CN109589877A - The small fluidized-bed reactor of airwater mist cooling photocatalysis - Google Patents
The small fluidized-bed reactor of airwater mist cooling photocatalysis Download PDFInfo
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- CN109589877A CN109589877A CN201811601241.6A CN201811601241A CN109589877A CN 109589877 A CN109589877 A CN 109589877A CN 201811601241 A CN201811601241 A CN 201811601241A CN 109589877 A CN109589877 A CN 109589877A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00004—Scale aspects
- B01J2219/00011—Laboratory-scale plants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/0873—Materials to be treated
- B01J2219/0892—Materials to be treated involving catalytically active material
Abstract
The invention discloses the small fluidized-bed reactors of airwater mist cooling photocatalysis, the small fluidized-bed reactor of airwater mist cooling photocatalysis, bead including quartz ampoule and in quartz ampoule, bottom is equipped with gas-liquid distribution device in quartz ampoule and the quartzy bottom of the tube in the lower section of gas-liquid distribution device is provided with import, import is connected to conveyance conduit, overflow weir is provided at the top of quartz ampoule, liquid outlet is provided on overflow weir, liquid stream weir crest portion is provided with gas discharge outlet, and liquid outlet is connected to by liquid discharge tube line with air-tight bottle；It is connected to by the first connecting pipeline with the liquid-inlet of conveyance conduit for conveying the outlet of the first micro-injection pump of liquid, it is connected to by the second connecting pipeline with the gas feed of conveyance conduit for conveying the outlet of the second micro-injection pump of gas, a unidirectional stop valve is connected in the second connecting pipeline.The present apparatus improves reaction rate, keeps intensity of illumination relatively uniform, decays small.
Description
Technical field
The present invention relates to photocatalysis technology, sewage treatment field more particularly to the small fluidized-bed reactions of airwater mist cooling
Device technology.
Background technique
The gas-liquid-solid small fluidized-bed reactor of photocatalysis has important answer in industrial circles such as chemical industry, the energy and environment
Still relevant patent report is not seen still both at home and abroad with prospect.Compared with fixed bed, fluidized-bed reactor is shown
Following advantages: mixability is strong, mass transfer rate high (Renewable Energy, 2014,71:276-285；
Chem.Eng.Sci., 2001,56 (2): 293-303) [21,22], temperature gradient it is small (Environ.Chem.Eng.J., 2013,
1 (3): 150-158) [23], reaction temperature is controllable.Compared with macroreaction device, microresponse system due to its characteristic size compared with
It is small, chemical synthesis, Reaction kinetics research, in terms of have big advantage (CES, 2001,56 (2): 293-
303)[22]: since higher mass transfer, heat transfer efficiency can be achieved in the reduction of mass transfer distance；More easily realize the collection of functionalization structure
At reduction equipment room property depending therefrom.Microresponse device is applied to photocatalytic degradation organic sewage field and has the advantage that
(Cur rent Opinion in Chem.Eng.,2013,2(3):338-345；Photochem.&Photobio.Sci.,
2008,7(11):1313-1322)[28,29]: the characteristic size of microresponse device ensures that radiation profiles are relatively equal in reactor
It is even；Reaction time is controllable；The application for minimizing light source (LED) not only can reduce reaction system size, reduce energy consumption,
And since its fuel factor does not make the cost that reaction temperature is more uniform, reduces cooling equipment significantly.Chinese patent
(there are the board-like photocatalysis microreactor of the titanium dioxide of metal ion mixing in Liu Mingyan etc., University Of Tianjin to CN201410415832.X
And the preparation method of catalyst reactor film) a kind of flat photocatalysis microreactor has been invented, it is used for photocatalytic degradation
Organic sewage.Further, Chinese patent CN106215827A (Liu Mingyan etc., University Of Tianjin, the liquid-solid small fluidisation of photocatalysis
Bed reactor), liquid-solid small fluidized bed of the one kind for photocatalysis degradation organic contaminant has been invented, Fe has been probed into3+Modification
TiO2Efficiency and the preliminary examinations enlarge-effect of small fluidized-bed reactor as photocatalyst for degrading MB.Chinese patent
It is micro- that CN106237953A (Liu Mingyan etc., University Of Tianjin, the small bubbling column reactor of photocatalysis solution-air) has invented a kind of solution-air
Small bubble tower structure of reactor, in the small bubbling column reactor of solution-air, new gas distributor can be realized in small bubble tower
The flow pattern of multiple microbubble dispersion stream.Above-mentioned structure of reactor respectively after introducing fluidized particles, a variety of heavy bubbles of dispersion,
The mass-transfer performance of reactor greatly promotes, but still that there are treating capacities is too low, and the requirement of industrial applications is not achieved.
