CN104014291A - Fluorescent rotary plate reactor utilizing Ag/BiOBr visible light catalytic film - Google Patents
Fluorescent rotary plate reactor utilizing Ag/BiOBr visible light catalytic film Download PDFInfo
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- CN104014291A CN104014291A CN201410268525.3A CN201410268525A CN104014291A CN 104014291 A CN104014291 A CN 104014291A CN 201410268525 A CN201410268525 A CN 201410268525A CN 104014291 A CN104014291 A CN 104014291A
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- biobr
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Abstract
The invention discloses a technical scheme for applying a Ag/BiOBr visible light catalytic film to a fluorescent rotary plate reactor. The precious metal Ag is deposited on the surface of a catalyst film, a fluorescent rotary plate reactor which is matched with a light absorption range of the Ag/BiOBr catalyst is designed to be used for processing organic pollutants in the industrial waste water. The light absorption of the BiOBr light catalyst in the range of 440nm to 500nm is enhanced through the Plasman effect of silver, the light catalytic reaction is continuously processed after no light is provided through the fluorescent rotary plate, the all-weather light catalysis is realized, the utilization rate of the sunlight by the reaction system is increased, and the energy consumption problem can be solved.
Description
Technical field
The invention belongs to the technical field of conductor photocatalysis film preparation and photo catalysis reactor design, be specifically related to solvent-thermal method and prepare photocatalysis film, photoreduction met hod depositing noble metal and design rotating disk fluorescence reaction device.
Background technology
Semiconductor nano material can provide the novel energies such as hydrogen by organic compound mineralising with environment purification and decomposition water by photocatalysis, is therefore subject to extensive concern.BiOBr visible light catalyst is because its superior photocatalytic activity and chemical stability become study hotspot in recent years, made up that titanium oxide can only absorb ultraviolet light and defect to sunshine utilization rate deficiency.But in actual applications, powder photocatalyst is difficult to separate recovery, be unfavorable for recycling, and BiOBr molecular weight is greater than titanium oxide, carry out light-catalyzed reaction in heterogeneous system time, more easily fall to reactor bottom, thereby reduce the utilization rate of catalyst.By can effectively addressing this problem at substrate surface control growth BiOBr film.
In addition, photo catalysis reactor also has important impact for light degradation process, and photo catalysis reactor rational in infrastructure can effectively improve the utilization rate of photochemical catalyst to light.But current research work mainly concentrates on by doping, depositing noble metal, the method such as compound the extinction scope of titanium oxide is expanded to visible region and developed non-oxide titanium visible light catalyst, as Bi series visible-light catalyst etc.And the photo catalysis reactor that exploitation can effectively improve light utilization efficiency is also very important research direction, especially round-the-clock reactor.
In the present invention, build fluorescence disk reactor, make light-emitting phosphor wavelength and Ag/BiOBr visible light catalytic film absorption Wavelength matched.Excitated fluorescent powder in utilizing illumination degrading pollutant, when fluorescent material after unglazed photograph can continue luminously, makes light-catalyzed reaction continue to carry out.Meanwhile, prepared Ag/BiOBr film is combined with substrate firmly, and active high, excellent in stability, can reuse, and has solved powder catalyst and has been difficult to the problem reclaiming.
Summary of the invention
The object of the invention is to prepare photocatalysis film by photoreduction met hod at BiOBr film surface depositing silver particle, thereby the visible ray that utilizes its Prusman effect can absorb specific band significantly strengthens the absorption of Ag/BiOBr at visible region, improve photocatalytic activity, and build fluorescence disk reactor with this, employing can send the fluorescent material of 480nm visible ray and the Prusman effect of Ag enhancing wave-length coverage (440-500nm) matches, realize in the situation that gauge without light source irradiates, continue to utilize light-emitting phosphor to continue to carry out light-catalyzed reaction, greatly improve the utilization rate of catalyst to sunshine.
