CN105688948A - Photocatalyst and preparing method and application thereof - Google Patents
Photocatalyst and preparing method and application thereof Download PDFInfo
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- CN105688948A CN105688948A CN201511007973.9A CN201511007973A CN105688948A CN 105688948 A CN105688948 A CN 105688948A CN 201511007973 A CN201511007973 A CN 201511007973A CN 105688948 A CN105688948 A CN 105688948A
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- bioi
- bivo
- photocatalyst
- bivo4
- heterojunction composite
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title abstract description 14
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 67
- 239000002131 composite material Substances 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000746 purification Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 28
- 238000002360 preparation method Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 14
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 230000000844 anti-bacterial effect Effects 0.000 claims description 7
- 230000015556 catabolic process Effects 0.000 claims description 6
- 238000006731 degradation reaction Methods 0.000 claims description 6
- 229910003206 NH4VO3 Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 18
- 238000007146 photocatalysis Methods 0.000 abstract description 9
- 238000000975 co-precipitation Methods 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000005215 recombination Methods 0.000 abstract description 4
- 230000006798 recombination Effects 0.000 abstract description 4
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 230000004044 response Effects 0.000 abstract description 2
- 230000002265 prevention Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 33
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 16
- 229960000907 methylthioninium chloride Drugs 0.000 description 16
- 238000002474 experimental method Methods 0.000 description 14
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 9
- 230000001954 sterilising effect Effects 0.000 description 9
- 238000006555 catalytic reaction Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 244000005700 microbiome Species 0.000 description 8
- 229910021642 ultra pure water Inorganic materials 0.000 description 8
- 239000012498 ultrapure water Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- OCLXJTCGWSSVOE-UHFFFAOYSA-N ethanol etoh Chemical compound CCO.CCO OCLXJTCGWSSVOE-UHFFFAOYSA-N 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- 229910052724 xenon Inorganic materials 0.000 description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 6
- 230000001580 bacterial effect Effects 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000001963 growth medium Substances 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 230000004083 survival effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- -1 Methylene Chemical group 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000013207 serial dilution Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
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- B01J35/39—
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/10—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
- A62D3/17—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
-
- 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
- B01J27/06—Halogens; Compounds thereof
-
- 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
- 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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/26—Organic substances containing nitrogen or phosphorus
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/28—Organic substances containing oxygen, sulfur, selenium or tellurium, i.e. chalcogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention belongs to the field of photocatalysis, and particularly relates to a BiOI/BiVO4 heterojunction composite photocatalyst and a preparing method and application thereof. The BiOI/BiVO4 heterojunction composite photocatalyst is composed of BiOI and BiVO4, and the molar ratio of BiOI to BiVO4 is (1:18)-(18:1). According to the preparing method, the BiOI/BiVO4 heterojunction composite photocatalyst is obtained with the coprecipitation method under the hydrothermal condition. The preparing process is simple and easy to control, cost is low, a BiOI/BiVO4 heterojunction structure capable of achieving visible-light response is built, photo-induced carrier separation is accelerated, the recombination probability of photo-induced electron-hole pairs is reduced, photocatalytic activity and stability are high under visible light, and the BiOI/BiVO4 heterojunction composite photocatalyst can efficiently kill and degrade harmful organisms and dye pollutants in water and has high practical value and broad potential application prospects in the fields such as water purification and marine pollutant prevention.