Catalyst is in small fluidized-bed reaction system there are two types of application form: be freely suspended in aqueous solution, it is immobilized in
Inert substrate surface.For TiO2Suspension system, can be achieved higher catalyst illumination specific surface area in microreactor, but by
It is needed before discharge in sewage after processing by TiO2It is filtered to remove in advance, this just needs to increase by one after mud reactor
A liquid-solid separator, since ultrafine particles low separation efficiency, the meeting of cost of equipment valuableness are so that entire reaction system installation and behaviour
It is greatly increased as expense.In addition to this, due to TiO2With strong absorption of the dark dye to photon radiation radiation is seeped
Saturating distance is restricted.Therefore the disadvantages mentioned above of mud reactor makes the amplification of its scale become very difficult.
Immobilized TiO2The advantages of catalyst film, is embodied in: not needing to carry out catalyst granules to treated sewage to divide
From processing so that sewage treatment can operate continuously；Catalyst film micropore provides biggish surface area for carrying out photocatalytic degradation
Contaminant molecule；All catalyst films can obtain uniform illumination in reactor, improve the utilization rate of catalyst.However,
There is also some disadvantages for solid-carried catalyst: reactant and the diffusion length of photon radiation increase so that low flow velocity operating condition
Influence of the lower external diffusion to mass transfer rate is significant；When catalyst film increases to certain thickness, close to the catalyst of bases
Its utilization rate is reduced since enough radiation intensity can not be received.
Summary of the invention
The purpose of the present invention is to provide a kind of characteristic sizes between microreactor and macroreaction device, both combined
The advantages of microreactor and macroscopical fluidized-bed reactor, but it is small to overcome microreactor treating capacity, macroscopical fluidized-bed reactor
The disadvantages of reaction time is long, the small fluidized-bed reactor of airwater mist cooling photocatalysis of degradation efficiency with higher.
The small fluidized-bed reactor of airwater mist cooling photocatalysis of the invention, the small fluidisation of airwater mist cooling photocatalysis
Bed reactor, the bead including quartz ampoule and in the quartz ampoule, in the quartzy inside pipe wall and bead
Load has catalyst film, the setting of source alignment quartz ampoule on outer surface, and the quartz ampoule waterpower internal diameter is 3-10mm, wall
Thick 0.1-2.0mm, length 20-100mm, bead diameter are 50-250 μm, and bottom is equipped with gas-in the quartz ampoule
Liquid distributor and quartzy bottom of the tube in the lower section of gas-liquid distribution device are provided with import, and the import and conveyance conduit connect
It is logical, it is provided with overflow weir at the top of the quartz ampoule, liquid outlet is provided on the overflow weir, liquid stream weir crest portion opens
There is gas discharge outlet, the liquid outlet is connected by liquid discharge tube line with the brown air-tight bottle being immersed in cooling water glass
It is logical；
For convey liquid the first micro-injection pump outlet by the liquid of the first connecting pipeline and conveyance conduit into
Mouth connection, for conveying the gas feed that the outlet of the second micro-injection pump of gas passes through the second connecting pipeline and conveyance conduit
Connection, is connected with a unidirectional stop valve in second connecting pipeline.
