CN105289673A - Bi2WO6/Ag3PO4 heterojunction composite photocatalyst and preparation method and application thereof - Google Patents

Bi2WO6/Ag3PO4 heterojunction composite photocatalyst and preparation method and application thereof Download PDF

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CN105289673A
CN105289673A CN201510789041.8A CN201510789041A CN105289673A CN 105289673 A CN105289673 A CN 105289673A CN 201510789041 A CN201510789041 A CN 201510789041A CN 105289673 A CN105289673 A CN 105289673A
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composite photocatalyst
heterojunction composite
preparation
heterojunction
bi2wo6
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鞠鹏
张盾
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Institute of Oceanology of CAS
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Institute of Oceanology of CAS
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Abstract

The invention belongs to the field of photocatalysis and specifically relates to a Bi2WO6/Ag3PO4 heterojunction composite photocatalyst and its preparation method and application. The Bi2WO6/Ag3PO4 heterojunction composite photocatalyst is composed of Bi2WO6 and Ag3PO4, wherein Ag3PO4 nanoparticles are deposited on the Bi2WO6 surface of a three-dimensional layered rod-like structure; and the molar ratio of Bi2WO6 to Ag3PO4 is 1:0.1-10. The preparation method of the invention has a simple process, is easy to control and is low-cost. A Bi2WO6/Ag3PO4 heterojunction structure with visible light response is constructed, photon-generated carrier separation is accelerated, and recombination probability of photogenerated electron-hole pairs is minimized. The Bi2WO6/Ag3PO4 heterojunction composite photocatalyst has high-efficiency photocatalytic activity and stability in visible light, has highly-efficient killing and degradation effects on harmful microbes and dye pollutants in a water body and has good practical value and potential application prospect in fields of water body purification, marine pollution prevention and the like.

Description

A kind of Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst and its preparation method and application
Technical field
The invention belongs to photocatalysis field, be specifically related to a kind of Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst and its preparation method and application.
Background technology
Photocatalysis technology is a kind of technology utilizing luminous energy to carry out Substance Transformation, from Japanese Scientists Fujishima in 1972 and Honda reported first TiO 2can after photocatalytic water produce hydrogen and oxygen under ultraviolet lighting, Photocatalitic Technique of Semiconductor receives increasing concern [1].For semi-conducting material, they can produce electron-hole pair under illumination condition, a part electronics and hole body mutually in or surface meet and compound, another part electron transfer has very strong reducing power to semiconductor surface, can be combined with the oxygen of absorption, generate the free radical with strong oxidizing property; And there is very strong oxidability in the hole moving to semiconductor surface, the OH of semiconductor surface can be adsorbed on -and H 2o is oxidized, and produces the free radical of strong oxidizing property, such as OH, HO 2, H 2o 2and O 2 -deng [2], can directly and reactant to have an effect and by its oxidation Decomposition, and do not produce secondary pollution.In recent years, the application study development of photocatalysis technology is very rapid, because of its have efficiently, non-selectivity, stability are high, green non-poisonous, non-secondary pollution, energy consumption are low, easy and simple to handle and the outstanding advantages such as low cost, and the solar energy of cleanliness without any pollution can be made full use of, at sewage disposal, exhaust-gas treatment, purification of air, sterilizing, catalyzing manufacturing of hydrogen, reduction CO 2etc. aspect be widely used, and respond well.
In recent years, the visible light catalyst of people to development of new has done large quantity research, wherein contains the In of d0 and d10 electron configuration 3+, Ce 3+, Bi 3+, Ag +deng.Wherein, Bi 2wO 6be one the simplest Aurivillius type oxide, be a kind of N-shaped direct semiconductor material, the Bi from reported first such as Kudo in 1999 2wO 6after there is photocatalytic activity be greater than the visible radiation of 420nm at wavelength under [3], Bi 2wO 6because of its narrower energy gap (about 2.7eV), also can be had higher catalytic activity under visible light thus cause increasing concern as a kind of novel visible catalysis material by excited by visible light [4].But due at monomers B i 2wO 6in the right migration distance of the electronics that excites and hole long, the probability of body phase compound increases, and is unfavorable for the quick separating of electron-hole, causes photocatalytic activity relatively not high.Therefore, composite can be built by semiconductors coupling and can accelerate electron-hole separation, improve the photocatalysis performance of monomer material [5,6].Ag 3pO 4a kind of new and effective catalysis material, the strong oxidizing property in optical excitation hole in its distinctive indirect band gap, valence band, its electron transfer rate is higher than hole migration speed simultaneously, thus impels electron-hole to be separated, and makes it have good photocatalysis performance; Simultaneously Ag vacancy defect can participate in photoelectron and catches, and provides more optical excitation hole, is also conducive to electron-hole and is separated [7].Therefore, now need to build a kind of composite catalyst.
