CN103623803A - Visible light photocatalyst and preparation method therefor - Google Patents

Visible light photocatalyst and preparation method therefor Download PDF

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CN103623803A
CN103623803A CN201210313414.0A CN201210313414A CN103623803A CN 103623803 A CN103623803 A CN 103623803A CN 201210313414 A CN201210313414 A CN 201210313414A CN 103623803 A CN103623803 A CN 103623803A
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visible
solution
semi
light photocatalyst
lower transition
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孙卓
潘丽坤
刘心娟
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SUZHOU JINGNENG TECHNOLOGY Co Ltd
Najing Science & Technology Co Ltd Shanghai
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SUZHOU JINGNENG TECHNOLOGY Co Ltd
Najing Science & Technology Co Ltd Shanghai
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Abstract

Provided is a visible light photocatalyst and a preparation method therefor. The visible light photocatalyst comprises down conversion materials and semiconductor materials. The mass percent of the down conversion materials to the semiconductor materials is 0.5%-5%. The visible light photocatalyst with down conversion functions is advantaged by high visible light catalytic degradation rate, no pollution, simple preparation method and low cost. The invention also provides a preparation method for the visible light photocatalyst with down conversion functions.

Description

A kind of visible-light photocatalyst and preparation method thereof
Technical field
The present invention relates to a kind of visible-light photocatalyst, be specifically related to a kind of visible-light photocatalyst with lower translation function and preparation method thereof.
Background technology
Along with industrial expansion, the becoming increasingly conspicuous of environmental problem, the method for seeking effectively to remove organic pollution has been extremely urgent eager task, causes national governments and people's great attention.Photocatalitic Technique of Semiconductor, as a kind of novel depollution of environment and energy conversion technology, has been shown wide application prospect in fields such as producing hydrogen, water treatment, various organic matter degradation and air cleaning.This technology has the following advantages: under illumination, can directly react, can effectively destroy many constitutionally stable bio-refractory organic pollutions, make them be degraded to carbon dioxide and water etc.; Oxidability is strong, and degraded thoroughly, not selective to pollutant, any organic matter of almost can degrading, and non-secondary pollution; Energy consumption is low, easy and simple to handle, and catalyst can reuse etc.Therefore, Photocatalitic Technique of Semiconductor is flourish and be expected to become 21 century environmental pollution and control and the desirable technique of administering at nearly 30 years, and more and more causes researcher's attention.
Semiconductor TiO 2have that specific area is large, active good, nontoxic, cheap, the stable chemical nature of ultraviolet light photocatalysis, the feature such as oxidation-reduction quality is strong, cost is low, become the photochemical catalyst that has potential application most, and be proved to be very effective aspect degradation water, airborne organic pollution.But, TiO 2energy gap be approximately 3.2 eV, only can be by ultraviolet excitation, and ultraviolet light approximately only accounts for 4% left and right of sunshine gross energy.In order to effectively utilize solar energy, find the corresponding photochemical catalyst of visible ray, become one of hot issue of photocatalysis field research.
Light-converting material is a kind of luminescent material that can send high energy (low energy) photon under low energy (high energy) photon excitation.Recently, semi-conducting material and light-converting material, in conjunction with forming new photochemical catalyst, cause the concern of researcher in photocatalysis field.
Patent 1(CN101642702) a kind of ruddiness being comprised of semiconductor and up-conversion or infrared light catalytic material are disclosed.This catalyst is to absorb low energy ruddiness or infrared light by up-conversion, transmitting high energy ultraviolet light, thus vitalizing semiconductor is realized infrared light catalysis.
Patent 2(CN102078807A) a kind of load Er is disclosed 3+: YAlO 3/ TiO 2photochemical catalyst and preparation method thereof.This material is by Er 3+: YAlO 3tiO 2powder load is to the surface of spherical activated charcoal, degradable organic pollutant under radiation of visible light.
Patent 3(CN1792424) a kind of supported titanium that luminescent material is carrier of take is disclosed 2photochemical catalyst and preparation method and application, the carrier of this catalyst is luminescent material SrAl 2o 4-: Eu 2+, Dy 3+.Under UV-irradiation, SrAl 2o 4-: Eu 2+, Dy 3+in Dy 3+and the trap level that lattice defect forms can be caught TiO 2light induced electron, reduce electron-hole recombination rate, thereby greatly improved TiO 2the catalytic activity of photochemical catalyst.
Patent 4(CN1712126) a kind of energy accumulated catalysis material is disclosed.Accumulation of energy long after glow luminous material and catalysis material are combined, improve photocatalysis effect, realize the catalytic degradation function under unglazed photograph.
