CN104014291B - A kind of fluorescence disk reactor applying Ag/BiOBr visible light catalytic film - Google Patents
A kind of fluorescence disk reactor applying Ag/BiOBr visible light catalytic film Download PDFInfo
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- CN104014291B CN104014291B CN201410268525.3A CN201410268525A CN104014291B CN 104014291 B CN104014291 B CN 104014291B CN 201410268525 A CN201410268525 A CN 201410268525A CN 104014291 B CN104014291 B CN 104014291B
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Abstract
The invention discloses and a kind of Ag/BiOBr visible light catalytic film is applied to the technical scheme in fluorescence disk reactor, by at catalyst film surface depositing noble metal Ag, devise the fluorescence disk reactor matched with Ag/BiOBr catalyst light absorption range for processing Industry Waste organic pollutants.The present invention enhances BiOBr photochemical catalyst light in the range of 440 500nm by the Prusman effect of silver and absorbs, and by fluorescence rotating disk, light-catalyzed reaction is proceeded after unglazed photograph, achieve all-weather light catalysis, improve the reaction system utilization rate to sunshine, solve problems of energy consumption.
Description
Technical field
The invention belongs to conductor photocatalysis film preparation and the technical field of photo catalysis reactor design,
Be specifically related to solvent-thermal method prepare photocatalysis film, photoreduction met hod depositing noble metal and design rotating disk glimmering
Photoreactor.
Background technology
Organic compound mineralising with environment purification and can be divided by semiconductor nano material by photocatalysis
Xie Shui provides the novel energies such as hydrogen, therefore suffers from extensive concern.BiOBr visible light catalyst is due to it
Superior photocatalytic activity and chemical stability become study hotspot in recent years, only compensate for titanium oxide
Can absorb ultraviolet light and to the not enough defect of sunshine utilization rate.But in actual applications, powder light
Catalyst is difficult to separate and recover, and is unfavorable for recycling, and BiOBr molecular weight is more than titanium oxide,
Heterogeneous system is carried out during light-catalyzed reaction, be easier to fall to reactor bottom, thus reduce catalysis
The utilization rate of agent.This problem can be effectively solved by controlling growth BiOBr film at substrate surface.
Additionally, photo catalysis reactor also has important impact, light rational in infrastructure for light degradation process
Catalytic reactor can be effectively improved the photochemical catalyst utilization rate to light.But current research work is main
Concentrate on and the light absorption range of titanium oxide expanded to can by doping, depositing noble metal, the method such as compound
Jian Guang district and develop non-oxide titanium visible light catalyst, such as Bi series visible-light catalyst etc..And develop
The photo catalysis reactor that can be effectively improved light utilization efficiency is also very important research direction, the most entirely
Weather reactor.
The present invention builds fluorescence disk reactor, makes light-emitting phosphor wavelength and Ag/BiOBr visible ray
Catalytic film absorbing wavelength is mated.Excitated fluorescent powder while utilizing illumination degrading pollutant, works as nothing
After illumination, fluorescent material can continue luminescence so that light-catalyzed reaction is persistently carried out.Meanwhile, prepared
Ag/BiOBr film is firmly combined with substrate, and activity is high, excellent in stability, repeatable utilization, solves
The problem that powder catalyst is difficult to reclaim.
Summary of the invention
It is an object of the invention to prepare light by photoreduction met hod in BiOBr film surface deposition silver particles
Catalytic film, utilizes its Prusman effect to can absorb the visible ray of specific band thus significantly strengthens
Ag/BiOBr, in the absorption of visible region, improves photocatalytic activity, and builds the reaction of fluorescence rotating disk with this
Device, uses the fluorescent material that can send 480nm visible ray to strengthen wavelength model with the Prusman effect of Ag
Enclose (440-500nm) to match, it is achieved in the case of gauge without light source irradiates, continue with fluorescent material
Luminescence persistently carries out light-catalyzed reaction, is greatly improved the catalyst utilization rate to sunshine.
Details are as follows for technical scheme:
A kind of fluorescence disk reactor applying Ag/BiOBr visible light catalytic film, described rotating disk material
For quartz glass, it is characterised in that described rotating disk outer surface posts Ag/BiOBr visible light catalytic film,
Rotating disk is built with fluorescent material.