[1]K.Nakata,A.Fujishima.TiO 2photocatalysis: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]A.Kudo,S.Hijii。H-2orO-2evolutionfromaqueoussolutionsonlayeredoxidephotocatalystsconsistingofBi 3+with6s(2)configurationandd(0)transitionmetalions[J].ChemistryLetters,1999,10:1103-1104.
[4]X.F.Cao,L.Zhang,X.T.Chen,Z.L.Xue.Microwave-assistedsolution-phasepreparationofflower-likeBi2WO6anditsvisible-light-drivenphotocatalyticproperties[J].CrystEngComm,2011,13:306-311.
[5]Y.Hu,D.Z.Li,Y.Zheng,W.Chen,Y.H.He,Y.Shao,X.Z.Fu,G.C.Xiao.BiVO 4/TiO 2nanocrystallineheterostructure:Awidespectrumresponsivephotocatalysttowardsthehighlyefficientdecompositionofgaseousbenzene[J].AppliedCatalysisB:Environmental,2011,104:30-36.
[6]Z.J.Zhang,W.Z.Wang,L.Wang,S.M.Sun.Enhancementofvisible-lightphotocatalysisbycouplingwithnarrow-band-gapsemiconductor:AcasestudyonBi 2S 3/Bi 2WO 6[J].ACSAppliedMaterials&Interfaces,2012,4:593-597.
[7]Z.G.Yi,J.H.Ye,N.Kikugawa,T.Kako,S.X.Ouyang,H.Stuart-Williams,H.Yang,J.Y.Cao,W.J.Luo,Z.S.Li,Y.Liu,R.L.Withers.Anorthophosphatesemiconductorwithphotooxidationpropertiesundervisible-lightirradiation[J].NatureMaterials,2010,9:559-564.
Summary of the invention
The object of the invention is to for problems of the prior art, a kind of Bi is provided 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst and its preparation method and application.
For achieving the above object, the present invention implements by the following technical solutions:
A kind of Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst, by Bi 2wO 6and Ag 3pO 4composition; Wherein, Ag 3pO 4nanoparticle deposition is at the Bi of three-dimensional layering club shaped structure 2wO 6surface; Bi 2wO 6with Ag 3pO 4mol ratio be 1:0.1 ~ 10.
Described Bi 2wO 6with Ag 3pO 4mol ratio be 1:0.1 ~ 5.
A kind of Bi 2wO 6/ Ag 3pO 4the preparation method of heterojunction composite photocatalyst:
(1) Bi 2wO 6preparation: by Bi (NO 3) 35H 2o is scattered in ultra-pure water, obtains dispersion liquid; Simultaneously by Na 2wO 42H 2o joins in ultra-pure water, and magnetic agitation, to dissolving completely, obtains lysate; Then under magnetic stirring by above-mentioned Na 2wO 4lysate dropwise joins above-mentioned Bi (NO 3) 3in dispersion liquid, obtain suspension, and after regulating pH of suspension to 5 ~ 9 to stir, suspension is transferred in autoclave, put into electric heating constant-temperature blowing drying box 120 ~ 180 DEG C of heat treatment 12 ~ 36h, then reactor is cooled to room temperature, the Bi of three-dimensional layering club shaped structure can be obtained through suction filtration, washing and 40 ~ 80 DEG C of drying 2 ~ 10h 2wO 6; Wherein, Bi (NO 3) 35H 2o and Na 2wO 42H 2the ratio of the amount of substance of O is 2:1;
(2) Bi 2wO 6/ Ag 3pO 4the preparation of heterojunction composite photocatalyst: by the Bi obtained in step (1) 2wO 6be scattered in ultra-pure water and obtain dispersion liquid, then add AgNO under magnetic stirring 3, be stirred to and dissolve to obtain mixed liquor completely, then dropwise add the precursor solution of phosphorous acid group, continue lucifuge afterwards and stir 2 ~ 8h, can Bi be obtained through suction filtration, washing and 40 ~ 80 DEG C of vacuum drying 2 ~ 10h 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst; Wherein, phosphate radical and AgNO in the precursor of phosphorous acid group 3the ratio of the amount of substance of middle silver ion is 1:3.