Details are as follows for technical scheme of the present invention:
Apply a fluorescence disk reactor for Ag/BiOBr visible light catalytic film, described rotating disk material is quartz glass, it is characterized in that, described rotating disk outer surface posts Ag/BiOBr visible light catalytic film, and fluorescent material is housed in rotating disk.
Described Ag/BiOBr visible light catalytic film is that Ag nano particle is deposited on sheet BiOBr visible light catalytic film, sheet BiOBr visible light catalytic film and substrate of glass strong bonded, the cubic BiOBr crystalline phase (JCPDS93-0393) that wherein BiOBr crystal formation is pure phase.
The preparation of described Ag/BiOBr visible light catalytic film comprises the following steps:
(1) glass surface treatment:
Common soda-lime glass is successively placed on to 80 DEG C of oven dryings with hydrochloric acid solution and ultrasonic the cleaning of absolute ethyl alcohol, afterwards the sheet glass of oven dry is stood in water heating kettle, add deionized water, put into baking oven and keep 6h at 180 DEG C, after taking out, clean three times by absolute ethyl alcohol and deionized water, place under room temperature dry;
(2) preparation of BiOBr film:
Take Bi (NO
3)
35H
2o adds in the mixed solution of ethylene glycol and isopropyl alcohol, and the volume ratio of ethylene glycol and isopropyl alcohol is 5:35, and after stirring is dissolved it completely, adding Br/Bi mol ratio is 1-cetyl trimethyl imidazoles bromine the salt ([C of 2:1
16min] Br), continue to be stirred to solution clarification, after being stood in water heating kettle, processed good sheet glass adds gained settled solution, at 160 DEG C, react 12h, after reaction, take out sheet glass ethanol washing three times and at room temperature dry after roasting 4 hours at 450 DEG C, obtaining load has the sheet glass of sheet BiOBr visible light catalytic film;
(3) deposition Ag nano particle: have the sheet glass of sheet BiOBr visible light catalytic film to lie against AgNO load
3methanol solution in, in solution, in Ag content and film, the mol ratio of Bi content is 1.5-6.0%, with UV illumination reduction, the photo-reduction time is respectively 10-25min, then cleans up film surface with ultra-pure water, under room temperature, dries sheet glass.
Above-mentioned visible light catalytic film is affixed on the fluorescence disk reactor outer surface that rotating disk material is quartz glass, can be for the photocatalytic degradation processing of organic pollution.Concrete grammar is:
In fluorescence disk reactor rotating disk, pack the fluorescent material that emission wavelength is 480nm into, rotating speed is made as 90 revs/min, disk reactor excites the fluorescent material of rotating disk inside under extraneous illumination in degradation of contaminant, when after unglazed photograph, fluorescent material continuation is luminous makes light-catalyzed reaction continue to carry out.
The present invention has the following advantages compared with prior art tool: in fluorescence disk reactor, adopt and can send the fluorescent material of 480nm visible ray and the Prusman effect of Ag enhancing wave-length coverage (440-500nm) and match, realize in the situation that irradiating without additional light source, utilize light-emitting phosphor to continue to carry out light-catalyzed reaction, greatly improved the utilization rate to sunshine.The reagent using is that common agents, preparation method are easy, easily control.The BiOBr film that has deposited Ag improves being absorbed with significantly of visible ray, has further improved photocatalytic activity.
Brief description of the drawings
Fig. 1 is the XRD figure of embodiment 1-2.
Fig. 2 is the XPS collection of illustrative plates of embodiment 1 and 3-5.
Fig. 3 is the UV-vis DRS collection of illustrative plates of embodiment 1-2.
Fig. 4 is degrade in the disk reactor without the fluorescent material photocatalytic activity of RhB of embodiment 1-5.
Fig. 5 is degrade in the disk reactor without the fluorescent material photocatalytic activity of RhB of embodiment 1 and 6-8.
Fig. 6 is degrade in the fluorescence disk reactor photocatalytic activity of RhB of embodiment 1.