Described Ag/BiOBr visible light catalytic film is that Ag nano particle is deposited on sheet BiOBr visible ray
On catalytic film, sheet BiOBr visible light catalytic film and substrate of glass strong bonded, wherein BiOBr
Crystal formation is the cubic BiOBr crystalline phase (JCPDS93-0393) of pure phase.
The preparation of described Ag/BiOBr visible light catalytic film comprises the following steps:
(1) glass surface treatment:
Ultrasonic to common soda lime glass priority hydrochloric acid solution and absolute ethyl alcohol cleaning is placed on 80 DEG C of baking ovens
Be dried, afterwards the sheet glass of drying is stood in water heating kettle, add deionized water, put into baking oven in
Keep 6h at 180 DEG C, clean three times by absolute ethyl alcohol and deionized water after taking-up, place under room temperature dry
Dry；
(2) preparation of BiOBr film:
Weigh Bi (NO3)3·5H2O adds in the mixed solution of ethylene glycol and isopropanol, ethylene glycol and isopropyl
The volume ratio of alcohol is 5:35, and stirring adds the 1-ten that Br/Bi mol ratio is 2:1 after making it be completely dissolved
Six alkyl trimethyl imidazoles bromide ([C16Min] Br), continue stirring and clarify to solution, by processed good
Sheet glass stand in water heating kettle after add gained settled solution, at 160 DEG C, react 12h, instead
After taking out sheet glass ethanol washing three times after should and being dried at room temperature for, at 450 DEG C, roasting 4 is little
Time, obtain being loaded with the sheet glass of sheet BiOBr visible light catalytic film；
(3) deposition Ag nano particle: the sheet glass of sheet BiOBr visible light catalytic film will be loaded with
Lie against AgNO3Methanol solution in, in solution, Ag content with the mol ratio of Bi content in film is
1.5-6.0%, reduces by UV illumination, and the photo-reduction time is respectively 10-25min, then with ultrapure
Water cleans up and dries sheet glass under film surface, room temperature.
Above-mentioned visible light catalytic film is affixed on outside the fluorescence disk reactor that rotating disk material is quartz glass
On surface, the photocatalytic degradation that may be used for organic pollution processes.Method particularly includes:
Loading emission wavelength in fluorescence disk reactor rotating disk is the fluorescent material of 480nm, and rotating speed is set to
90 revs/min, disk reactor excites within rotating disk under extraneous illumination while degradation of contaminant glimmering
Light powder, when, after unglazed photograph, fluorescent material continues luminescence and makes light-catalyzed reaction persistently carry out.
The present invention relatively prior art has the advantage that in fluorescence disk reactor to use and can send 480
The fluorescent material of nm visible ray strengthens wave-length coverage (440-500nm) phase with the Prusman effect of Ag
Coupling, it is achieved in the case of irradiating without additional light source, utilize light-emitting phosphor persistently to carry out photocatalysis
Reaction, substantially increases the utilization rate to sunshine.The reagent used is common agents, preparation
Method is easy, easily-controllable.The absorption of visible ray is greatly improved by the BiOBr film that deposited Ag, enters
One step improves photocatalytic activity.
Accompanying drawing explanation
Fig. 1 is the XRD 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 that embodiment 1-5 is degraded the photocatalytic activity of RhB in the disk reactor of unstressed configuration powder.
Fig. 5 is that embodiment 1 and 6-8 is degraded the photocatalysis of RhB in the disk reactor of unstressed configuration powder
Activity.
Fig. 6 is that embodiment 1 is degraded the photocatalytic activity of RhB in fluorescence disk reactor.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.
The present invention carries out structural characterization by the following means to Ag/BiOBr film: use Rigaku
X-ray diffraction (XRD) collection of illustrative plates that D/Max-RB type X-ray diffractometer is measured carries out the structure of sample
Analyze, use the absorbability of the light of UV-2450 type spectrophotometric analysis sample, use Perkin
Elmer PHI5000ESCT System x-ray photoelectron spectroscopy analyzes the valence state of silver in sample.