Description
Technical field
The invention belongs to photocatalysis field, be specifically related to a kind of photocatalyst and its preparation method and application。
Background technology
Sustainable development is a global problem。But, the problem such as environmental pollution particularly water pollution is day by day serious。Various noxious pollutants accumulation not only heavy damage ecological balance in the environment such as water body, soil and air, also endangers the life of the mankind with healthy。It addition, economic development needs to consume the substantial amounts of energy, causing new energy crisis, and substantial amounts of exploitation and the use tradition mineral products energy inherently can cause serious environmental problem。
Photocatalitic Technique of Semiconductor is a kind of technology utilizing luminous energy to carry out Substance Transformation, reports TiO from Japanese Scientists Fujishima and Honda in 19722Since ultraviolet light photocatalytic water can be utilized to produce hydrogen and oxygen, Photocatalitic Technique of Semiconductor begins to have been a great concern[1]。Current Photocatalitic Technique of Semiconductor is obtained for extensive use in the fields such as degerming and sewage disposal of keeping a public place clean of indoor air purification, public place。At present, TiO2Because there is the advantage such as stable chemical nature, nontoxic, low cost become most widely used catalysis material, but due to TiO2There is also as high in photo-generate electron-hole recombination rate, the utilization rate of visible ray is low and reclaim the defects such as difficulty so that it is range of application receives very big restriction[2]。Therefore, exploitation can effectively utilize solar energy, and the new and effective catalysis material of environmental protection has important practical significance。
Bismuth based material has good absorbing properties because of it in visible ray (λ > 420nm) district, and its pattern has multiformity and gets the attention and further investigate。The composites that bismuth and other metals are formed has good visible light catalytic performance[3-6]。Such as BiOX (BiOX (X=Cl, Br, I)), it generally has cubic crystalline structure, is by [Bi2O2] lamella and the alternately arranged formation of two-layer halogens laminar structured, wherein BiOI is because having minimum energy gap (about 1.80eV) and having in visible region and well absorb and receive extensive concern[3]。Additionally, BiVO4It it is a kind of n-type direct semiconductor material, there is narrower energy gap (about 2.4eV), visible ray according under there is higher catalysis activity, in the depollution of environment and new energy development field, there is potential using value, become one of widely studied at present photocatalyst[4]。But owing in monomer photocatalyst, photoelectron-hole separates slower, the easy compound of photo-generated carrier, cause that the photocatalysis performance of semi-conducting material is limited, and build composite by semiconductors coupling and can accelerate electron-hole separation, improve the photocatalysis performance of material[5,6]。Therefore, it is badly in need of developing synthesizing new composite catalyst in photocatalysis field。
[1]K.Nakata,A.Fujishima.TiO2photocatalysis:Designandapplications[J].JournalofPhotochemistryandPhotobiologyC:PhotochemistryReviews,2012,13:169-189.
[2]X.B.Chen,S.S.Mao.Titaniumdioxidenanomaterials:Synthesis,properties,modifications,andapplications[J].ChemicalReviews,2007,107:2891-2959.
[3]X.Xiao,W.D.Zhang,FacilesynthesisofnanostructuredBiOImicrosphereswithhighvisiblelight-inducedphotocatalyticactivity[J].JournalofMaterialsChemistry,2010,20:5866-5870.
[4]R.A.He,S.W.Cao,P.Zhou,J.G.Yu,RecentadvancesinvisiblelightBi-basedphotocatalysts,Chin.J.Catal.,35(2014)989-1007.
[5]Y.Y.Li,J.S.Wang,H.C.Yao,L.Y.Dang,Z.J.Li.ChemicaletchingpreparationofBiOI/Bi2O3heterostructureswithenhancedphotocatalyticactivities[J].CatalysisCommunications,2011,12:660-664.
[6]Y.Park,K.J.McDonald,K.S.Choi,Progressinbismuthvanadatephotoanodesforuseinsolarwateroxidation,Chem.Soc.Rev.,42(2013)2321-2337.
Summary of the invention
Present invention aims to problems of the prior art, it is provided that a kind of photocatalyst and its preparation method and application。
For achieving the above object, the present invention implements by the following technical solutions:
A kind of photocatalyst, photocatalyst is BiOI/BiVO4Heterojunction composite, it, by BiOI and BiVO4Composition, BiOI and BiVO4Mol ratio be 18:1～1:18。
