it is 25 DEG C in reaction temperature, in visible light（150 W xenon lamps, λ>400 nm）
The lower catalysis reaction of irradiation 8 hours, recycles 5 times, hydrogen output is respectively 800,810,795,790,795 μm of ol g-1.It is flat
Equal hydrogen output is 798 μm of ol g-1。
Embodiment seven
Using the niobium pentoxide nano stick/nitrogen-doped graphene complex light for the cadmium sulfide nano-particles modification that embodiment one obtains
Catalyst.The above-mentioned catalyst of 0.25 mg and 70 mL contain 0.35 M Na2S and 0.25 M Na2SO3Aqueous solution mixing, ultrasound
After stirring 0.5 hour, it is added into photo catalysis reactor.It it is 25 DEG C in reaction temperature, in ultraviolet-visible light（150 W xenon lamps）
The lower catalysis reaction of irradiation 8 hours, hydrogen output is 1576 μm of ol g-1。
As can be seen from the above embodiments, the niobium pentoxide nano for the cadmium sulfide nano-particles modification that prepared by the present invention
Stick/nitrogen-doped graphene composite photo-catalyst not only has higher photocatalytic activity under action of ultraviolet light；And visible
Under light action, it may have preferable photocatalytic activity；And the catalyst circulation stability of the present invention is good, after five cycles still
With higher photocatalytic activity；Catalyst preparation process of the present invention is simple, reasonable simultaneously, and application conditions are simple, is suitable for work
Industry metaplasia is produced.
Claims (9)
1. a kind of niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalyst of cadmium sulfide nano-particles modification, special
Sign is, the system of niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalyst of the cadmium sulfide nano-particles modification
Preparation Method includes the following steps：
（1）By niobic acid ultrasonic disperse in the mixed solvent, mixed liquor is stirred to get；Then it is high mixed liquor to be put into polytetrafluoro inner sleeve
It presses in reaction kettle, after 100~200 DEG C are aged 20~40 hours, obtains solid through suction filtration, deionized water washing, drying successively；
Then by solid in Muffle furnace, with the rate of 5~20 DEG C/min by room temperature to 400~700 DEG C, then heat preservation roasting 2
It is down to room temperature naturally after~10 hours, niobium pentoxide nano stick is made；
（2）Niobium pentoxide nano stick is dispersed in alcohols solvent, after ultrasonic disperse, is flowed back instead after cadmium ion agent for capturing is added
It answers 2~5 hours, is cooled to room temperature, acetic acid cadmium solution is added, stir 50~75 minutes；Then Na is added2S solution；Stirring 50~
It is placed within 75 minutes in polytetrafluoro inner sleeve autoclave, is reacted 20~30 hours at 150~200 DEG C；Then reaction solution according to
It is secondary through filter, deionized water washing, dry cadmium sulfide nano-particles modification niobium pentoxide nano stick；
（3）By step（2）The niobium pentoxide nano stick and nitrogen-doped graphene for the cadmium sulfide nano-particles modification being prepared
Room temperature ultrasonic reaction 1~3 hour after suspension and deionized water mixing；It is then centrifuged for handling, obtained solid is through deionized water
After washing, drying, niobium pentoxide nano stick/nitrogen-doped graphene composite photocatalyst of cadmium sulfide nano-particles modification is obtained
Agent；The niobium pentoxide nano stick of the cadmium sulfide nano-particles modification, the matter of nitrogen-doped graphene suspension and deionized water
Amount is than being 1: 0.01~0.06: 30~50.
2. niobium pentoxide nano stick/nitrogen-doped graphene of cadmium sulfide nano-particles modification is compound according to claim 1
Photochemical catalyst, it is characterised in that：Step（1）In, the mass ratio of niobic acid and mixed solvent is 1: 50~3000；Mixed solvent is second
The mixture of alcohol and water；Mixing time is 20~50 minutes；In Muffle furnace, heating rate is 10 DEG C/min, and roasting time is 5 small
When.
3. niobium pentoxide nano stick/nitrogen-doped graphene of cadmium sulfide nano-particles modification is compound according to claim 1
Photochemical catalyst, it is characterised in that：Step（2）In, the alcohols solvent is small molecule alcohol solvent；The time of ultrasonic disperse is 50
~75 minutes；The cadmium ion agent for capturing is 3- aminopropyl triethoxysilanes, D-Glucose, one kind in polyethylene glycol or more
Kind；Reflux time is 3 hours；A concentration of 4 mg/mL of acetic acid cadmium solution；Na2A concentration of 25 mg/mL of S solution；It is mixed
It closes object to be placed in polytetrafluoro inner sleeve autoclave, be reacted 20~25 hours at 160~180 DEG C；Drying condition is 70~80
DEG C vacuum drying.
4. niobium pentoxide nano stick/nitrogen-doped graphene of cadmium sulfide nano-particles modification is compound according to claim 3
Photochemical catalyst, it is characterised in that：Step（2）In, the alcohols solvent is methanol, isopropanol, ethyl alcohol or propyl alcohol；Ultrasonic disperse
1 hour time；The polyethylene glycol is polyethylene glycol 400.
5. niobium pentoxide nano stick/nitrogen-doped graphene of cadmium sulfide nano-particles modification is compound according to claim 1
Photochemical catalyst, it is characterised in that：Step（2）In, the niobium pentoxide nano stick, cadmium ion agent for capturing, cadmium acetate, Na2S's
Molar ratio is（1.5~2）∶（4~4.5）∶（0.5~1）∶（0.8~1.2）.
6. niobium pentoxide nano stick/nitrogen-doped graphene of cadmium sulfide nano-particles modification is compound according to claim 1
Photochemical catalyst, it is characterised in that：Step（3）In, the N doping amount of nitrogen-doped graphene is 1~5 atm%；Nitrogen-doped graphene
A concentration of 0.1 mg/mL of suspension；The ultrasonic reaction time is 1.5~2.5 hours；Centrifugal treating technique is 1800~2200
Rev/min, centrifugation time are 25~40 minutes；Drying condition is to be dried in vacuo at 70~80 DEG C.
7. niobium pentoxide nano stick/nitrogen-doped graphene of cadmium sulfide nano-particles modification is compound according to claim 1
Photochemical catalyst, it is characterised in that：A length of 0.5~1.0 μm of niobium pentoxide nano stick, a diameter of 90~130 nm；Cadmium sulfide
Grain size is 5~20 nm.
8. niobium pentoxide nano stick/nitrogen-doped graphene complex light that cadmium sulfide nano-particles described in claim 1 are modified is urged
Application of the agent in photocatalysis hydrogen production.
9. application according to claim 8, it is characterised in that：Photocatalysis hydrogen production carries out under normal temperature and pressure, visible light.
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