Detailed description of the invention
Below in conjunction with specific embodiment, further set forth the present invention.
The present invention carries out structural characterization by following means to Ag/BiOBr film: X-ray diffraction (XRD) collection of illustrative plates that adopts Rigaku D/Max-RB type X-ray diffractometer to measure carries out the structural analysis of sample, adopt the absorbability of the light of UV-2450 type spectrophotometer analytic sample, with the valence state of silver in Perkin Elmer PHI5000ESCT System x-ray photoelectron spectroscopy analytic sample.
Embodiment 1
By ultrasonic 2h in the concentrated hydrochloric acid of 10mol/L for slide, rinse well with clear water, be positioned over deionized water for ultrasonic 2h, take out slide and be placed in 80 DEG C of oven for drying.Take out slide and stand in 50L water heating kettle, add 35mL deionized water, put into 180 DEG C of baking ovens and leave standstill after 6h and rinse well with ultra-pure water, be put in air, dry for subsequent use.Take 0.12g Bi (NO
3)
35H
2o adds in the mixed solution of 40ml ethylene glycol and isopropyl alcohol.The volume ratio of ethylene glycol and isopropyl alcohol is 5:35.Stirring adds Br/Bi mol ratio after it is dissolved be completely the 1-cetyl trimethyl imidazoles bromine salt of 2:1
([C
16min] Br), continue to be stirred to solution clarification.After the sheet glass of handling well is stood in 50ml water heating kettle, add settled solution, at 160 DEG C, react 12h.Take out sheet glass ethanol washing three times, after being dried under room temperature, 450 DEG C of roastings 4 hours, obtain the sheet BiOBr photocatalysis film of high-crystallinity.The slide of three load BiOBr films is lain against to 60ml and dissolve AgNO
3methanol solution in, Ag/Bi ratio is 3.0mol%, and the uviol lamp photo-reduction 15min that is 365nm with emission wavelength.Clean sample surfaces with ultra-pure water, under room temperature, dry.
The process of fluorescence disk reactor degraded simulating pollution thing rhodamine B (RhB) is as follows: the sheet glass that is coated with catalyst film that sticks 4 22 × 20mm at fluorescence disk reactor outer surface.Using 55mL15mg/L RhB solution as reaction solution, and the rotating disk area that maintenance is immersed in solution is 43%.As light source, and be less than the light of 420nm with optical filter elimination with 300W xenon lamp.Rotary speed is 90rpm, and reaction temperature is 30 DEG C.Before carrying out photocatalytic activity test, sample dark absorption 40min in reactant liquor, to reach adsorption equilibrium, then turns on light and carries out degradation reaction, samples every 25min.After reaction 1h, close xenon lamp, fluorescent material will continue luminous continuation degraded RhB because extinction reaches capacity.Adopt UV spectrophotometer to measure its absorbance at the characteristic absorption wavelength 553nm place of RhB, calculate the degradation rate of differential responses time.
In Fig. 1, the XRD collection of illustrative plates of the present embodiment shows that obtained film is the cubic BiOBr crystalline phase of high-crystallinity, and free from admixture generates.In Fig. 2, XPS collection of illustrative plates shows, the Ag of the present embodiment is present in BiOBr surface with the form of simple substance.In Fig. 3, UV-vis DRS collection of illustrative plates shows that the Prusman effect of Ag in the present embodiment has strengthened the light absorpting ability of 440-500nm visible region.In Fig. 4-5, the present embodiment simulating pollution thing rhodamine B of degrading in the disk reactor without fluorescent material has best photocatalytic activity, and the degradation rate of rhodamine B is approached to 80%.In Fig. 6, the present embodiment was degraded RhB after mono-hour in fluorescence disk reactor, closed radiation source and only utilized the luminous continuation of fluorescent material to degrade (emission wavelength is 480nm), and degradation rate increases by 16%.And during without fluorescent material, cannot there is degradation reaction.