Suspension pH value is regulated to adopt concentration to be the NH of 0.1 ~ 5.0mol/L in described step (1) 3h 2o or NaOH.
In described step (2), the precursor of phosphorous acid group is Na 2hPO 4, NaH 2pO 4, Na 3pO 4, K 2hPO 4, KH 2pO 4or K 3pO 4one wherein.
Bi in described step (2) 2wO 6with the AgNO added 3the ratio of amount of substance be 1:0.3 ~ 15.
Disperse to be adopt ultrasonic disperse 10 ~ 60min, then magnetic agitation 10 ~ 60min in described step (1) and step (2).
A kind of Bi 2wO 6/ Ag 3pO 4the application of heterojunction composite photocatalyst, described Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst is as the application of bactericide in water body.
A kind of Bi 2wO 6/ Ag 3pO 4the application of heterojunction composite photocatalyst, described Bi 2wO 6/ Ag 3pO 4the application of heterojunction composite photocatalyst in degradation of dye.
A kind of Bi 2wO 6/ Ag 3pO 4the application of heterojunction composite photocatalyst, described Bi 2wO 6/ Ag 3pO 4the application of heterojunction composite photocatalyst in water body purification.
Bi 2wO 6/ Ag 3pO 4heterojunction 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, adopt 500W xenon lamp as light source, its wave-length coverage is 420 ~ 760nm; Described microorganism concn is 10 6cfu/mL; Described methylene blue concentration is 20mg/L; Described Bi 2wO 6/ Ag 3pO 4the consumption of heterojunction composite photocatalyst is 1.0mg/mL.
The concrete method of testing of its photocatalytic activity is: adopt 500W xenon lamp as light source, be aided with optical filter; Microorganism and methylene blue solution are joined in reactor, then adds Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst, dark adsorption starts illumination after reaching balance, separated in time sampling in During Illumination, measures surviving bacteria concentration and remaining methylene blue concentration by colony counting method and ultraviolet-visible spectrophotometry, calculates killing rate and degradation rate.Described light source is xenon lamp, and its wave-length coverage is 420 ~ 760nm; Described microorganism concn is 10 6cfu/mL; Described methylene blue concentration is 20mg/L; Described Bi 2wO 6/ Ag 3pO 4the consumption of heterojunction composite photocatalyst is 1.0mg/mL.
Beneficial effect of the present invention is:
The present invention passes through Ag 3pO 4with Bi 2wO 6compound, builds the composite with heterojunction structure, accelerates the separation of photo-generated carrier at composite material surface, and then improves the photocatalysis performance of composite, to Bi 2wO 6and Ag 3pO 4bi-material is significant in the practical application of photocatalysis field; Concrete:
(1) preparation method's technique of adopting of the present invention simple, be easy to control, with low cost;
(2) the present invention prepare by three-dimensional layering club shaped structure Bi 2wO 6loaded Ag 3pO 4the Bi that nano particle builds 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst, has larger specific area and good visible absorption performance;
(3) Bi for preparing of the present invention 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst visible light catalysis activity compares Bi 2wO 6and Ag 3pO 4be significantly increased, under 500W xenon lamp irradiates, 1.0mg/mLBi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst is 10 to concentration 6the microorganism 20min killing rate of cfu/mL can reach 99.99%, to concentration be 20mg/L methylene blue 25min in realize degradable;
(4) Bi for preparing of the present invention 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst has good stability and reusing, still has efficient photocatalytic activity after reusing for 6 times;
(5) Bi for preparing of the present invention 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst has heterojunction structure, accelerate the separation of photo-generated carrier, reduce the recombination probability that photo-generate electron-hole is right, 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 X-ray diffraction (XRD) collection of illustrative plates of Fig. 1 sample prepared by the present invention, and unit is degree (degree); Ordinate is Intensity (intensity), and unit is a.u. (absolute unit));
SEM (FESEM) photo of Fig. 2 sample prepared by the present invention: (A) Ag 3pO 4, (B) Bi 2wO 6, (C, D) Bi 2wO 6/ Ag 3pO 4-1;
(wherein abscissa is Wavelength (wavelength) to UV-vis DRS spectrum (UV-DRS) figure of Fig. 3 sample prepared by the present invention, unit is nm (nanometer), ordinate is Absorbance (absorbance), and unit is a.u. (absolute unit));
During sample photocatalytic degradation reaction Methylene Blue concentration changes with time curve (A) of Fig. 4 prepared by the present invention and photo-catalyst react, (wherein in A figure, abscissa is Time (time) for the survival curve (B) of pseudomonas aeruginosa, unit is min (minute), and ordinate is C t/ C 0, C 0for reaction starts front methylene blue initial concentration, C tfor the methylene blue concentration when reaction time is t; In B figure, abscissa is Time (time), and unit is min (minute), and ordinate is Celldensity (cell concentration), and unit is logCcfu/mL (clump count));
Fig. 5 is the Bi of preparation in the embodiment of the present invention 2 2wO 6/ Ag 3pO 4(wherein in A figure, abscissa is Cyclenumbers (reusing number of times) for sterilizing rate (A) after-1 heterojunction composite photocatalyst repeats 6 sterilization experiments and XRD collection of illustrative plates (B), ordinate is Antibacterialrate (sterilizing rate), and unit is %; In B figure, abscissa is 2 θ (angles), and unit is degree (degree), and ordinate is Intensity (intensity), and unit is a.u. (absolute unit)).