Patent 5(CN1712126) a kind of novel composite energy accumulated catalysis material and preparation method thereof is disclosed.This material is that visible-light photocatalysis material BiOCl is prepared with Hydrolyze method original position on long-afterglow material surface, under making it to irradiate at visible ray or without outer light source, all has efficient catalytic degradation effect.
Above-mentioned patent documentation 1 and 2, article up-conversion and the compound new photochemical catalyst obtaining of semi-conducting material.Patent 1 has been utilized the upper conversion function of luminescent material, has realized infrared light catalysis.Although patent 2 has been utilized up-conversion, do not mention translation function.What in addition, patent documentation 3-5 adopted is the new photochemical catalyst of long-afterglow material and the compound composition of semiconductor.But patent 3 is not mentioned the accumulation of energy function of long-afterglow material.At present, in visible light catalytic field, utilize the lower translation function of luminescent material to improve visible light catalytic performance, so far there are no reports.Lower transition material is under the photon excitation of high energy, the material of transmitting lower energy photon.If by lower transition material and semi-conducting material combination, form new photochemical catalyst, the photon of lower transition material transmitting can vitalizing semiconductor or organic matter, improves semi-conductive photocatalysis or organic from degraded, and then improves visible light catalytic efficiency.Therefore, under a kind of simple efficient tool, the visible-light photocatalyst of translation function urgently occurs.
Summary of the invention
The object of the invention is for the problems referred to above, a kind of visible light catalyst with lower translation function is provided, have that photocatalytic activity is high, pollution-free, preparation method is simple, low cost and other advantages.
For achieving the above object, technical scheme provided by the invention is: a kind of visible-light photocatalyst, it is characterized in that, and described visible-light photocatalyst comprises lower transition material and semi-conducting material, the mass ratio of described lower transition material and semi-conducting material is 0.5% ~ 5%.
Preferably, described visible-light photocatalyst comprises lower transition material and semi-conducting material, described lower transition material and with the mass ratio of semi-conducting material be 1% ~ 4%.
Preferably, described visible-light photocatalyst comprises lower transition material and semi-conducting material, and the mass ratio of described lower transition material and semi-conducting material is 1.5% ~ 3%.
Preferably, described semi-conducting material is ZnO, TiO 2, SnO 2, ZrO 2, Co 3o 4, Fe 3o 4, La 2o 3, Ni (OH) 2, In 2tiO 5, BiOCl, BiOF, BiPO 4, CdMoO 4, CdWO 4, La 2sn 2o 7, La 2ti 2o 7, LaCoO 3, PbMoO 4, PbSb 2o 6, PbWO 4, Sr 2ta 2o 7, SrTiO 3, SrWO 4, ZnMoO 4, ZnSb 2o 6, ZnWO 4, WO 3, Cu 2o, In 2o 3, ZnS, CdS, CdSe, Bi 2o 3, BiOI, BiVO 4, BiWO 4, Bi 2moO 6, InVO 4, InNbO 4, Ag 3pO 4, AgCl, AgBr, AgI, MoO 3, MoS 2in one or more.
Preferably, doping vario-property material in described semi-conducting material, described material modified be one or more in Au, Ag, Graphene, CNT, the described material modified mass fraction adulterating in semi-conducting material is 0.5-2%.
Preferably, described lower transition material comprises one or more in garnet structure fluorescent material, non-garnet structure oxide fluorescent powder, sulphide fluorescent material, nitride and oxygen nitrogen fluorescent material.
Preferably, described garnet structure fluorescent material is Y 3al 5o 12: Ce 3+, Tb 3al 5o 12: Ce 3+, Lu 3al 5o 12: Ce 3+, Lu 2caMg 2(Si, Ge) 3o 12: Ce 3+, Ca 3sc 2si 3o 12: Ce 3+in one or more; Described non-garnet structure oxide fluorescent powder is Sr 2siO 4: Eu 2+, LiSrPO 4: Eu 2+, Sr 3siO 5: Eu 2+, Sr 3siO 5: Ce 3+, Li +, Li 2srSiO 4: Eu 2+, LaSr 2alO 5: Ce 3+, Ca 2bO 3cl:Eu 2+, Sr 3(Al 2o 5) C l2: Eu 2+in one or more; Described sulphide fluorescent material is CaS:Eu 2+, SrS:Eu 2+ce 3+, Ca 2siS 4: Eu 2+, Y 2o 2s:Eu 2+, (Ca, Sr) S:Eu 2+in one or more; Described nitride and oxygen nitrogen fluorescent material are MSi 2o 2n 2: Eu 2+, Ba 3si 6o 12n 2: Eu 2+, SrSi 5alO 2n 7: Eu 2+, SrSiAl 2o 3n 2: Eu 2+, CaAlSiN 3: Eu 2+, M 2si 5n 8: Eu 2+, MSiN 2: Eu 2+in one or more, M=Ca wherein, Sr, Ba.