Embodiment 1
By 2h ultrasonic in the concentrated hydrochloric acid of slide 10mol/L, rinse well with clear water, placed
Ultrasonic 2h in deionized water, takes out slide and is placed in 80 DEG C of oven for drying.Taking-up slide is upright
In 50L water heating kettle, add 35mL deionized water, put into and use after 180 DEG C of baking ovens stand 6h
Ultrapure water is clean, be put in air dry standby.Weigh 0.12g Bi (NO3)3·5H2O adds 40ml
In the mixed solution of ethylene glycol and isopropanol.Ethylene glycol is 5:35 with the volume ratio of isopropanol.Stirring
The 1-cetyl trimethyl imidazoles bromide that Br/Bi mol ratio is 2:1 is added after making it be completely dissolved
([C16Min] Br), continue stirring and clarify to solution.The sheet glass handled well is stood on 50ml water
Add settled solution after in hot still, at 160 DEG C, react 12h.Take out sheet glass ethanol and wash three
Secondary, dried 450 DEG C of roastings 4 hours under room temperature, i.e. obtain the sheet BiOBr light of high-crystallinity
Catalytic film.The slide of three load BiOBr films is lain against 60ml and dissolves AgNO3Methyl alcohol
In solution, Ag/Bi ratio is 3.0mol%, and with the uviol lamp photo-reduction that emission wavelength is 365nm
15min.Clean with ultra-pure water and dry under sample surfaces, room temperature.
The process of fluorescence disk reactor degraded simulating pollution thing rhodamine B (RhB) is as follows: at fluorescence
Disk reactor outer surface sticks the sheet glass being coated with catalyst film of 4 22 × 20mm.With 55
ML15mg/L RhB solution is as reaction solution, and the rotating disk area remained immersed in solution is
43%.With 300W xenon lamp as light source, and filter off the light less than 420nm with optical filter.Rotating disk turns
Speed is 90rpm, and reaction temperature is 30 DEG C.Before carrying out photocatalytic activity test, sample is instead
Dark absorption 40min in liquid is answered to reach adsorption equilibrium, then to turn on light and carry out degradation reaction, every 25min
Sampling.Closing xenon lamp after reaction 1h, continuous illumination is continued degraded because extinction reaches saturated by fluorescent material
RhB.UV spectrophotometer is used to measure its absorbance at characteristic absorption wavelength 553nm of RhB,
Calculate the degradation rate of differential responses time.
The cubic BiOBr that film is high-crystallinity obtained by the XRD stave of the present embodiment is bright in Fig. 1
Crystalline phase, free from admixture generates.In Fig. 2, XPS collection of illustrative plates shows, the Ag of the present embodiment is the form with simple substance
It is present in BiOBr surface.In Fig. 3, UV-vis DRS collection of illustrative plates shows the Prusman of Ag in the present embodiment
Effect enhances the light absorpting ability of 440-500nm visible region.In Fig. 4-5, the present embodiment is in nothing
Simulating pollution thing rhodamine B of degrading in the disk reactor of fluorescent material has optimal photocatalytic activity,
To the degradation rate of rhodamine B close to 80%.In Fig. 6, the present embodiment is degraded in fluorescence disk reactor
After RhB mono-hour, close radiation source and continue degraded merely with fluorescent material luminous (emission wavelength is
480nm), degradation rate increases by 16%.And during unstressed configuration powder, then degradation reaction cannot occur.
Embodiment 2
Identical with the method preparing BiOBr film catalyst in embodiment 1, do not deposit Ag particle.Figure
The cubic BiOBr crystalline phase that film is high-crystallinity obtained by the XRD stave of the present embodiment is bright in 1,
Free from admixture generates.In Fig. 3, the UV-vis DRS collection of illustrative plates of the present embodiment shows that BiOBr film catalyst is to visible
Light has certain absorbability.Fig. 4 has degradation to RhB under the present embodiment visible ray.
Embodiment 3
The ratio of Ag/Bi is tuned as 1.5mol%, and other guide is identical with described in embodiment 1.Figure
In 2, XPS collection of illustrative plates shows, the Ag of the present embodiment is to be present on BiOBr with the form of simple substance.Fig. 4
Under middle the present embodiment visible ray, RhB had degradation.
Embodiment 4
The ratio of Ag/Bi is tuned as 4.5mol%, and other guide is identical with described in embodiment 1.Figure
In 2, XPS collection of illustrative plates shows, the Ag of the present embodiment is to be present on BiOBr with the form of simple substance.Fig. 4
Under middle the present embodiment visible ray, RhB had degradation.