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 more fully understand the present invention, but do not limit the present invention in any way.
The present invention has prepared Bi by hydrothermal synthesis method and in situ Precipitation 2wO 6/ Ag 3pO 4heterojunction 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 that photo-generate electron-hole is right, there is efficient photocatalytic activity and stability under visible light, have harmful microorganism in water body and dyestuff contaminant and kill 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.This composite photo-catalyst preparation method has the features such as simple, cheap and reproducible simultaneously.
Embodiment 1:
Bi 2wO 6/ Ag 3pO 4the preparation method of heterojunction composite photocatalyst:
(1) Bi of three-dimensional layering club shaped structure is prepared by hydrothermal synthesis method 2wO 6: take 5.0mmolBi (NO 3) 35H 2o joins in 30mL ultra-pure water, and ultrasonic disperse 30min, then magnetic agitation 30min, obtain dispersion liquid; Simultaneously by 5.0mmolNa 2wO 42H 2o joins in 30.0mL ultra-pure water, and magnetic agitation, to dissolving completely, obtains lysate; Afterwards to above-mentioned Bi (NO 3) 3above-mentioned Na is dropwise added in dispersion liquid 2wO 4lysate, obtains suspension, then uses 2.0mol/LNH 3h 2o solution regulates the pH of suspension to be 7, continues afterwards to stir 60min; After stirring terminates, suspension is transferred to and is furnished with in teflon-lined autoclave, put into electric heating constant-temperature blowing drying box 160 DEG C of heat treatment 24h; After reaction terminates, reactor is cooled to room temperature, product is through suction filtration, and suction filtration gained precipitation, successively through ultra-pure water and absolute ethanol washing, then in 60 DEG C of dry 6h, can obtain the Bi with three-dimensional layering club shaped structure 2wO 6(see Fig. 1-3).
(2) Bi is prepared by situ Precipitation 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst: control Bi 2wO 6with Ag 3pO 4mol ratio be 1:1, take above-mentioned gained 1.0mmolBi 2wO 6join in 30mL ultra-pure water, ultrasonic disperse 30min, then magnetic agitation 30min, obtain dispersion liquid; Take 3.0mmolAgNO afterwards 3join above-mentioned Bi 2wO 6in dispersion liquid, be stirred to and dissolve completely, obtain mixed liquor; Simultaneously by 1.0mmolNa 2hPO 412H 2o joins in 30mL ultra-pure water, and magnetic agitation makes it dissolve completely, obtains lysate; Then by above-mentioned Na 2hPO 4lysate dropwise joins above-mentioned Bi 2wO 6with AgNO 3mixed liquor in, continue at room temperature lucifuge stir 5h; After stirring terminates, product is through suction filtration, and suction filtration gained precipitation is successively through ultra-pure water and absolute ethanol washing, and then dry 6h in 60 DEG C of vacuum drying chambers, can obtain Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst, is designated as Bi 2wO 6/ Ag 3pO 4-1 (see Fig. 1-3).