A preparation method for visible-light photocatalyst, is characterized in that, described preparation method comprises the following steps:
(1), according to the proportioning of claim 1, weigh lower transition material and/or material modified; (2) load weighted material is joined in the salting liquid of 0.05-0.2 mol/l of 10-20 ml, solution is put in the microwave tube of 35 ml, stir 0.5-1 hour at 25-35 ℃, make solution even; (3) drip Na (OH) 2solution, makes the pH value of solution between 7-9, stirs 0.5-1 hour at room temperature 25-35 ℃; (4) solution being stirred is put in microwave reaction synthesizer, under temperature 110-160 ℃ and power 80-150 W condition, reacted and obtain composite photo-catalyst after 10-30 minute.
The invention has the beneficial effects as follows, visible-light photocatalyst of the present invention has higher organic removal rate.Lower transition material is under the photon excitation of high energy, the material of transmitting lower energy photon.The present invention, by lower transition material and semi-conducting material combination, forms new photochemical catalyst.Its mechanism is: in light-catalyzed reaction process, under excited by visible light, lower transition material can be launched photon, vitalizing semiconductor or organic matter produce electron-hole pair, organic matter is degraded, thereby improve semi-conductive photocatalysis or organic from degraded, improve visible light catalytic efficiency.Compared with prior art, have that visible light photocatalytic degradation rate is high, pollution-free, preparation method is simple, low cost and other advantages, is conducive to light-catalysed scale application and universalness.
Accompanying drawing explanation
Fig. 1 is the photocatalysis efficiency figure of the embodiment of the present invention 1.
Fig. 2 is the photocatalysis efficiency figure of the embodiment of the present invention 2.
Fig. 3 is the photocatalysis efficiency figure of the embodiment of the present invention 3.
Fig. 4 is the photocatalysis efficiency figure of the embodiment of the present invention 4.
Fig. 5 is the photocatalysis efficiency figure of the embodiment of the present invention 5.
Fig. 6 is the photocatalysis efficiency figure of the embodiment of the present invention 6.
Fig. 7 is the photocatalysis efficiency figure of the embodiment of the present invention 7.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that, after having read content of the present invention, those skilled in the art can make various changes or modifications the present invention, these equivalent form of values fall within equally the application the scope that limits of attached claims.
A kind of visible-light photocatalyst of the present invention, described visible-light photocatalyst comprises lower transition material and semi-conducting material, the mass ratio of described lower transition material and semi-conducting material is 0.5% ~ 5%.
Described semi-conducting material is ZnO, TiO 2, SnO 2, ZrO 2, Co 3o 4, Fe 3o 4, La 2o 3, Ni (OH) 2, In 2tiO 5, BiOCl, BiOF, BiPO 4, CdMoO 4, CdWO 4, La 2sn 2o 7, La 2ti 2o 7, LaCoO 3, PbMoO 4, PbSb 2o 6, PbWO 4, Sr 2ta 2o 7, SrTiO 3, SrWO 4, ZnMoO 4, ZnSb 2o 6, ZnWO 4, WO 3, Cu 2o, In 2o 3, ZnS, CdS, CdSe, Bi 2o 3, BiOI, BiVO 4, BiWO 4, Bi 2moO 6, InVO 4, InNbO 4, Ag 3pO 4, AgCl, AgBr, AgI, MoO 3, MoS 2in one or more.
Doping vario-property material in described semi-conducting material, described material modified be one or more in Au, Ag, Graphene, CNT, the described material modified mass fraction adulterating in semi-conducting material is 0.5-2%.
Described lower transition material comprises one or more in garnet structure fluorescent material, non-garnet structure oxide fluorescent powder, sulphide fluorescent material, nitride and oxygen nitrogen fluorescent material.
