CN105289666A - Bi2WO6/BiOI composite photocatalysis bactericide and preparation method thereof - Google Patents

Bi2WO6/BiOI composite photocatalysis bactericide and preparation method thereof Download PDF

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CN105289666A
CN105289666A CN201510789973.2A CN201510789973A CN105289666A CN 105289666 A CN105289666 A CN 105289666A CN 201510789973 A CN201510789973 A CN 201510789973A CN 105289666 A CN105289666 A CN 105289666A
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bactericide
bioi
catalysis
composite photo
preparation
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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/BiOI composite photocatalysis bactericide and its preparation method. The Bi2WO6/BiOI composite photocatalysis bactericide is a three-dimensional layered flower-like structured catalyst composed of Bi2WO6 and BiOI, wherein the molar ratio of Bi2WO6 to BiOI is 1:0.01-100. According to the preparation method, the three-dimensional layered flower-like structured Bi2WO6/BiOI composite photocatalysis bactericide is prepared under the hydrothermal condition by a one-step coprecipitation method. The preparation method of the invention has a simple process, is easy to control and is low-cost. A Bi2WO6/BiOI 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/BiOI composite photocatalysis bactericide has high-efficiency photocatalytic activity and stability in visible light, has a highly-efficient killing effect on harmful microbes 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/ BiOI composite photo-catalysis bactericide and preparation method thereof
Technical field
The invention belongs to photocatalysis field, be specifically related to a kind of Bi 2wO 6/ BiOI composite photo-catalysis bactericide and preparation method thereof.
Background technology
Sustainable development is world today's question of common concern.But the problem such as energy shortage, environmental pollution is day by day serious.Various noxious pollutant is constantly put aside in the environment such as water body, soil and air, migration and conversion, the heavy damage ecological balance, also endangers the life of the mankind with healthy.In addition, economic development needs to consume a large amount of energy, is causing new energy crisis, and a large amount of exploitation and use traditional mineral products energy inherently can cause serious environmental problem.
Semiconductor light-catalyst has huge potentiality in the solution energy and environment.One, low-density solar energy can be converted into highdensity chemical energy or electric energy by conductor photocatalysis material, its two, the oxide species that semiconductor light-catalyst produces under light illumination can be degraded the organic pollution in air and water body.The development of photochemical catalyst is the key that photocatalysis technology is applied.N-type semiconductor TiO is utilized since Fujishima and Honda in 1972 reports 2electrode is since under UV-irradiation, decomposition water prepares hydrogen and oxygen, and Photocatalitic Technique of Semiconductor receives increasing concern [1].In recent years, photocatalysis technology all has huge using value at the numerous areas of environmental pollution improvement, and the application as the fields such as degerming and sewage disposal of keeping a public place clean in indoor air purification, public place is extensively approved and pays close attention to.At present, TiO 2because the advantages such as its stable chemical nature, nontoxic, low cost become most popular catalysis material, but due to TiO 2also also exist as high in photo-generate electron-hole recombination rate, visible ray utilization rate is low and reclaim difficulty etc. defect, greatly limit TiO 2application [2].Therefore, in order to realize effective utilization of solar energy, exploitation and design have novel photocatalysis material that is visible light-responded, environmental protection and have important practical significance.
Bismuth based material is because it to have good photocatalysis performance and pattern diversity in visible ray (λ >420nm) district by extensive concern and further investigation, and the composite that bismuth and other metals are formed also has good visible light catalytic performance [3-6].As BiOX (BiOX (X=Cl, Br, I)), having cubic crystalline structure, is by [Bi 2o 2] lamella and two-layer halogens be alternately arranged and formed laminar structured, wherein BiOI has good absorption because having minimum energy gap (1.77 ~ 1.92eV) in visible region [3], receive the extensive concern of researcher.In addition, Bi 2wO 6it is one the simplest Aurivillius type oxide, it is a kind of N-shaped direct semiconductor material, there is narrower energy gap (about 2.7eV), under visible ray shines, there is higher catalytic activity, in the depollution of environment and new energy development field, there is potential using value, become one of photochemical catalyst of extensively research at present [4].But because photoelectron in monomer photochemical catalyst-hole is separated comparatively slow, the easy compound of photo-generated carrier, causes photocatalysis performance limited, and can accelerate electron-hole separation by semiconductors coupling structure composite, improves the photocatalysis performance of material [5,6].Therefore, a kind of composite catalyst is now needed.