Described BiOI and BiVO4Mol ratio be 9:1～1:9。
The preparation method of a kind of photocatalyst, by KI and NH4VO3It is scattered in excessive ethanol water, obtains dispersion liquid A；Meanwhile, by Bi (NO3)3·5H2O is dissolved in excessive ethanol water, obtains dispersion liquid B；When stirring, solution A is added dropwise in solution B, transfer in water heating kettle after above-mentioned suspension is stirred 40～80min, 160～200 DEG C of hydro-thermal 12～36h, after hydro-thermal terminates, the BiOI/BiVO with lamellar and flower ball-shaped shape structure can be obtained after sucking filtration, washing and 50～100 DEG C of dry 3～24h4。
Described KI and NH4VO3Between with magnitude relation 1:18～18:1；Use magnitude relation 1:2～2:1 between dispersion liquid A and dispersion liquid B；Bi (NO in dispersion liquid B3)3·5H2Final concentration of 0.25～1mol/L in O。
Described acquisition dispersion liquid A and dispersion liquid B adopts dispersed with stirring 10～60min。
Described ethanol water ethanol and water volume ratio are 1:1。
A kind of application of photocatalyst, described BiOI/BiVO4Heterojunction composite photocatalyst is as the antibacterial in water body。
Described BiOI/BiVO4Heterojunction composite photocatalyst application in degradation of dye。
Described BiOI/BiVO4Heterojunction composite photocatalyst application in water body purification。
BiOI/BiVO4Heterojunction composite photocatalyst is applied in water body, the visible light catalytic of harmful microorganism pseudomonas aeruginosa (P.aeruginosa) and dyestuff contaminant methylene blue (MB) is killed and degraded, adopting 500W xenon lamp as light source, its wave-length coverage is 420～760nm；Described microorganism concn is 108Cfu/mL；Described methylene blue concentration is 20mg/L；Described BiOI/BiVO4The consumption of heterojunction composite photocatalyst is 1.0mg/mL。
The concrete method of testing of its photocatalytic activity is: adopts 500W xenon lamp as light source, is aided with optical filter；Microorganism and methylene blue solution are joined in reactor, is subsequently adding BiOI/BiVO4Heterojunction composite photocatalyst, dark adsorption starts illumination after reaching balance, separated in time sampling in During Illumination, is measured surviving bacteria concentration and remaining methylene blue concentration, calculates killing rate and degradation rate by colony counting method and UV-VIS spectrophotometry。Described light source is xenon lamp, and its wave-length coverage is 420～760nm；Described microorganism concn is 108Cfu/mL；Described methylene blue concentration is 20mg/L；Described BiOI/BiVO4The consumption of heterojunction composite photocatalyst is 1.0mg/mL。
The beneficial effects of the present invention is:
The present invention is by by BiOI and BiVO4Compound, builds and forms the composite with heterojunction structure, accelerates the photo-generated carrier separation at composite material surface, and then improves photocatalysis performance, to BiOI and BiVO4Bi-material is significant in the practical application of photocatalysis field。Concrete:
(1) present invention adopts simple co-precipitation-hydrothermal synthesis method to prepare BiOI/BiVO4Heterojunction composite photocatalyst, preparation method technique is simple, easily controllable, with low cost；
(2) BiOI/BiVO prepared by the present invention4Heterojunction composite photocatalyst, has good visible absorption performance；
(3) BiOI/BiVO prepared by the present invention4Heterojunction composite photocatalyst visible light catalysis activity compares BiOI and BiVO4It is significantly increased, under 500W xenon lamp irradiates, 1.0mg/mLBiOI/BiVO4Concentration is 10 by heterojunction composite photocatalyst8In the microorganism 120min of cfu/mL, killing rate can reach 99.99%, degradable to realizing in the methylene blue 240min of concentration 20mg/L；
(4) BiOI/BiVO prepared by the present invention4Heterojunction composite photocatalyst has good stability and reusing, still has efficient photocatalytic activity after recycling for 5 times；
(5) BiOI/BiVO prepared by the present invention4Heterojunction composite photocatalyst has heterojunction structure, accelerate the separation of photo-generated carrier, reduce the recombination probability of photo-generate electron-hole pair, improve visible light catalysis activity and stability, there is in the field such as water body purification and marine anti-pollution good practical value and potential application prospect。
Accompanying drawing explanation