Embodiment 2
Identical with the method for preparing BiOBr film catalyst in embodiment 1, do not deposit Ag particle.In Fig. 1, the XRD collection of illustrative plates of the present embodiment shows that obtained film is the cubic BiOBr crystalline phase of high-crystallinity, and free from admixture generates.In Fig. 3, the UV-vis DRS collection of illustrative plates of the present embodiment shows that BiOBr film catalyst has certain absorbability to visible ray.In Fig. 4, under the present embodiment visible ray, RhB is had to degradation.
Embodiment 3
The ratio of Ag/Bi is tuned as to 1.5mol%, and other guide is with identical described in embodiment 1.In Fig. 2, XPS collection of illustrative plates shows, the Ag of the present embodiment is present on BiOBr with the form of simple substance.In Fig. 4, under the present embodiment visible ray, RhB is had to degradation.
Embodiment 4
The ratio of Ag/Bi is tuned as to 4.5mol%, and other guide is with identical described in embodiment 1.In Fig. 2, XPS collection of illustrative plates shows, the Ag of the present embodiment is present on BiOBr with the form of simple substance.In Fig. 4, under the present embodiment visible ray, RhB is had to degradation.
Embodiment 5
The ratio of Ag/Bi is tuned as to 6.0mol%, and other guide is with identical described in embodiment 1.In Fig. 2, XPS collection of illustrative plates shows, the Ag of the present embodiment is present on BiOBr with the form of simple substance.In Fig. 4, under the present embodiment visible ray, RhB is had to degradation.
Embodiment 6
The photo-reduction time is tuned as to 10min, and other guide is with identical described in embodiment 1.In Fig. 5, under the present embodiment visible ray, RhB is had to degradation.
Embodiment 7
The photo-reduction time is tuned as to 20min, and other guide is with identical described in embodiment 1.In Fig. 5, under the present embodiment visible ray, RhB is had to degradation.
Embodiment 8
The photo-reduction time is tuned as to 25min, and other guide is with identical described in embodiment 1.In Fig. 5, under the present embodiment visible ray, RhB is had to degradation.
Claims (3)
1. apply a fluorescence disk reactor for Ag/BiOBr visible light catalytic film, described rotating disk material is quartz glass, it is characterized in that, described rotating disk outer surface posts Ag/BiOBr visible light catalytic film, and fluorescent material is housed in rotating disk.
2. the fluorescence disk reactor of application Ag/BiOBr visible light catalytic film according to claim 1, it is characterized in that, described Ag/BiOBr visible light catalytic film is that Ag nano particle is deposited on sheet BiOBr visible light catalytic film, sheet BiOBr visible light catalytic film and substrate of glass strong bonded, the cubic BiOBr crystalline phase (JCPDS93-0393) that wherein BiOBr crystal formation is pure phase.
3. the fluorescence disk reactor of application Ag/BiOBr visible light catalytic film according to claim 1, is characterized in that, the preparation of described Ag/BiOBr visible light catalytic film comprises the following steps:
(1) glass surface treatment:
Common soda-lime glass is successively placed on to 80 DEG C of oven dryings with hydrochloric acid solution and ultrasonic the cleaning of absolute ethyl alcohol, afterwards the sheet glass of oven dry is stood in water heating kettle, add deionized water, put into baking oven and keep 6h at 180 DEG C, after taking out, clean three times by absolute ethyl alcohol and deionized water, place under room temperature dry;
(2) preparation of BiOBr film:
Take Bi (NO
3)
35H
2o adds in the mixed solution of ethylene glycol and isopropyl alcohol, and the volume ratio of ethylene glycol and isopropyl alcohol is 5:35, and after stirring is dissolved it completely, adding Br/Bi mol ratio is 1-cetyl trimethyl imidazoles bromine the salt ([C of 2:1
16min] Br), continue to be stirred to solution clarification, after being stood in water heating kettle, processed good sheet glass adds gained settled solution, at 160 DEG C, react 12h, after reaction, take out sheet glass ethanol washing three times and at room temperature dry after roasting 4 hours at 450 DEG C, obtaining load has the sheet glass of sheet BiOBr visible light catalytic film;
(3) deposition Ag nano particle: have the sheet glass of sheet BiOBr visible light catalytic film to lie against AgNO load
3methanol solution in, in solution, in Ag content and film, the mol ratio of Bi content is 1.5-6.0%, with UV illumination reduction, the photo-reduction time is respectively 10-25min, then cleans up film surface with ultra-pure water, under room temperature, dries sheet glass.