Described garnet structure fluorescent material is Y 3al 5o 12: Ce 3+, Tb 3al 5o 12: Ce 3+, Lu 3al 5o 12: Ce 3+, Lu 2caMg 2(Si, Ge) 3o 12: Ce 3+, Ca 3sc 2si 3o 12: Ce 3+in one or more; Described non-garnet structure oxide fluorescent powder is Sr 2siO 4: Eu 2+, LiSrPO 4: Eu 2+, Sr 3siO 5: Eu 2+, Sr 3siO 5: Ce 3+, Li +, Li 2srSiO 4: Eu 2+, LaSr 2alO 5: Ce 3+, Ca 2bO 3cl:Eu 2+, Sr 3(Al 2o 5) C l2: Eu 2+in one or more; Described sulphide fluorescent material is CaS:Eu 2+, SrS:Eu 2+ce 3+, Ca 2siS 4: Eu 2+, Y 2o 2s:Eu 2+, (Ca, Sr) S:Eu 2+in one or more; Described nitride and oxygen nitrogen fluorescent material are MSi 2o 2n 2: Eu 2+, Ba 3si 6o 12n 2: Eu 2+, SrSi 5alO 2n 7: Eu 2+, SrSiAl 2o 3n 2: Eu 2+, CaAlSiN 3: Eu 2+, M 2si 5n 8: Eu 2+, MSiN 2: Eu 2+in one or more, M=Ca wherein, Sr, Ba.
A preparation method for visible-light photocatalyst, is characterized in that, described preparation method comprises the following steps:
(1), according to the proportioning of claim 1, weigh lower transition material and/or material modified; (2) load weighted material is joined in the salting liquid of 0.05-0.2 mol/l of 10-20 ml, solution is put in the microwave tube of 35 ml, stir 0.5-1 hour at 25-35 ℃, make solution even; (3) drip Na (OH) 2solution, makes the pH value of solution between 7-9, stirs 0.5-1 hour at room temperature 25-35 ℃; (4) solution being stirred is put in microwave reaction synthesizer, under temperature 110-160 ℃ and power 80-150 W condition, reacted and obtain composite photo-catalyst after 10-30 minute.
Embodiment 1
Adopt Y 3al 5o 12: Ce 3+composite visible light catalyst with ZnO.
1) preparation of photochemical catalyst
The mass ratio of weighing and semi-conducting material is 0.5%, 1%, 3% and 5% lower transition material Y respectively 3al 5o 12: Ce 3+, by load weighted Y 3al 5o 12: Ce 3join respectively the ZnSO of 0.1 mol/l of 20 ml 4in solution, solution is put in the microwave tube of 35 ml, under room temperature, stirred half an hour, make solution even.Then drip Na (OH) 2solution, makes the pH=9 of solution, stirs 1 hour under room temperature, then puts in microwave reaction synthesizer, in temperature 150 ounder C and power 100 W conditions, react and after 10 minutes, obtain four kinds of ZnO-Y 3al 5o 12: Ce 3+composite photo-catalyst.By Y 3al 5o 12: Ce 3+with the mass ratio of ZnO be: 0.5%, 1%, 3% and 5% composite photo-catalyst difference called after: ZY-0.5, ZY-1, ZY-3 and ZY-5.
2) photocatalysis experiment
Respectively by the photochemical catalyst preparing (2 g l -1) put into the methylene blue solution that concentration is 10 ppm (100 ml), under magnetic agitation condition, dark reaction, after 30 minutes, is opened gold-halogen lamp light source (390-800 nanometer), carries out light-catalyzed reaction.Get at set intervals a certain amount of methylene blue solution, with the absorption spectrum of ultraviolet-visible spectrophotometer test solution, by the variation of absorption peak strength, can calculate the degradation rate of methylene blue solution.Experimental result is shown in Fig. 1.
As Fig. 1, abscissa represents irradiation time, and ordinate represents the normalized concentration of methylene blue solution, has shown the ZnO-Y of different quality ratio in figure 3al 5o 12: Ce 3+photochemical catalyst is removed the different-effect of pollutant, works as Y 3al 5o 12: Ce 3+while being 3% with ZnO mass ratio, (composite photo-catalyst is ZY-3), the highest to the degradation rate of methylene blue, is 93%.
Embodiment 2
Adopt Y 2o 2s:Eu 2+composite visible light catalyst with ZnO.
1) preparation of photochemical catalyst
The mass ratio of weighing and semi-conducting material is 0.25%, 0.5% and 1% lower transition material Y respectively 2o 2s:Eu 2+, by load weighted Y 2o 2s:Eu 2+join respectively the ZnSO of 0.1 mol/l of 20 ml 4in solution, solution is put in the microwave tube of 35 ml, under room temperature, stirred half an hour, make solution even.Then drip Na (OH) 2solution, makes the pH=9 of solution, stirs 1 hour under room temperature, then puts in microwave reaction synthesizer, in temperature 150 ounder C and power 100 W conditions, react after 10 minutes and obtain ZnO-Y 2o 2s:Eu 2+composite photo-catalyst.By Y 2o 2s:Eu 2+with the mass ratio of ZnO be: 0.25%, 0.5% and 1% composite photo-catalyst difference called after: ZY-0.25-0, ZY-0.5-0 and ZY-1-0.