(wherein abscissa is 2 θ (angles) to the XRD figure spectrum of the sample that Fig. 1 provides for the embodiment of the present invention, and unit is degree (degree)；Vertical coordinate is Intensity (intensity), and unit is a.u. (absolute unit))；
Fig. 2 is the FESEM photo of sample prepared by the present invention: (A) BiVO4, (B) 10%BiOI/BiVO4, (C) 30%BiOI/BiVO4, (D) 50%BiOI/BiVO4, (E) 70%BiOI/BiVO4, (F) 90%BiOI/BiVO4, (G) BiOI；
(wherein abscissa is Wavelength (wavelength) to the UV-vis DRS spectrogram (UV-DRS) of the sample that Fig. 3 provides for the embodiment of the present invention, unit is nm (nanometer), vertical coordinate is Absorbance (absorbance), and unit is a.u. (absolute unit))；
Fig. 4 for the embodiment of the present invention provide sample photocatalytic degradation reaction Methylene Blue concentration changes with time curve (in figure, abscissa is Time (time), and unit is min (minute), and vertical coordinate is Ct/C0, C0Front methylene blue initial concentration, C is started for reactiontMethylene blue concentration for the response time is during t)。
Fig. 5 for the embodiment of the present invention provide the reaction of sample photocatalytic degradation in photo-catalyst rate (in figure, vertical coordinate is Antibacterialrate (sterilizing rate), and unit is %) to pseudomonas aeruginosa。
Fig. 6 is the 30%BiOI/BiVO of preparation in the embodiment of the present invention 14Heterojunction composite photocatalyst repeat 5 sterilization experiments after sterilizing rate (in figure, abscissa is Cyclenumber (reusing number of times), and vertical coordinate is Antibacterialrate (sterilizing rate), and unit is %)。
Detailed description of the invention
Below by way of specific embodiment, the invention will be further described, contributes to those of ordinary skill in the art and is more completely understood by the present invention, but does not limit the present invention in any way。
The present invention is prepared for BiOI/BiVO by co-precipitation and hydrothermal synthesis method4Heterojunction composite photocatalyst, this composite photo-catalyst has good visible absorption performance, the heterojunction structure built accelerates the separation of photo-generated carrier, reduce the recombination probability of photo-generate electron-hole pair, there is efficient photocatalytic activity and stability under visible light, harmful microorganism in water body and dyestuff contaminant are had and kills efficiently and degradation effect, there is in the field such as water body purification and marine anti-pollution good practical value and potential application prospect。The preparation method of this composite photo-catalyst has the features such as simple, cheap and reproducible simultaneously。
Embodiment 1:
KI and the 0.0014molNH of 0.0006mol4VO3Being dissolved in 40mL50% ethanol water, stirring 30min obtains solution A。Meanwhile, the Bi (NO of 0.002moL3)3·5H2O is dissolved in 40mL50% ethanol ethanol water, and stirring 30min obtains solution B。So when stirring, solution A is being added dropwise in solution B。Above-mentioned suspension is transferred in 100mL reactor after stirring 60min, 180 DEG C of hydro-thermal 24h。After being cooled to room temperature, sucking filtration on the microporous filter membrane in 0.22 μm of aperture, product respectively with ultra-pure water and absolute ethanol washing for several times, is placed in vacuum drying oven 60 DEG C of dry 6h, obtains sample and is labeled as 30%BiOI/BiVO4(referring to Fig. 1-3)。
Comparative example 1:
Monomer BiVO4Preparation method:
0.002molNH4VO3Being dissolved in 40mL50% ethanol water, stirring 30min obtains solution A。Meanwhile, the Bi (NO of 0.002moL3)3·5H2O is dissolved in 40mL50% ethanol ethanol water, and stirring 30min obtains solution B。So when stirring, solution A is being added dropwise in solution B。Above-mentioned suspension is transferred in 100mL reactor after stirring 60min, 180 DEG C of hydro-thermal 24h。After being cooled to room temperature, sucking filtration on the microporous filter membrane in 0.22 μm of aperture, product respectively with ultra-pure water and absolute ethanol washing for several times, is placed in vacuum drying oven 60 DEG C of dry 6h, obtains sample and is labeled as BiVO4(referring to Fig. 1-3)。