[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]X.Xiao,W.D.Zhang,FacilesynthesisofnanostructuredBiOImicrosphereswithhighvisiblelight-inducedphotocatalyticactivity[J].JournalofMaterialsChemistry,2010,20:5866-5870.
[4]X.F.Cao,L.Zhang,X.T.Chen,Z.L.Xue.Microwave-assistedsolution-phasepreparationofflower-likeBi 2WO 6anditsvisible-light-drivenphotocatalyticproperties[J].CrystEngComm,2011,13(1):306-311.
[5]Y.Y.Li,J.S.Wang,H.C.Yao,L.Y.Dang,Z.J.Li,ChemicaletchingpreparationofBiOI/Bi 2O 3heterostructureswithenhancedphotocatalyticactivities[J].CatalysisCommunications,2011,12:660-664.
[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.
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/ BiOI composite photo-catalysis bactericide and preparation method thereof.
For achieving the above object, the present invention implements by the following technical solutions,
A kind of Bi 2wO 6/ BiOI composite photo-catalysis bactericide, by Bi 2wO 6with the catalyst with three-dimensional layering flower-like structure that BiOI is formed; Wherein, Bi 2wO 6be 1:0.01 ~ 100 with the mol ratio of BiOI.
Described Bi 2wO 6be 1:0.02 ~ 50 with the mol ratio of BiOI.
A kind of Bi 2wO 6the preparation method of/BiOI composite photo-catalysis bactericide: by Bi (NO 3) 35H 2o is scattered in absolute ethyl alcohol, obtains dispersion liquid, then will add NaOH solution to above-mentioned dispersion liquid, and obtain mixed liquor A; Simultaneously by Na 2wO 42H 2o and KI joins in ultra-pure water, and magnetic agitation, to dissolving completely, obtains lysate B; Then under magnetic stirring above-mentioned lysate B is dropwise joined in above-mentioned mixed liquor A, obtain suspension, after continuing to stir, suspension is transferred in autoclave, puts into electric heating constant-temperature blowing drying box heat treatment; Then reactor is cooled to room temperature, the Bi with three-dimensional layering flower-like structure can be obtained through suction filtration, washing and drying 2wO 6/ BiOI composite photo-catalysis bactericide; Wherein, above-mentioned Na 2wO 42H 2the ratio of the amount of substance of O and KI is 1:0.02 ~ 50, above-mentioned Bi (NO 3) 35H 2o and Na 2wO 42H 2the ratio of the amount of substance of O is 2:1, above-mentioned Bi (NO 3) 35H 2the ratio of the amount of substance of O and KI is 1:1.
Described dispersion adopts ultrasonic disperse 10 ~ 60min.
Described NaOH and Bi (NO 3) 35H 2the ratio of the amount of substance of O is 1 ~ 10:1.
Described being dropwise added drop-wise to by lysate B in mixed liquor A continues stirring 30 ~ 90min afterwards.
Heat treatment temperature in described electric heating constant-temperature blowing drying box is 120 ~ 200 DEG C, and the reaction time is 12 ~ 36h.
Described baking temperature is 40 ~ 80 DEG C, and drying time is 2 ~ 10h.
A kind of Bi 2wO 6the application of/BiOI composite photo-catalysis bactericide, described Bi 2wO 6/ BiOI composite photo-catalysis bactericide is as the application of photochemical catalyst or bactericide.
Described Bi 2wO 6/ BiOI composite photo-catalysis bactericide is as the application of the photochemical catalyst in water body purification or bactericide.
A kind of Bi 2wO 6the application of/BiOI composite photo-catalysis bactericide, described Bi 2wO 6the application of/BiOI composite photo-catalysis bactericide in water body purification.
Bi 2wO 6/ BiOI composite photo-catalysis bactericide is applied in water body, kills the visible light catalytic of harmful microorganism pseudomonas aeruginosa (P.aeruginosa), and adopt 500W xenon lamp as light source, its wave-length coverage is 420 ~ 760nm; Described microorganism concn is 10 6cfu/mL; Described Bi 2wO 6the consumption of/BiOI composite photo-catalysis bactericide 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; Microbial solution is joined in reactor, then add Bi 2wO 6/ BiOI composite photo-catalysis bactericide, dark adsorption starts illumination after reaching balance, and in During Illumination, separated in time sampling, measures surviving bacteria concentration by colony counting method, calculates killing rate.Described light source is xenon lamp, and its wave-length coverage is 420 ~ 760nm; Described microorganism concn is 10 6cfu/mL; Described Bi 2wO 6the consumption of/BiOI composite photo-catalysis bactericide is 1.0mg/mL.