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| CN104549269A (en) * | 2014-12-31 | 2015-04-29 | 上海师范大学 | Method for preparing Ag/Bi2WO6 photocatalyst with hollow shell structure by depositing Ag particles with ultrasonic-assisted photoreduction method |
| CN105036436A (en) * | 2015-06-25 | 2015-11-11 | 上海师范大学 | Ag/BiOBr photocatalysis-membrane distillation reaction system |
| CN108355682A (en) * | 2018-02-06 | 2018-08-03 | 常州大学 | A kind of preparation method and application for handling eutrophic raw water catalysis material |
| CN108499580A (en) * | 2017-02-23 | 2018-09-07 | 南开大学 | A method of poor iodine-type BiOI photocatalysis films are prepared by solvent-thermal method |
| CN108587602A (en) * | 2018-05-31 | 2018-09-28 | 陕西科技大学 | A method of it is modified by long after glow luminous material surface and improves luminescent properties |
| CN108722428A (en) * | 2018-06-04 | 2018-11-02 | 朱修齐 | A kind of composite material and its application for photocatalytic degradation organic matter |
| CN108816253A (en) * | 2018-05-31 | 2018-11-16 | 宁夏大学 | A kind of Au/Bi24O31Br10Composite photo-catalyst and preparation method thereof |
| CN109046400A (en) * | 2018-07-23 | 2018-12-21 | 汕头大学 | A kind of BiOI photochemical catalyst and its preparation and application that precious metals pt is modified |
| CN113546523A (en) * | 2021-07-23 | 2021-10-26 | 上海师范大学 | PVDF ultrafiltration membrane of composite Ag @ BiOBr photocatalytic material as well as preparation method and application of PVDF ultrafiltration membrane |
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| CN105036436A (en) * | 2015-06-25 | 2015-11-11 | 上海师范大学 | Ag/BiOBr photocatalysis-membrane distillation reaction system |
| CN108499580A (en) * | 2017-02-23 | 2018-09-07 | 南开大学 | A method of poor iodine-type BiOI photocatalysis films are prepared by solvent-thermal method |
| CN108355682A (en) * | 2018-02-06 | 2018-08-03 | 常州大学 | A kind of preparation method and application for handling eutrophic raw water catalysis material |
| CN108587602A (en) * | 2018-05-31 | 2018-09-28 | 陕西科技大学 | A method of it is modified by long after glow luminous material surface and improves luminescent properties |
| CN108816253A (en) * | 2018-05-31 | 2018-11-16 | 宁夏大学 | A kind of Au/Bi24O31Br10Composite photo-catalyst and preparation method thereof |
| CN108722428A (en) * | 2018-06-04 | 2018-11-02 | 朱修齐 | A kind of composite material and its application for photocatalytic degradation organic matter |
| CN108722428B (en) * | 2018-06-04 | 2021-03-16 | 朱修齐 | Composite material for photocatalytic degradation of organic matters and application thereof |
| CN109046400A (en) * | 2018-07-23 | 2018-12-21 | 汕头大学 | A kind of BiOI photochemical catalyst and its preparation and application that precious metals pt is modified |
| CN113546523A (en) * | 2021-07-23 | 2021-10-26 | 上海师范大学 | PVDF ultrafiltration membrane of composite Ag @ BiOBr photocatalytic material as well as preparation method and application of PVDF ultrafiltration membrane |
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