BiOI, BiVO as seen from Figure 14BiOI/BiVO with the amount ratio of different material4The XRD spectra of complex。These diffraction peak intensities are higher, and peak type is better；Illustrate that the sample of synthesis all has good crystal formation。It addition, can be seen that from Fig. 1 a all of diffraction maximum can with the BiVO of Tetragonal4(JCPDSNo.14-0688) well it coincide；Meanwhile, in Fig. 1 b, all of diffraction maximum can match with the BiOI (JCPDSNo.10-0445) of orthorhombic phase。And Fig. 1 c～1g comprises the BiVO of all Tetragonals4And the characteristic peak of the BiOI of orthorhombic phase (JCPDSNo.10-0445), and there is no other assorted peak (JCPDSNo.14-0688)。Illustrate that the complex of synthesis is by BiVO4With two kinds of thing phase compositions of BiOI。
The BiVO of pure phase is can be seen that by Fig. 2 A4It is made up of nanometer sheet。And the BiOI/BiVO prepared by coprecipitation method4Sample, it can be seen that along with the increase of KI consumption, pattern changes and gradually gradually to nano flower-like structural transformation from Fig. 2 B～2G, the BiOI of pure phase is flower-like structure (Fig. 2 G)。
Result is as shown in Figure 3: BiOI/BiVO4The light abstraction width of sample there occurs significant change compared with BiOI。As can be seen from the figure BiOI and BiVO4Define heterojunction structure after compound, cause that the visible absorption performance of composite strengthens。
Embodiment 2:
BiOI/BiVO4The preparation method of heterojunction composite photocatalyst:
Being prepared by co-precipitation and hydrothermal method, difference from Example 1 is in that, controls BiOI and BiVO4Mol ratio be 1:9。KI and the 0.0018molNH of 0.0002mol4VO3Being dissolved in 40mL50% ethanol water, stirring 30min obtains solution A。Meanwhile, the Bi (NO of 0.002moL3)3·5H2O is dissolved in 40mL50% ethanol ethanol water, and stirring 30min obtains solution B。So when stirring, solution A is being added dropwise in solution B。Above-mentioned suspension is transferred in 100mL reactor after stirring 60min, 180 DEG C of hydro-thermal 24h。After being cooled to room temperature, sucking filtration on the microporous filter membrane in 0.22 μm of aperture, product respectively with ultra-pure water and absolute ethanol washing for several times, is placed in vacuum drying oven 60 DEG C of dry 6h, obtains sample and is labeled as 10%BiOI/BiVO4。
Embodiment 3:
BiOI/BiVO4The preparation method of heterojunction composite photocatalyst:
Being prepared by co-precipitation and hydrothermal method, difference from Example 1 is in that, controls BiOI and BiVO4Mol ratio be 5:5。KI and the 0.001molNH of 0.001mol4VO3Being dissolved in 40mL50% ethanol water, stirring 30min obtains solution A。Meanwhile, the Bi (NO of 0.002moL3)3·5H2O is dissolved in 40mL50% ethanol ethanol water, and stirring 30min obtains solution B。So when stirring, solution A is being added dropwise in solution B。Above-mentioned suspension is transferred in 100mL reactor after stirring 60min, 180 DEG C of hydro-thermal 24h。After being cooled to room temperature, sucking filtration on the microporous filter membrane in 0.22 μm of aperture, product respectively with ultra-pure water and absolute ethanol washing for several times, is placed in vacuum drying oven 60 DEG C of dry 6h, obtains sample and is labeled as 50%BiOI/BiVO4。
Embodiment 4:
BiOI/BiVO4The preparation method of heterojunction composite photocatalyst:
Being prepared by co-precipitation and hydrothermal method, difference from Example 1 is in that, controls BiOI and BiVO4Mol ratio be 7:3。KI and the 0.0006molNH of 0.0014mol4VO3Being dissolved in 40mL50% ethanol water, stirring 30min obtains solution A。Meanwhile, the Bi (NO of 0.002moL3)3·5H2O is dissolved in 40mL50% ethanol ethanol water, and stirring 30min obtains solution B。So when stirring, solution A is being added dropwise in solution B。Above-mentioned suspension is transferred in 100mL reactor after stirring 60min, 180 DEG C of hydro-thermal 24h。After being cooled to room temperature, sucking filtration on the microporous filter membrane in 0.22 μm of aperture, product respectively with ultra-pure water and absolute ethanol washing for several times, is placed in vacuum drying oven 60 DEG C of dry 6h, obtains sample and is labeled as 70%BiOI/BiVO4。
Embodiment 5:
BiOI/BiVO4The preparation method of heterojunction composite photocatalyst:
Being prepared by co-precipitation and hydrothermal method, difference from Example 1 is in that, controls BiOI and BiVO4Mol ratio be 9:1。KI and the 0.0002molNH of 0.0018mol4VO3Being dissolved in 40mL50% ethanol water, stirring 30min obtains solution A。Meanwhile, the Bi (NO of 0.002moL3)3·5H2O is dissolved in 40mL50% ethanol ethanol water, and stirring 30min obtains solution B。So when stirring, solution A is being added dropwise in solution B。Above-mentioned suspension is transferred in 100mL reactor after stirring 60min, 180 DEG C of hydro-thermal 24h。After being cooled to room temperature, sucking filtration on the microporous filter membrane in 0.22 μm of aperture, product respectively with ultra-pure water and absolute ethanol washing for several times, is placed in vacuum drying oven 60 DEG C of dry 6h, obtains sample and is labeled as 90%BiOI/BiVO4。
Application examples 1:
Above-mentioned gained BiOI/BiVO4Heterojunction composite photocatalyst is applied to the visible light photocatalytic degradation of dyestuff contaminant methylene blue (MB):
Using 500W xenon lamp as light source, it is aided with optical filter and filters ultraviolet light so that it is wave-length coverage is 420～760nm。The methylene blue solution of 50mL20mg/L is joined in 50mL reactor, add photocatalyst prepared by the 50mg present invention, dark adsorption carries out light-catalyzed reaction after reaching balance, separated in time sampling in course of reaction, take the supernatant after centrifugation on ultraviolet-visible spectrophotometer, measure the absorbance of methylene blue solution under 664nm wavelength, obtain the residual concentration of methylene blue solution, calculate degradation rate, blank experiment and dark-state with this to test as control experiment (referring to Fig. 4)。
From fig. 4, it can be seen that blank experiment and dark-state experiment Methylene Blue are hardly degraded, the impact of experiment can be ignored。Under visible ray shines, 30%BiOI/BiVO4Heterojunction composite photocatalyst demonstrates good photocatalytic activity, and photocatalysis performance is substantially better than monomer BiOI and BiVO4, within the 240min light-catalyzed reaction time, the degradation rate of methylene blue can be reached 100%。Therefore, will there is BiOI and the BiVO of good visible absorption performance and photocatalytic activity4Being compounded to form heterojunction structure can make photo-generate electron-hole efficiently separate at composite material surface, and improves visible absorption performance and the specific surface area of composite, enhances the visible light catalytic performance of composite。
Application examples 2:
Above-mentioned gained BiOI/BiVO4Heterojunction composite photocatalyst is applied in water body, and the visible ray of harmful microorganism pseudomonas aeruginosa is killed:
Using 500W xenon lamp as light source, it is aided with optical filter and filters ultraviolet light so that it is wave-length coverage is 420～760nm。With pseudomonas aeruginosa (P.aeruginosa, 3.5 × 108Cfu/mL) BiOI/BiVO is evaluated4The visible light catalytic bactericidal property of heterojunction composite photocatalyst:
First prepare bacterial suspension, pseudomonas aeruginosa is stored liquid and is inoculated in sterilizing LB fluid medium, be then placed on 37 DEG C, in the air constant-temperature table of 150rpm, incubated overnight。Cultivating after the bacterial suspension obtained is centrifuged and be suspended in 0.01mol/LPBS (pH=7.4) buffer, obtaining concentration is 3.5 × 108The pseudomonas aeruginosa suspension of cfu/mL。
Taking 49.5mL sterilizing 0.01mol/LPBS (pH=7.4) buffer in photocatalysis experiment to join in 50mL reactor, be subsequently adding 500 μ L bacterial suspensions, making bacterial concentration in reactant liquor is 8.0 × 106Cfu/mL, adds photocatalyst prepared by the 50mg present invention。Dark adsorption carries out light-catalyzed reaction after reaching balance, and in course of reaction, separated in time sampling, determines survival rate and the sterilizing rate of antibacterial by colony counting method。Concretely comprise the following steps: take 1.0mL reactant liquor, several gradient is diluted successively according to serial dilutions with 0.01mol/LPBS (pH=7.4) buffer, then from the solution of different extension rates, take 100 μ L to the LB solid medium being already prepared to, bacterium solution is spread upon in LB culture medium equably。LB culture medium being inverted, put into 37 DEG C of cultivation 24h in electro-heating standing-temperature cultivator, by counting the bacterium colony number grown in culture medium, and corresponding extension rate draws bacterial concentration, to determine survival rate and the sterilizing rate of antibacterial。Experiment is often organized experiment and is both needed to parallel assay 3 times, average and test as control experiment (referring to Fig. 5) as end product, blank experiment and dark-state。?