2) photocatalysis experiment
By the photochemical catalyst preparing (2 g l -1) put into the methylene blue solution that concentration is 10 ppm (100 ml), under magnetic agitation condition, dark reaction, after 30 minutes, is opened gold-halogen lamp light source (390-800 nanometer), carries out light-catalyzed reaction.Get at set intervals a certain amount of methylene blue solution, with the absorption spectrum of ultraviolet-visible spectrophotometer test solution, by the variation of absorption peak strength, can calculate the degradation rate of methylene blue solution.Experimental result is shown in Fig. 2.
As Fig. 2, abscissa represents irradiation time, and ordinate represents the normalized concentration of methylene blue solution, has shown the ZnO-Y of different quality ratio in figure 2o 2s:Eu 2+photochemical catalyst is removed the different-effect of pollutant, works as Y 2o 2s:Eu 2+while being 0.5% with ZnO mass ratio, (composite photo-catalyst is ZY-0.5-0), the highest to the degradation rate of methylene blue, is 96%.
Embodiment 3
Adopt SrSi 2o 2n 2: Eu 2+with ZnWO 4the composite visible light catalyst of-Au.
1) preparation of photochemical catalyst
First weigh the material modified HAuCl that four parts of mass ratioes with semi-conducting material are 0.5% 4, then to weigh respectively mass ratio with semi-conducting material be 0%, 0.5%, 1% and 2% lower transition material SrSi 2o 2n 2: Eu 2+, then by load weighted SrSi 2o 2n 2: Eu 2+with HAuCl 4join respectively the Na of 0.05 mol/l of 10 ml 2wO 4in solution, solution is put in the microwave tube of 35 ml, under room temperature, stirred half an hour, make solution even.Then by the ZnSO of 0.05 mol/l of 10 ml 4solution drips in above-mentioned solution, at room temperature stirs half an hour, drips Na (OH) 2solution, makes the pH=7 of solution, stirs 1 hour under room temperature, then puts in microwave reaction synthesizer, in temperature 150 ounder C and power 100 W conditions, react after 10 minutes and obtain ZnWO 4-Au-SrSi 2o 2n 2: Eu 2+composite photo-catalyst.By SrSi 2o 2n 2: Eu 2+with ZnWO 4mass ratio be: 0%, respectively called after: ZAS-0, ZAS-0.5, ZAS-1 and ZAS-2 of 0.5%, 1% and 2% composite photo-catalyst.
2) photocatalysis experiment
Respectively by the photochemical catalyst preparing (2 g l -1) put into the rhodamine B solution that concentration is 10 ppm (100 ml), under magnetic agitation condition, dark reaction, after 30 minutes, is opened gold-halogen lamp light source (390-800 nanometer), carries out light-catalyzed reaction.Get at set intervals a certain amount of rhodamine B solution, with the absorption spectrum of ultraviolet-visible spectrophotometer test solution, by the variation of absorption peak strength, can calculate the degradation rate of rhodamine B solution.Experimental result is shown in Fig. 3.
As Fig. 3, abscissa represents irradiation time, and ordinate represents the normalized concentration of rhodamine B solution, has shown the ZnWO of different quality ratio in figure 4-Au-SrSi 2o 2n 2: Eu 2+photochemical catalyst is removed the different-effect of pollutant, works as SrSi 2o 2n 2: Eu 2+account for ZnWO 4when mass ratio is 1%, (composite photo-catalyst is ZAS-1), the highest to the degradation rate of rhodamine B, is 94%.
Embodiment 4
Adopt LiSrPO 4: Eu 2+with Bi 2moO 6the composite visible light catalyst of-graphene.
1) preparation of photochemical catalyst
First weigh the material modified graphite oxide that four parts of mass ratioes with semi-conducting material are 1%, then to weigh respectively mass ratio with semi-conducting material be 0%, 0.25%, 0.5% and 1% lower transition material LiSrPO 4: Eu 2+, then by load weighted LiSrPO 4: Eu 2+join respectively the Na of 0.025 mol/l of 10 ml with graphite oxide 2moO 4in solution, solution is put in the microwave tube of 35 ml, under room temperature, stirred half an hour, make solution even.Then by the Bi (NO of 0.05 mol/l of 10 ml 3) 3solution drips in above-mentioned solution, at room temperature stirs half an hour, drips Na (OH) 2solution, makes the pH=7 of solution, stirs 1 hour under room temperature, then puts into microwave reaction Cheng Yili, in temperature 150 ounder C and power 100 W conditions, react after 10 minutes and obtain Bi 2moO 6-graphene-LiSrPO 4: Eu 2+composite photo-catalyst.By LiSrPO 4: Eu 2+with Bi 2moO 6mass ratio be: 0%, respectively called after: BRL-0, BRL-0.25, BRL-0.5 and BRL-1 of 0.25%, 0.5% and 1% composite photo-catalyst.