Beneficial effect of the present invention is:
The present invention passes through Bi 2wO 6build the composite with heterojunction structure with BiOI compound, accelerate the separation of photo-generated carrier at composite material surface, and then improve photocatalysis performance, to Bi 2wO 6be significant with the practical application of BiOI bi-material in photocatalysis field; Concrete:
(1) the present invention adopts simple hydro-thermal method one-step synthesis Bi 2wO 6/ BiOI composite photo-catalysis bactericide, preparation method's technique is simple, is easy to control, with low cost;
(2) Bi with three-dimensional flower-shaped structure that prepared by the present invention 2wO 6/ BiOI composite photo-catalysis bactericide, has larger specific area and good visible absorption performance;
(3) Bi for preparing of the present invention 2wO 6/ BiOI composite photo-catalysis bactericide visible light catalysis activity compares Bi 2wO 6all be significantly increased with BiOI, under 500W xenon lamp irradiates, 1.0mg/mLBi 2wO 6/ BiOI composite photo-catalysis bactericide is 10 to concentration 6in the microorganism 60min of cfu/mL, killing rate can reach 99.99%;
(4) Bi for preparing of the present invention 2wO 6/ BiOI composite photo-catalysis bactericide has good stability and reusing, still has efficient photocatalytic activity after recycling for 6 times;
(5) Bi for preparing of the present invention 2wO 6/ BiOI composite photo-catalysis bactericide 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 the 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));
The FESEM photo of Fig. 2 sample prepared by the present invention: (A) BiOI, (B) Bi 2wO 6, (C, D) Bi 2wO 6/ BiOI-1;
(wherein abscissa is Wavelength (wavelength) to the UV-DRS collection of illustrative plates of Fig. 3 sample prepared by the present invention, and unit is degree (degree); Ordinate is Absorbance (absorbance), and unit is a.u. (absolute unit));
The sample visible ray of Fig. 4 prepared by the present invention is according to the lower sterilizing rate to pseudomonas aeruginosa (ordinate is Antibacterialrate (sterilizing rate), and unit is %);
Fig. 5 is the Bi of preparation in the embodiment of the present invention 1 2wO 6(wherein in A figure, abscissa is Cyclenumber (reusing number of times) for sterilizing rate (A) after/BiOI-1 composite photo-catalysis bactericide 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); 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 the Bi with three-dimensional layering flower-like structure by simple hydrothermal synthesis method one step 2wO 6/ BiOI composite photo-catalysis bactericide, this composite photo-catalysis bactericide 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, to harmful microorganism in water body, there is efficient killing 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:
Bi 2wO 6the preparation method of/BiOI composite photo-catalysis bactericide:
Prepared by hydrothermal synthesis method.Take 3.0mmolBi (NO 3) 35H 2o joins in 30.0mL absolute ethyl alcohol, and ultrasonic disperse 30min, obtains dispersion liquid, then will add 20mL0.75mol/LNaOH solution to above-mentioned dispersion liquid, and obtain mixed liquor A; Simultaneously by 1.0mmolNa 2wO 42H 2o and 1.0mmolKI joins in 30.0mL ultra-pure water, and magnetic agitation makes it dissolve completely, obtains lysate B; Then under magnetic stirring above-mentioned lysate B is dropwise joined in above-mentioned mixed liquor A, obtain suspension, continue 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 180 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 flower-like structure 2wO 6/ BiOI composite photo-catalysis bactericide, is designated as Bi 2wO 6/ BiOI-1 (see Fig. 1-3).
Comparative example 1:
The preparation method of monomers B iOI:
Take 1.0mmolBi (NO 3) 35H 2o joins in 30.0mL absolute ethyl alcohol, and ultrasonic disperse 30min, obtains dispersion liquid, then will add 20mL0.75mol/LNaOH solution to above-mentioned dispersion liquid, and obtain mixed liquor A; Joined by 1.0mmolKI in 30.0mL ultra-pure water, magnetic agitation makes it dissolve completely simultaneously, obtains lysate B; Then under magnetic stirring above-mentioned lysate B is dropwise joined in above-mentioned mixed liquor A, obtain suspension, continue 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 180 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 BiOI monomer material, be designated as BiOI (see Fig. 1-3).