Embodiment 5
The ratio of Ag/Bi is tuned as 6.0mol%, and other guide is identical with described in embodiment 1.Figure
In 2, XPS collection of illustrative plates shows, the Ag of the present embodiment is to be present on BiOBr with the form of simple substance.Fig. 4
Under middle the present embodiment visible ray, RhB had degradation.
Embodiment 6
The photo-reduction time is tuned as 10min, and other guide is identical with described in embodiment 1.In Fig. 5
Under the present embodiment visible ray, RhB had degradation.
Embodiment 7
The photo-reduction time is tuned as 20min, and other guide is identical with described in embodiment 1.In Fig. 5
Under the present embodiment visible ray, RhB had degradation.
Embodiment 8
The photo-reduction time is tuned as 25min, and other guide is identical with described in embodiment 1.In Fig. 5
Under the present embodiment visible ray, RhB had degradation.
Claims (3)
1. apply a fluorescence disk reactor for Ag/BiOBr visible light catalytic film, described rotating disk material
Matter is quartz glass, it is characterised in that it is thin that described rotating disk outer surface posts Ag/BiOBr visible light catalytic
Film, rotating disk is built with fluorescent material.
The fluorescence rotating disk of application Ag/BiOBr visible light catalytic film the most according to claim 1 is anti-
Answer device, it is characterised in that described Ag/BiOBr visible light catalytic film is that Ag nano particle is deposited on sheet
On shape BiOBr visible light catalytic film, sheet BiOBr visible light catalytic film is firmly tied with substrate of glass
Closing, wherein BiOBr crystal formation is the cubic BiOBr crystalline phase (JCPDS93-0393) of pure phase.
The fluorescence rotating disk of application Ag/BiOBr visible light catalytic film the most according to claim 1 is anti-
Answer device, it is characterised in that the preparation of described Ag/BiOBr visible light catalytic film comprises the following steps:
(1) glass surface treatment:
Ultrasonic to common soda lime glass priority hydrochloric acid solution and absolute ethyl alcohol cleaning is placed on 80 DEG C of baking ovens
Be dried, afterwards the sheet glass of drying is stood in water heating kettle, add deionized water, put into baking oven in
Keep 6h at 180 DEG C, clean three times by absolute ethyl alcohol and deionized water after taking-up, place under room temperature dry
Dry；
(2) preparation of BiOBr film:
Weigh Bi (NO3)3·5H2O adds in the mixed solution of ethylene glycol and isopropanol, ethylene glycol and isopropyl
The volume ratio of alcohol is 5:35, and stirring adds the 1-ten that Br/Bi mol ratio is 2:1 after making it be completely dissolved
Six alkyl trimethyl imidazoles bromide ([C16Min] Br), continue stirring and clarify to solution, by processed good
Sheet glass stand in water heating kettle after add gained settled solution, at 160 DEG C, react 12h, instead
After taking out sheet glass ethanol washing three times after should and being dried at room temperature for, at 450 DEG C, roasting 4 is little
Time, obtain being loaded with the sheet glass of sheet BiOBr visible light catalytic film；
(3) deposition Ag nano particle: the sheet glass of sheet BiOBr visible light catalytic film will be loaded with
Lie against AgNO3Methanol solution in, in solution, Ag content with the mol ratio of Bi content in film is
1.5-6.0%, reduces by UV illumination, and the photo-reduction time is 10-25min, then clear with ultra-pure water
Wash clean film surface, dries sheet glass under room temperature.
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| CN104549269B (en) * | 2014-12-31 | 2017-03-15 | 上海师范大学 | Ultrasonic wave added photoreduction met hod deposits Ag particles to prepare hollow shell structure Ag/Bi2WO6The method of photocatalyst |
| 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 |
| CN108816253A (en) * | 2018-05-31 | 2018-11-16 | 宁夏大学 | A kind of Au/Bi24O31Br10Composite photo-catalyst and preparation method thereof |
| 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 |
| 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 |
| CN113546523B (en) * | 2021-07-23 | 2023-03-31 | 上海师范大学 | PVDF ultrafiltration membrane of composite Ag @ BiOBr photocatalytic material and preparation method and application thereof |
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| CN101850263A (en) * | 2010-06-17 | 2010-10-06 | 江西理工大学 | Ag doped BiOBr catalytic material and preparation method and application thereof |
| CN102295318B (en) * | 2011-08-18 | 2012-10-03 | 河南工程学院 | Nanometer rotating disc photocatalytic water treatment device |
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