2) photocatalysis experiment
By the photochemical catalyst preparing (2 g l -1) put into the Acid Orange II solution that concentration is 10 ppm (100 ml), under magnetic agitation condition, dark reaction, after 30 minutes, is opened gold-halogen lamp light source (390-800 nanometer), carries out light-catalyzed reaction.Get at set intervals a certain amount of Acid Orange II solution, with the absorption spectrum of ultraviolet-visible spectrophotometer test solution, by the variation of absorption peak strength, can calculate the degradation rate of Acid Orange II solution.Experimental result is shown in Fig. 4.
As Fig. 4, abscissa represents irradiation time, and ordinate represents the normalized concentration of Acid Orange II solution, has shown the Bi of different quality ratio in figure 2moO 6-graphene-LiSrPO 4: Eu 2+photochemical catalyst is removed the different-effect of pollutant, works as LiSrPO 4: Eu 2+account for Bi 2moO 6when mass ratio is 0.5%, (composite photo-catalyst is BRL-0.5), the highest to the degradation rate of Acid Orange II, is 93%.
Embodiment 5
Adopt Sr 2si 5n 8: Eu 2+with SnO 2composite visible light catalyst.
1) preparation of photochemical catalyst
The mass ratio of weighing and semi-conducting material is 0.5%, 1% and 2% lower transition material Sr respectively 2si 5n 8: Eu 2+, by load weighted Sr 2si 5n 8: Eu 2+join respectively the SnCl of 0.1 mol/l of 20 ml 4in solution, solution is put in the microwave tube of 35 ml, under room temperature, stirred half an hour, make solution even.Then drip Na (OH) 2solution, makes the pH=7 of solution, stirs 1 hour under room temperature, then puts in microwave reaction synthesizer, in temperature 150 ounder C and power 100 W conditions, react after 10 minutes and obtain SnO 2-Sr 2si 5n 8: Eu 2+composite photo-catalyst.By Sr 2si 5n 8: Eu 2+with SnO 2mass ratio be: 0.5%, respectively called after: SS-0.5, SS-1 and SS-2 of 1% and 2% composite photo-catalyst.
2) photocatalysis experiment
By the photochemical catalyst preparing (2 g l -1) put into the phenol solution that concentration is 10 ppm (100 ml), under magnetic agitation condition, dark reaction, after 30 minutes, is opened gold-halogen lamp light source (390-800 nm), carries out light-catalyzed reaction.Get at set intervals a certain amount of phenol solution, with the absorption spectrum of ultraviolet-visible spectrophotometer test solution, by the variation of absorption peak strength, can calculate the degradation rate of phenol solution.Experimental result is shown in Fig. 5.
As Fig. 5, abscissa represents irradiation time, and ordinate represents the normalized concentration of phenol solution, has shown the SnO of different quality ratio in figure 2-Sr 2si 5n 8: Eu 2+photochemical catalyst is removed the different-effect of pollutant, works as Sr 2si 5n 8: Eu 2+account for SnO 2when mass ratio is 1% (composite photo-catalyst is SS-1), Pyrogentisinic Acid's degradation rate is the highest, is 90%.
Embodiment 6
Adopt Sr 2siO 4: Eu 2+with Bi 2o 3composite visible light catalyst.
1) preparation of photochemical catalyst
The mass ratio of weighing and semi-conducting material is 0.5%, 1% and 1.5% lower transition material Sr respectively 2siO 4: Eu 2+, by load weighted Sr 2siO 4: Eu 2+join respectively the Bi (NO of 0.05 mol/l of 20 ml 3) 3in solution, solution is put in the microwave tube of 35 ml, under room temperature, stirred half an hour, make solution even.Then drip Na (OH) 2solution, makes the pH=7 of solution, stirs 1 hour under room temperature, then puts in microwave reaction synthesizer, in temperature 150 ounder C and power 100 W conditions, react after 10 minutes and obtain Bi 2o 3-Sr 2siO 4: Eu 2+composite photo-catalyst.By Sr 2siO 4: Eu 2+with Bi 2o 3mass ratio be: 0.5%, respectively called after: BS-0.5, BS-1 and BS-1.5 of 1% and 1.5% composite photo-catalyst.