Comparative example 1:
Monomer A g 3pO 4preparation method:
Prepared by coprecipitation.By 3.0mmolAgNO 3be dissolved in 30mL ultra-pure water, magnetic agitation makes it dissolve completely; Simultaneously by 1.0mmolNa 2hPO 412H 2o joins in 30mL ultra-pure water, and magnetic agitation makes it dissolve completely, obtains lysate respectively; Then by above-mentioned Na 2hPO 4lysate is dropwise added drop-wise to above-mentioned AgNO under magnetic stirring 3in lysate, obtain suspension, continue at room temperature lucifuge and stir 5h; After stirring terminates, product is through suction filtration, and suction filtration postprecipitation is successively through ultra-pure water and absolute ethanol washing several, and then dry 6h in 60 DEG C of vacuum drying chambers, can obtain Ag 3pO 4monomer material, is designated as Ag 3pO 4(see Fig. 1-3).
As shown in Figure 1, a curve is monomers B i prepared by embodiment 1 2wO 6xRD collection of illustrative plates, position and the standard card JCPDSNo.73-1126 of all diffraction maximums fit like a glove, and all belong to rhombic Bi 2wO 6, and there is not any impurity phase, can determine that sample prepared by embodiment 1 is pure oblique side phase Bi 2wO 6.B curve is monomer A g prepared by comparative example 1 3pO 4xRD collection of illustrative plates, as seen from the figure, diffraction maximums all in figure all with the cubic system Ag of standard 3pO 4corresponding (JCPDSNo.06-0505), and do not have dephasign diffraction maximum to occur, show that the sample prepared by comparative example 1 is pure cubic structure Ag 3pO 4.C curve in figure is Bi prepared by embodiment 1 2wO 6/ Ag 3pO 4the XRD collection of illustrative plates of-1 heterojunction composite photocatalyst, contains Emission in Cubic Ag in collection of illustrative plates 3pO 4with oblique side phase Bi 2wO 6all characteristic peaks, Ag is described 3pO 4and Bi 2wO 6successfully be combined with each other formation composite.In the XRD collection of illustrative plates of composite, there are not other impurity peaks, illustrate in composite just by Bi 2wO 6and Ag 3pO 4two kinds of material compositions, other impurity phases do not exist.
From Fig. 2 (A), Ag prepared by comparative example 1 3pO 4for being spherical particle, degree of crystallinity is higher, and size is about 200nm, and particle dispersion is good, does not have obvious agglomeration between crystal grain.From Fig. 2 (B), Bi prepared by embodiment 1 2wO 6for the club shaped structure of three-dimensional layering, be about 10 μm, wide about 1 μm, the club shaped structure of this layering is piled up by the two-dimensional nano lamellae cross of many rules to form, and each nanometer sheet size is about 100nm, and thickness is about 20nm.From Fig. 2 (C) and Fig. 2 (D), Bi prepared by embodiment 1 2wO 6/ Ag 3pO 4-1 heterojunction composite photocatalyst is about the three-dimensional layering club shaped structure Bi of 10 μm by size 2wO 6load particle diameter is about the Ag of 50nm 3pO 4nano particle assembles, and this load short grained layering three-dimensional structure will have larger specific area and good visible absorption performance.
As seen from Figure 3, Bi 2wO 6, Ag 3pO 4and Bi 2wO 6/ Ag 3pO 4-1 composite all has good absorption in ultra-violet (UV) band and visible region, demonstrates good visible absorption performance.In addition, there is the Ag of good visible absorption performance 3pO 4with Bi 2wO 6compound substantially increases Bi 2wO 6visible absorption performance.
Embodiment 2:
Bi 2wO 6/ Ag 3pO 4the preparation method of heterojunction composite photocatalyst:
Prepared by situ Precipitation, difference from Example 1 is, control Bi 2wO 6with Ag 3pO 4mol ratio be 1:0.75, take above-mentioned gained 1.0mmolBi 2wO 6join in 30mL ultra-pure water, ultrasonic disperse 30min, then magnetic agitation 30min, obtain dispersion liquid; Take 2.25mmolAgNO afterwards 3join above-mentioned Bi 2wO 6in dispersion liquid, be stirred to and dissolve completely, obtain mixed liquor; Simultaneously by 0.75mmolNa 2hPO 412H 2o joins in 30mL ultra-pure water, and magnetic agitation makes it dissolve completely, obtains lysate; Then by above-mentioned Na 2hPO 4lysate dropwise joins above-mentioned Bi 2wO 6with AgNO 3mixed liquor in, continue at room temperature lucifuge stir 5h; After stirring terminates, product is through suction filtration, and suction filtration gained precipitation is successively through ultra-pure water and absolute ethanol washing, and then dry 6h in 60 DEG C of vacuum drying chambers, can obtain Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst, is designated as Bi 2wO 6/ Ag 3pO 4-0.75.