Comparative example 2:
Monomers B i 2wO 6preparation method:
Take 2.0mmolBi (NO 3) 35H 2o joins in 30.0mL absolute ethyl alcohol, and ultrasonic disperse 30min, obtains dispersion liquid, then will add 20mL0.75mol/LNaOH solution to above-mentioned dispersion liquid, and obtain mixed liquor A; Simultaneously by 1.0mmolNa 2wO 42H 2o joins in 30.0mL ultra-pure water, and magnetic agitation makes it dissolve completely, obtains lysate B; Then under magnetic stirring above-mentioned lysate B is dropwise joined in above-mentioned mixed liquor A, obtain suspension, continue 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 180 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 Bi 2wO 6monomer material, is designated as Bi 2wO 6(see Fig. 1-3).
As shown in Figure 1, a curve is the XRD collection of illustrative plates of monomers B iOI prepared by comparative example 1, and position and the standard card JCPDSNo.73-2062 of all diffraction maximums fit like a glove, and all belong to the BiOI of tetragonal crystal system, and do not occur any impurity phase.B curve is monomers B i prepared by comparative example 2 2wO 6xRD collection of illustrative plates, diffraction maximums all in figure all with the orthorhombic system Bi of standard 2wO 6it is corresponding that (JCPDSNo.39-0256, the diffraction maximum without any impurity phase occurs, shows that sample prepared by comparative example 1 is pure monoclinic phase Bi 2wO 6.C curve in Fig. 1 is Bi prepared by embodiment 1 2wO 6the XRD collection of illustrative plates of/BiOI-1 composite photo-catalysis bactericide, contains Tetragonal BiOI and oblique side phase Bi in collection of illustrative plates 2wO 6all characteristic diffraction peaks, Bi is described 2wO 6successfully be combined with each other with BiOI and define composite.In the XRD collection of illustrative plates of composite, there are not other impurity peaks, illustrate in composite just by Bi 2wO 6with BiOI two kinds of material compositions, other impurity phases do not exist.
From Fig. 2 (A), monomers B iOI prepared by comparative example 1 is layering flower-like structure, and diameter is about 3 μm, is piled up form by the two-dimensional nano thin slice of many rules.From Fig. 2 (B), monomers B i prepared by comparative example 1 2wO 6for the nanometer sheet of rule, size is about 500nm, and thickness is about 20nm, and the accumulation of these nanometer sheet intersects, but does not form three-dimensional structure.The Bi that Fig. 2 (C) and Fig. 2 (D) is prepared for embodiment 1 2wO 6/ BiOI-1 composite photo-catalysis bactericide, as seen from the figure, Bi 2wO 6/ BiOI-1 composite photo-catalysis bactericide is three-dimensional layering flower-like structure, and diameter is about 3 μm, is about 500nm by many sizes, and the two-dimensional nano thin slice accumulation that thickness is about 20nm assembles.
As seen from Figure 3, Bi 2wO 6, BiOI and Bi 2wO 6/ BiOI-1 composite all has good absorption at ultraviolet region and visible region, shows good visible absorption performance.Bi 2wO 6the light abstraction width of/BiOI-1 can arrive about 600nm, and BiOI and the Bi with good visible absorption performance is described 2wO 6substantially increase the visible absorption performance of composite after compound, make it in photocatalysis, have good application prospect.
Embodiment 2:
Bi 2wO 6the preparation method of/BiOI composite photo-catalysis bactericide:
Prepared by hydrothermal synthesis method, difference from Example 1 is, control Bi 2wO 6be 1:2 with the mol ratio of BiOI.Take 3.0mmolBi (NO 3) 35H 2o joins in 30.0mL absolute ethyl alcohol, and ultrasonic disperse 30min, obtains dispersion liquid, then will add 20mL0.75mol/LNaOH solution to above-mentioned dispersion liquid, and obtain mixed liquor A; Simultaneously by 0.75mmolNa 2wO 42H 2o and 1.5mmolKI joins in 30.0mL ultra-pure water, and magnetic agitation makes it dissolve completely, obtains lysate B; Then under magnetic stirring above-mentioned lysate B is dropwise joined in above-mentioned mixed liquor A, obtain suspension, continue 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 180 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 Bi 2wO 6/ BiOI composite photo-catalysis bactericide, is designated as Bi 2wO 6/ BiOI-2.