2) photocatalysis experiment
By the photochemical catalyst preparing (2 g l -1) to put into concentration be 2,4 of 10 ppm, in 5-trichlorophenol, 2,4,6,-T solution (100 ml), under magnetic agitation condition, dark reaction, after 30 minutes, is opened gold-halogen lamp light source (390-800 nanometer), carries out light-catalyzed reaction.Get at set intervals a certain amount ofly 2,4,5-trichlorophenol, 2,4,6,-T solution, with the absorption spectrum of ultraviolet-visible spectrophotometer test solution, can calculate the degradation rate of 2,4,5-trichlorophenol, 2,4,6,-T solution by the variation of absorption peak strength.Experimental result is shown in Fig. 6.
As Fig. 6, abscissa represents irradiation time, and ordinate represents the normalized concentration of 2,4,5-trichlorophenol, 2,4,6,-T solution, has shown the Bi of different quality ratio in figure 2o 3-Sr 2siO 4: Eu 2+photochemical catalyst is removed the different-effect of pollutant, works as Sr 2siO 4: Eu 2+account for Bi 2o 3when mass ratio is 1%, (composite photo-catalyst is BS-1), the highest to the degradation rate of 2,4,5-trichlorophenol, 2,4,6,-T, is 91%.
Embodiment can also adopt sol-gal process to prepare described visible-light photocatalyst, and concrete grammar is as follows:
Embodiment 7
Adopt Sr 3siO 5: Eu 2+with TiO 2the composite visible light catalyst of-CNTs.
1) preparation of photochemical catalyst
Getting 4 ml butyl titanates dropwise drips in 10 ml ethanol solutions and forms A solution.Weigh the material modified CNTs that four parts of mass ratioes with semi-conducting material are 1%, then to weigh respectively mass ratio with semi-conducting material be 0%, 1%, 3% and 5% lower transition material Sr 3siO 5: Eu 2+, by load weighted CNTs and Sr 3siO 5: Eu 2+be dispersed in respectively in the mixed solution of 2 ml distilled water, 5 ml glacial acetic acid and 7 ml absolute ethyl alcohols and form B solution.Then B solution dropwise drips in A solution, stirs 4 hours under normal temperature, obtains TiO 2-CNTs-Sr 3siO 5: Eu 2+colloidal sol.This colloidal sol ageing, after 12 hours, is put in drying box, 100 odry 12 hours of C after grinding, heat-treats in air atmosphere, and its heat treatment temperature is 500 oc, time are 1 hour, obtain TiO 2-CNTs-Sr 3siO 5: Eu 2+composite photo-catalyst.By Sr 3siO 5: Eu 2+with TiO 2mass ratio be: 0%, respectively called after: TCS-0, TCS-1, TCS-3 and TCS-5 of 1%, 3% and 5% composite photo-catalyst.
2) photocatalysis experiment
By the photochemical catalyst preparing (2 g l -1) put into the polycyclic aromatic hydrocarbon solution that concentration is 10 ppm (100 ml), under magnetic agitation condition, dark reaction, after 30 minutes, is opened gold-halogen lamp light source (390-800 nanometer), carries out light-catalyzed reaction.Get at set intervals a certain amount of polycyclic aromatic hydrocarbon solution, with the absorption spectrum of ultraviolet-visible spectrophotometer test solution, by the variation of absorption peak strength, can calculate the degradation rate of polycyclic aromatic hydrocarbon solution.Experimental result is shown in Fig. 7.
As Fig. 7, abscissa represents irradiation time, and ordinate represents the normalized concentration of polycyclic aromatic hydrocarbon solution, has shown the TiO of different quality ratio in figure 2-CNTs-Sr 3siO 5: Eu 2+photochemical catalyst is removed the different-effect of pollutant, works as Sr 3siO 5: Eu 2+account for TiO 2when mass ratio is 3%, (composite photo-catalyst is TCS-3), the highest to the degradation rate of polycyclic aromatic hydrocarbon, is 91%.
In concrete enforcement, also available employing water-bath chemical reaction method, spray pyrolysis, method of electrostatic spinning or ultrasonic reaction synthetic method are prepared described visible-light photocatalyst, and it is that implementation result is optimum that institute exemplifies microwave reaction synthesis method in embodiment.