Embodiment 3:
Bi 2wO 6/ Ag 3pO 4the preparation method of heterojunction composite photocatalyst:
Prepared by situ Precipitation, difference from Example 1 is, control Bi 2wO 6with Ag 3pO 4mol ratio be 1:0.5, take above-mentioned gained 1.0mmolBi 2wO 6join in 30mL ultra-pure water, ultrasonic disperse 30min, then magnetic agitation 30min, obtain dispersion liquid; Take 1.5mmolAgNO afterwards 3join above-mentioned Bi 2wO 6in dispersion liquid, be stirred to and dissolve completely, obtain mixed liquor; Simultaneously by 0.5mmolNa 2hPO 412H 2o joins in 30mL ultra-pure water, and magnetic agitation makes it dissolve completely, obtains lysate; Then by above-mentioned Na 2hPO 4lysate dropwise joins above-mentioned Bi 2wO 6with AgNO 3mixed liquor in, continue at room temperature lucifuge stir 5h; After stirring terminates, product is through suction filtration, and suction filtration gained precipitation is successively through ultra-pure water and absolute ethanol washing, and then dry 6h in 60 DEG C of vacuum drying chambers, can obtain Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst, is designated as Bi 2wO 6/ Ag 3pO 4-0.5.
Embodiment 4:
Bi 2wO 6/ Ag 3pO 4the preparation method of heterojunction composite photocatalyst:
Prepared by situ Precipitation, difference from Example 1 is, control Bi 2wO 6with Ag 3pO 4mol ratio be 1:0.25, take above-mentioned gained 1.0mmolBi 2wO 6join in 30mL ultra-pure water, ultrasonic disperse 30min, then magnetic agitation 30min, obtain dispersion liquid; Take 0.75mmolAgNO afterwards 3join above-mentioned Bi 2wO 6in dispersion liquid, be stirred to and dissolve completely, obtain mixed liquor; Simultaneously by 0.25mmolNa 2hPO 412H 2o joins in 30mL ultra-pure water, and magnetic agitation makes it dissolve completely, obtains lysate; Then by above-mentioned Na 2hPO 4lysate dropwise joins above-mentioned Bi 2wO 6with AgNO 3mixed liquor in, continue at room temperature lucifuge stir 5h; After stirring terminates, product is through suction filtration, and suction filtration gained precipitation is successively through ultra-pure water and absolute ethanol washing, and then dry 6h in 60 DEG C of vacuum drying chambers, can obtain Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst, is designated as Bi 2wO 6/ Ag 3pO 4-0.25.
Application examples 1:
Above-mentioned gained Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst is applied to the visible light photocatalytic degradation of dyestuff contaminant methylene blue MB:
Using 500W xenon lamp as light source, be aided with optical filter and filter ultraviolet light, make its wave-length coverage be 420 ~ 760nm.The methylene blue solution of 50mL20mg/L is joined in 50mL reactor, add photochemical catalyst prepared by 50mg the present invention, dark adsorption carries out light-catalyzed reaction after reaching balance, separated in time sampling in course of reaction, the absorbance that supernatant liquor measures methylene blue solution under 664nm wavelength on ultraviolet-visible spectrophotometer is got after centrifugation, obtain the residual concentration of methylene blue solution, calculate degradation rate with this, blank assay and dark-state experiment test (see Fig. 4 A) in contrast.
From Fig. 4 (A), blank assay Methylene Blue is not almost degraded, and can ignore the impact of experiment.In addition, dark-state experiment shows Bi 2wO 6/ Ag 3pO 4-1 heterojunction composite photocatalyst has certain absorption property because having larger specific area, but can ignore the impact of light-catalyzed reaction.Under visible ray shines, Bi 2wO 6/ Ag 3pO 4-1 composite photo-catalyst demonstrates good photocatalytic activity, and photocatalysis performance is obviously better than monomers B i 2wO 6and Ag 3pO 4, within the 25min light-catalyzed reaction time, can 100% be reached to the degradation rate of methylene blue.Therefore, will there is the Ag of good visible absorption performance and photocatalytic activity 3pO 4with Bi 2wO 6being compounded to form heterojunction structure can make photo-generate electron-hole effectively be separated at composite material surface, and improves visible absorption performance and the specific area of composite, enhances the visible light catalytic performance of composite.