As seen from Figure 5, in blank experiment, pseudomonas aeruginosa number has almost no change, it was shown that the impact of visible ray photograph can be ignored；And under dark condition, number of bacteria is also without significant change, it was shown that the material itself that this experiment uses does not have bio-toxicity。And visible ray according under 30%BiOI/BiVO4Heterojunction composite photocatalyst shows good photocatalytic activity, and photo-catalyst performance is substantially better than monomer BiVO4And BiOI, the illumination through 60min only has the pseudomonas aeruginosa survival of about 1.7log, and sterilizing rate can reach 99.99%。Therefore, 30%BiOI/BiVO4Heterojunction composite photocatalyst has splendid photo-catalyst antifouling property, is attributable to BiOI and BiVO4Be compounded to form heterojunction structure, accelerate the separation of photo-generate electron-hole, improve the photocatalytic activity of composite。Meanwhile, BiOI/BiVO4Heterojunction composite photocatalyst has good visible absorption performance, causes that its visible light catalytic performance improves, has good visible light catalytic bactericidal property。
Application examples 3:
Above-mentioned gained BiOI/BiVO4Heterojunction composite photocatalyst is repeatedly applied in water body, and the visible ray of harmful microorganism pseudomonas aeruginosa is killed。
By 30%BiOI/BiVO used in photo-catalyst in application examples 24Heterojunction composite photocatalyst reclaims, and repeatedly washs with ultra-pure water and dehydrated alcohol respectively, carries out photo-catalyst reaction next time according to the step in application examples 2 after drying, continuously performs 5 times, keep other conditions constant (referring to Fig. 6)。
As seen from Figure 6,30%BiOI/BiVO4The killing rate of antibacterial is not substantially reduced by heterojunction composite photocatalyst after successive reaction 5 times, is still maintained at more than 99%, it is shown that good reusing。The 30%BiOI/BiVO of 5 photo-catalyst experiments will be continuously performed4Composite photo-catalyst reclaims, and repeatedly washs with ultra-pure water and dehydrated alcohol respectively, carries out XRD test after drying, as shown in Figure 6, as can be seen from the figure after continuous 5 photo-catalysts reaction, and 30%BiOI/BiVO4The crystal structure of composite photo-catalyst, peak intensity and composition all do not change, and show good stability, have good practical value and potential application prospect in the field such as water body purification and marine anti-pollution。
Claims (9)
1. a photocatalyst, it is characterised in that: photocatalyst is BiOI/BiVO4Heterojunction composite, it, by BiOI and BiVO4Composition, BiOI and BiVO4Mol ratio be 18:1～1:18。
2. photocatalyst according to claim 1, it is characterised in that: described BiOI and BiVO4Mol ratio be 9:1～1:9。
3. the preparation method of the photocatalyst described in a claim 1, it is characterised in that: by KI and NH4VO3It is scattered in excessive ethanol water, obtains dispersion liquid A；Meanwhile, by Bi (NO3)3·5H2O is dissolved in excessive ethanol water, obtains dispersion liquid B；When stirring, solution A is added dropwise in solution B, transfer in water heating kettle after above-mentioned suspension is stirred 40～80min, 160～200 DEG C of hydro-thermal 12～36h, after hydro-thermal terminates, the BiOI/BiVO with lamellar and flower ball-shaped shape structure can be obtained after sucking filtration, washing and 50～100 DEG C of dry 3～24h4。
4. the preparation method of photocatalyst according to claim 3, it is characterised in that: described KI and NH4VO3Between with magnitude relation 1:18～18:1；Use magnitude relation 1:2～2:1 between dispersion liquid A and dispersion liquid B；Bi (NO in dispersion liquid B3)3·5H2Final concentration of 0.25～1mol/L in O。
5. the preparation method of photocatalyst according to claim 3, it is characterised in that: described acquisition dispersion liquid A and dispersion liquid B adopts dispersed with stirring 10～60min。
6. the preparation method of photocatalyst according to claim 3, it is characterised in that: described ethanol water ethanol and water volume ratio are 1:1。
7. the application of the photocatalyst described in a claim 1, it is characterised in that: described BiOI/BiVO4Heterojunction composite photocatalyst is as the antibacterial in water body。
8. the application of the photocatalyst described in a claim 1, it is characterised in that: described BiOI/BiVO4Heterojunction composite photocatalyst application in degradation of dye。
9. the application of the photocatalyst described in a claim 1, it is characterised in that: described BiOI/BiVO4Heterojunction composite photocatalyst application in water body purification。
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