Be more than the description to the embodiment of the present invention, by the above-mentioned explanation to the disclosed embodiments, make professional and technical personnel in the field can realize or use the present invention.To the multiple modification of these embodiment, will be apparent for those skilled in the art, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.

Claims (8)

1. a visible-light photocatalyst, is characterized in that, described visible-light photocatalyst comprises lower transition material and semi-conducting material, and the mass ratio of described lower transition material and semi-conducting material is 0.5% ~ 5%.
2. visible-light photocatalyst according to claim 1, is characterized in that, described visible-light photocatalyst comprises lower transition material and semi-conducting material, and the mass ratio of described lower transition material and semi-conducting material is 1% ~ 4%.
3. visible-light photocatalyst according to claim 1, is characterized in that, described visible-light photocatalyst comprises lower transition material and semi-conducting material, and the mass ratio of described lower transition material and semi-conducting material is 1.5% ~ 3%.
4. according to the arbitrary described visible-light photocatalyst of claim 1 to 3, it is characterized in that, described semi-conducting material is ZnO, TiO 2, SnO 2, ZrO 2, Co 3o 4, Fe 3o 4, La 2o 3, Ni (OH) 2, In 2tiO 5, BiOCl, BiOF, BiPO 4, CdMoO 4, CdWO 4, La 2sn 2o 7, La 2ti 2o 7, LaCoO 3, PbMoO 4, PbSb 2o 6, PbWO 4, Sr 2ta 2o 7, SrTiO 3, SrWO 4, ZnMoO 4, ZnSb 2o 6, ZnWO 4, WO 3, Cu 2o, In 2o 3, ZnS, CdS, CdSe, Bi 2o 3, BiOI, BiVO 4, BiWO 4, Bi 2moO 6, InVO 4, InNbO 4, Ag 3pO 4, AgCl, AgBr, AgI, MoO 3, MoS 2in one or more.
5. visible-light photocatalyst according to claim 4, it is characterized in that, doping vario-property material in described semi-conducting material, described material modified be one or more in Au, Ag, Graphene, CNT, the described material modified mass fraction adulterating in semi-conducting material is 0.5-2%.
6. according to the arbitrary described visible-light photocatalyst of claim 1 to 3, it is characterized in that, described lower transition material comprises one or more in garnet structure fluorescent material, non-garnet structure oxide fluorescent powder, sulphide fluorescent material, nitride and oxygen nitrogen fluorescent material.
7. visible-light photocatalyst according to claim 6, is characterized in that, described garnet structure fluorescent material is Y 3al 5o 12: Ce 3+, Tb 3al 5o 12: Ce 3+, Lu 3al 5o 12: Ce 3+, Lu 2caMg 2(Si, Ge) 3o 12: Ce 3+, Ca 3sc 2si 3o 12: Ce 3+in one or more; Described non-garnet structure oxide fluorescent powder is Sr 2siO 4: Eu 2+, LiSrPO 4: Eu 2+, Sr 3siO 5: Eu 2+, Sr 3siO 5: Ce 3+, Li +, Li 2srSiO 4: Eu 2+, LaSr 2alO 5: Ce 3+, Ca 2bO 3cl:Eu 2+, Sr 3(Al 2o 5) C l2: Eu 2+in one or more; Described sulphide fluorescent material is CaS:Eu 2+, SrS:Eu 2+ce 3+, Ca 2siS 4: Eu 2+, Y 2o 2s:Eu 2+, (Ca, Sr) S:Eu 2+in one or more; Described nitride and oxygen nitrogen fluorescent material are MSi 2o 2n 2: Eu 2+, Ba 3si 6o 12n 2: Eu 2+, SrSi 5alO 2n 7: Eu 2+, SrSiAl 2o 3n 2: Eu 2+, CaAlSiN 3: Eu 2+, M 2si 5n 8: Eu 2+, MSiN 2: Eu 2+in one or more, M=Ca wherein, Sr, Ba.
8. a preparation method for visible-light photocatalyst, is characterized in that, described preparation method comprises the following steps:
(1), according to the proportioning of claim 1, weigh lower transition material and/or material modified; (2) load weighted material is joined in the salting liquid of 0.05-0.2 mol/l of 10-20 ml, solution is put in the microwave tube of 35 ml, stir 0.5-1 hour at 25-35 ℃, make solution even; ; (3) drip Na (OH) 2solution, makes the pH value of solution between 7-9, stirs 0.5-1 hour at room temperature 25-35 ℃; (4) solution being stirred is put in microwave reaction synthesizer, under temperature 110-160 ℃ and power 80-150 W condition, reacted and obtain composite photo-catalyst after 10-30 minute.
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