Application examples 2:
Above-mentioned gained Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst is applied in water body, kills the visible ray of harmful microorganism pseudomonas aeruginosa:
Using 500W xenon lamp as light source, be aided with optical filter and filter ultraviolet light, make its wave-length coverage be 420 ~ 760nm.With pseudomonas aeruginosa (P.aeruginosa, 8.0 × 10 8cfu/mL) Bi is evaluated 2wO 6/ Ag 3pO 4the visible light catalytic bactericidal property of heterojunction composite photocatalyst:
First prepare bacterial suspension, pseudomonas aeruginosa storage liquid is inoculated in sterilizing LB fluid nutrient medium, be then placed on 37 DEG C, in the air constant-temperature table of 150rpm, incubated overnight.Be suspended in 0.01mol/LPBS (pH=7.4) buffer solution after the bacterial suspension that cultivation obtains is centrifugal, obtaining concentration is 8.0 × 10 8the pseudomonas aeruginosa suspension of cfu/mL.
Getting 49.5mL sterilizing 0.01mol/LPBS (pH=7.4) buffer solution in photocatalysis experiment joins in 50mL reactor, then adds 500 μ L bacterial suspensions, makes bacterial concentration in reactant liquor be 8.0 × 10 6cfu/mL, adds photochemical catalyst prepared by 50mg the 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 bacterium by colony counting method.Concrete steps are: get 1.0mL reactant liquor, several gradient is diluted successively according to serial dilutions with 0.01mol/LPBS (pH=7.4) buffer solution, then get from the solution of different extension rate on 100 μ L to ready LB solid medium, bacterium liquid is spread upon on LB culture medium equably.Be inverted by LB culture medium, put into electro-heating standing-temperature cultivator 37 DEG C and cultivate 24h, by the bacterium colony number that counting culture medium grows, and corresponding extension rate draws bacterial concentration, to determine survival rate and the sterilizing rate of bacterium.In experiment, often group experiment all needs parallel determination 3 times, averages as end product, and blank assay and dark-state experiment test (see Fig. 4 B) in contrast.
From Fig. 4 (B), in blank assay, the number of pseudomonas aeruginosa has almost no change, and shows that the impact of visible ray photograph can be ignored; And under dark condition, the number of pseudomonas aeruginosa has certain minimizing, this is because Bi 2wO 6/ Ag 3pO 4containing Ag element in-1 heterojunction composite photocatalyst, have part Ag in aqueous +discharge, Ag +also there is certain bactericidal property, can have an effect with bacterium, cause bacterium apoptosis.And visible ray according under Bi 2wO 6/ Ag 3pO 4-1 heterojunction composite photocatalyst demonstrates good photocatalytic activity, and photo-catalyst performance is obviously better than monomers B i 2wO 6and Ag 3pO 4, the bacteria living of the 2.9log that only has an appointment through 20min illumination, sterilizing rate can reach 99.99%, if extend the reaction time to 30min, in system, bacterial concentration is negligible.Therefore, Bi 2wO 6/ Ag 3pO 4-1 heterojunction composite photocatalyst has splendid photo-catalyst antifouling property, is attributable to Ag 3pO 4with Bi 2wO 6be compounded to form heterojunction structure, accelerate the separation of photo-generate electron-hole, improve the photocatalytic activity of composite.Meanwhile, Bi 2wO 6/ Ag 3pO 4-1 heterojunction composite photocatalyst has larger specific area and good visible absorption performance, causes its visible light catalytic performance to improve, has good visible light catalytic bactericidal property.
Application examples 3:
Above-mentioned gained Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst repeated application, in water body, is killed the visible ray of harmful microorganism pseudomonas aeruginosa:
By Bi used in the photo-catalyst in application examples 2 2wO 6/ Ag 3pO 4-1 heterojunction composite photocatalyst reclaims, and repeatedly washs respectively with ultra-pure water and absolute ethyl alcohol, carries out photo-catalyst reaction next time after drying, carry out 6 times continuously, keep other conditions constant (see Fig. 5) according to the step in application examples 2.
From Fig. 5 (A), Bi 2wO 6/ Ag 3pO 4-1 heterojunction composite photocatalyst does not obviously reduce for 6 times in successive reaction afterwards to the killing rate of bacterium, still remains on more than 99%, demonstrates good reusing.The Bi of 6 photo-catalyst experiments will be carried out continuously 2wO 6/ Ag 3pO 4-1 heterojunction composite photocatalyst reclaims, and repeatedly washs respectively, carry out XRD test after drying with ultra-pure water and absolute ethyl alcohol, as shown in Fig. 5 (B), as can be seen from the figure after continuous 6 photo-catalysts reaction, and Bi 2wO 6/ Ag 3pO 4the crystal structure of-1 heterojunction composite photocatalyst does not change, and shows good stability, has good practical value and potential application prospect in the field such as water body purification and marine anti-pollution.