Embodiment 3:
Bi 2wO 6the preparation method of/BiOI composite photo-catalysis bactericide:
Prepared by hydrothermal synthesis method, difference from Example 1 is, control Bi 2wO 6be 1:3 with the mol ratio of BiOI.Take 3.0mmolBi (NO 3) 35H 2o joins in 30.0mL absolute ethyl alcohol, and ultrasonic disperse 30min, obtains dispersion liquid, then will add 20mL0.75mol/LNaOH solution to above-mentioned dispersion liquid, and obtain mixed liquor A; Simultaneously by 0.6mmolNa 2wO 42H 2o and 1.8mmolKI joins in 30.0mL ultra-pure water, and magnetic agitation makes it dissolve completely, obtains lysate B; Then under magnetic stirring above-mentioned lysate B is dropwise joined in above-mentioned mixed liquor A, obtain suspension, continue 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 180 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 Bi 2wO 6/ BiOI composite photo-catalysis bactericide, is designated as Bi 2wO 6/ BiOI-3.
Embodiment 4:
Bi 2wO 6the preparation method of/BiOI composite photo-catalysis bactericide:
Prepared by hydrothermal synthesis method, difference from Example 1 is, control Bi 2wO 6be 1:4 with the mol ratio of BiOI.Take 3.0mmolBi (NO 3) 35H 2o joins in 30.0mL absolute ethyl alcohol, and ultrasonic disperse 30min, obtains dispersion liquid, then will add 20mL0.75mol/LNaOH solution to above-mentioned dispersion liquid, and obtain mixed liquor A; Simultaneously by 0.5mmolNa 2wO 42H 2o and 2.0mmolKI joins in 30.0mL ultra-pure water, and magnetic agitation makes it dissolve completely, obtains lysate B; Then under magnetic stirring above-mentioned lysate B is dropwise joined in above-mentioned mixed liquor A, obtain suspension, continue 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 180 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 Bi 2wO 6/ BiOI composite photo-catalysis bactericide, is designated as Bi 2wO 6/ BiOI-4.
Embodiment 5:
Bi 2wO 6the preparation method of/BiOI composite photo-catalysis bactericide:
Prepared by hydrothermal synthesis method, difference from Example 1 is, control Bi 2wO 6be 1:0.5 with the mol ratio of BiOI.Take 3.0mmolBi (NO 3) 35H 2o joins in 30.0mL absolute ethyl alcohol, and ultrasonic disperse 30min, obtains dispersion liquid, then will add 20mL0.75mol/LNaOH solution to above-mentioned dispersion liquid, and obtain mixed liquor A; Simultaneously by 1.2mmolNa 2wO 42H 2o and 0.6mmolKI joins in 30.0mL ultra-pure water, and magnetic agitation makes it dissolve completely, obtains lysate B; Then under magnetic stirring above-mentioned lysate B is dropwise joined in above-mentioned mixed liquor A, obtain suspension, continue 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 180 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 Bi 2wO 6/ BiOI composite photo-catalysis bactericide, is designated as Bi 2wO 6/ BiOI-0.5.
Application examples 1:
Above-mentioned gained Bi 2wO 6/ BiOI composite photo-catalysis bactericide 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, 1.7 × 10 8cfu/mL) Bi is evaluated 2wO 6the visible light catalytic bactericidal property of/BiOI composite photo-catalysis bactericide:
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 1.7 × 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) in contrast.
As seen from Figure 4, in blank assay, pseudomonas aeruginosa number has almost no change, and shows that the impact of visible ray photograph can be ignored; And under dark condition, number of bacteria, also without significant change, shows that the material itself that this experiment uses does not have bio-toxicity.And visible ray according under Bi 2wO 6/ BiOI-1 composite photo-catalysis bactericide shows good photocatalytic activity, and photo-catalyst performance is obviously better than monomers B i 2wO 6and BiOI, can 99.99% be reached through 60min sterilizing rate.Therefore, Bi 2wO 6/ BiOI-1 composite photo-catalysis bactericide has splendid photo-catalyst performance, is attributable to BiOI and 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/ BiOI-1 composite photo-catalysis bactericide 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 2:
Above-mentioned gained Bi 2wO 6/ BiOI composite photo-catalysis bactericide repeated application, in water body, is killed the visible ray of harmful microorganism pseudomonas aeruginosa:
By Bi used in photo-catalyst in application examples 1 2wO 6/ BiOI-1 composite photo-catalysis bactericide 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 1.