Claims (10)

1. a Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst, is characterized in that: Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst is by Bi 2wO 6and Ag 3pO 4composition; Wherein, Ag 3pO 4nanoparticle deposition is at the Bi of three-dimensional layering club shaped structure 2wO 6surface; Bi 2wO 6with Ag 3pO 4mol ratio be 1:0.1 ~ 10.
2. Bi according to claim 1 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst, is characterized in that: described Bi 2wO 6with Ag 3pO 4mol ratio be 1:0.1 ~ 5.
3. a Bi according to claim 1 2wO 6/ Ag 3pO 4the preparation method of heterojunction composite photocatalyst, is characterized in that:
(1) Bi 2wO 6preparation: by Bi (NO 3) 35H 2o is scattered in ultra-pure water, obtains dispersion liquid; Simultaneously by Na 2wO 42H 2o joins in ultra-pure water, and magnetic agitation, to dissolving completely, obtains lysate; Then under magnetic stirring by above-mentioned Na 2wO 4lysate dropwise joins above-mentioned Bi (NO 3) 3in dispersion liquid, obtain suspension, and after regulating pH of suspension to 5 ~ 9 to stir, suspension is transferred in autoclave, put into electric heating constant-temperature blowing drying box 120 ~ 180 DEG C of heat treatment 12 ~ 36h, then reactor is cooled to room temperature, the Bi of three-dimensional layering club shaped structure can be obtained through suction filtration, washing and 40 ~ 80 DEG C of drying 2 ~ 10h 2wO 6; Wherein, Bi (NO 3) 35H 2o and Na 2wO 42H 2the ratio of the amount of substance of O is 2:1;
(2) Bi 2wO 6/ Ag 3pO 4the preparation of heterojunction composite photocatalyst: by the Bi obtained in step (1) 2wO 6be scattered in ultra-pure water and obtain dispersion liquid, then add AgNO under magnetic stirring 3, be stirred to and dissolve to obtain mixed liquor completely, then dropwise add the precursor solution of phosphorous acid group, continue lucifuge afterwards and stir 2 ~ 8h, can Bi be obtained through suction filtration, washing and 40 ~ 80 DEG C of vacuum drying 2 ~ 10h 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst; Wherein, phosphate radical and AgNO in the precursor of phosphorous acid group 3the ratio of the amount of substance of middle silver ion is 1:3.
4. Bi according to claim 3 2wO 6/ Ag 3pO 4the preparation method of heterojunction composite photocatalyst, is characterized in that: regulate suspension pH value to adopt concentration to be the NH of 0.1 ~ 5.0mol/L in described step (1) 3h 2o or NaOH.
5. Bi according to claim 3 2wO 6/ Ag 3pO 4the preparation method of heterojunction composite photocatalyst, is characterized in that: in described step (2), the precursor of phosphorous acid group is Na 2hPO 4, NaH 2pO 4, Na 3pO 4, K 2hPO 4, KH 2pO 4or K 3pO 4one wherein.
6. Bi according to claim 3 2wO 6/ Ag 3pO 4the preparation method of heterojunction composite photocatalyst, is characterized in that: Bi in described step (2) 2wO 6with the AgNO added 3the ratio of amount of substance be 1:0.3 ~ 15.
7. a kind of Bi according to claim 3 2wO 6/ Ag 3pO 4the preparation method of heterojunction composite photocatalyst, is characterized in that: disperse to be adopt ultrasonic disperse 10 ~ 60min, then magnetic agitation 10 ~ 60min in described step (1) and step (2).
8. a Bi according to claim 1 2wO 6/ Ag 3pO 4the application of heterojunction composite photocatalyst, is characterized in that: described Bi 2wO 6/ Ag 3pO 4heterojunction composite photocatalyst is as the bactericide in water body.
9. a Bi according to claim 1 2wO 6/ Ag 3pO 4the application of heterojunction composite photocatalyst, is characterized in that: described Bi 2wO 6/ Ag 3pO 4the application of heterojunction composite photocatalyst in degradation of dye.
10. a Bi according to claim 1 2wO 6/ Ag 3pO 4the application of heterojunction composite photocatalyst, is characterized in that: described Bi 2wO 6/ Ag 3pO 4the application of heterojunction composite photocatalyst in water body purification.
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