From Fig. 5 (A), Bi 2wO 6/ BiOI-1 composite photo-catalyst 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/ BiOI-1 composite photo-catalysis bactericide 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 6the crystal structure of/BiOI-1 composite photo-catalysis bactericide, 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 (10)

1. a Bi 2wO 6/ BiOI composite photo-catalysis bactericide, is characterized in that: Bi 2wO 6/ BiOI composite photo-catalysis bactericide is by Bi 2wO 6with the catalyst with three-dimensional layering flower-like structure that BiOI is formed; Wherein, Bi 2wO 6be 1:0.01 ~ 100 with the mol ratio of BiOI.
2. Bi according to claim 1 2wO 6/ BiOI composite photo-catalysis bactericide, is characterized in that: described Bi 2wO 6be 1:0.02 ~ 50 with the mol ratio of BiOI.
3. a Bi according to claim 1 2wO 6the preparation method of/BiOI composite photo-catalysis bactericide, is characterized in that: by Bi (NO 3) 35H 2o is scattered in absolute ethyl alcohol, obtains dispersion liquid, then will add NaOH solution to above-mentioned dispersion liquid, and obtain mixed liquor A; Simultaneously by Na 2wO 42H 2o and KI joins in ultra-pure water, and magnetic agitation, to dissolving completely, obtains lysate B; Then under magnetic stirring above-mentioned lysate B is dropwise joined in above-mentioned mixed liquor A, obtain suspension, after continuing to stir, suspension is transferred in autoclave, puts into electric heating constant-temperature blowing drying box heat treatment; Then reactor is cooled to room temperature, the Bi with three-dimensional layering flower-like structure can be obtained through suction filtration, washing and drying 2wO 6/ BiOI composite photo-catalysis bactericide; Wherein, Na 2wO 42H 2the ratio of the amount of substance of O and KI is 1:0.02 ~ 50, Bi (NO 3) 35H 2o and Na 2wO 42H 2the ratio of the amount of substance of O is 2:1, Bi (NO 3) 35H 2the ratio of the amount of substance of O and KI is 1:1.
4. Bi according to claim 3 2wO 6the preparation method of/BiOI composite photo-catalysis bactericide, is characterized in that: described dispersion adopts ultrasonic disperse 10 ~ 60min.
5. Bi according to claim 3 2wO 6the preparation method of/BiOI composite photo-catalysis bactericide, is characterized in that: described NaOH and Bi (NO 3) 35H 2the ratio of the amount of substance of O is 1 ~ 10:1.
6. Bi according to claim 3 2wO 6the preparation method of/BiOI composite photo-catalysis bactericide, is characterized in that: described being dropwise added drop-wise to by lysate B in mixed liquor A continues stirring 30 ~ 90min afterwards.
7. Bi according to claim 3 2wO 6the preparation method of/BiOI composite photo-catalysis bactericide, is characterized in that: the heat treatment temperature in described electric heating constant-temperature blowing drying box is 120 ~ 200 DEG C, and the reaction time is 12 ~ 36h.
8. Bi according to claim 3 2wO 6the preparation method of/BiOI composite photo-catalysis bactericide, is characterized in that: described baking temperature is 40 ~ 80 DEG C, and drying time is 2 ~ 10h.
9. a Bi according to claim 1 2wO 6the application of/BiOI composite photo-catalysis bactericide, is characterized in that: described Bi 2wO 6/ BiOI composite photo-catalysis bactericide is as the application of photochemical catalyst or bactericide.
10. a Bi according to claim 1 2wO 6the application of/BiOI composite photo-catalysis bactericide, is characterized in that: described Bi 2wO 6the application of/BiOI composite photo-catalysis bactericide in water body purification.
CN201510789973.2A 2015-11-17 2015-11-17 Bi2WO6/BiOI composite photocatalysis bactericide and preparation method thereof Pending CN105289666A (en)

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CN113289610A (en) * 2021-03-18 2021-08-24 合肥工业大学 Bi2WO6/Si composite photoelectrocatalysis anode material and preparation method thereof

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Application publication date: 20160203