Using the beneficial effects of the present invention are:
The fluidisation of particle in the 1 small fluidized-bed reactor of airwater mist cooling photocatalysis, the disturbance of bubble make reactant with
Catalyst is uniformly mixed, and resistance to mass tranfer is small, compared with the mass tranfer coefficient in general single-phase microreactor, improves a quantity
Grade.The only particulate load catalyst compared with general photocatalysis is liquid-solid fluidized bed, the inner surface of silica tube of small fluidized-bed reactor
With the equal supported catalyst in bead outer surface, additional photocatalysis area provided by inner surface of silica tube is further improved instead
Answer rate.
The characteristic size of the 2 small fluidized-bed reactors of airwater mist cooling photocatalysis is 3-10mm, between microreactor and
Between macroreaction device.Compared with microreactor, the increase of characteristic size can be such that the treating capacity of reactor significantly improves；With it is macro
It sees reactor to compare, the reduction of characteristic size, strong reduces catalyst granules to the blocking of light and solution to light
Absorption keeps intensity of illumination relatively uniform, decays small.
The average response rate and microreactor of the 3 small fluidized-bed reactors of airwater mist cooling photocatalysis are close, meanwhile,
Its reaction time is several minutes, far below a few hours of macroreaction device.It therefore is a kind of very efficient, while treating capacity is opposite
Biggish photo catalysis reactor.
Detailed description of the invention
Fig. 1 is the reaction unit schematic diagram of the small fluidized-bed reactor of airwater mist cooling photocatalysis；
Fig. 2 is the small fluidized-bed reactor internal quantum efficiency of airwater mist cooling photocatalysis；
Fig. 3 is the degradation efficiency of MB solution in the small fluidized-bed reactor of airwater mist cooling photocatalysis；
Fig. 4 is the small fluidized-bed reactor inner transmission matter coefficient of airwater mist cooling photocatalysis.
Specific embodiment
The present invention is described in detail in the following with reference to the drawings and specific embodiments.
The small fluidized-bed reactor of airwater mist cooling photocatalysis of the invention as shown in Figure 1, including quartz ampoule 5 and dress
Bead in the quartz ampoule 5, load has catalyst on the outer surface of 5 inner wall of quartz ampoule and bead
Film.The catalyst film can be prepared using sol-gal process, and be loaded with dip-coating method.Light source 6 is directed at quartz
Pipe 5 is arranged.Light source 6 can be LED light, xenon lamp or sunlight.
The 5 waterpower internal diameter of quartz ampoule is 3-10mm, wall thickness 0.1-2.0mm, length 20-100mm, bead diameter
It is 50-250 μm.Bottom is equipped with gas-liquid distribution device 7 and the stone in the lower section of gas-liquid distribution device 7 in the quartz ampoule
English bottom of the tube is provided with import.The import is connected to conveyance conduit, be provided at the top of the quartz ampoule overflow weir 4 with
It prevents catalyst granules to be carried over, liquid outlet is provided on the overflow weir 4, liquid stream weir crest portion is provided with gas discharge
Mouthful.The liquid outlet is connected to by liquid discharge tube line with the brown air-tight bottle 3 being immersed in cooling water glass 2.By
Liquid after photocatalytic degradation is flowed out from 4 liquid outlet of overflow weir, and solution is by the brown air-tight bottle that is immersed in cooling water glass 2
3 collect, to prevent from causing the inaccuracy of test data due to test solution evaporation.
For convey liquid the first micro-injection pump 1 outlet by the liquid of the first connecting pipeline and conveyance conduit into
Mouthful connection, for convey gas the second micro-injection pump 9 outlet by the gas of the second connecting pipeline and conveyance conduit into
Mouth connection, a unidirectional stop valve 8 is connected in second connecting pipeline, avoids making liquid due to misoperation
Reflux enters gas syringe, and keeps stable gas pressure in operating process syringe.
Embodiment 1
The first step, catalyst load.
Using the present apparatus before carrying out light-catalyzed reaction, the TiO of one layer of doping Fe element is coated in silica inner surface2Light
Catalyst-Fe-TiO2/ quartz ampoule coats the TiO of one layer of doping Fe element in bead outer surface2Photochemical catalyst-Fe-TiO2/
Bead.
It is prepared with Fe first3+The sol gel solution of doping, then, with dip-coating method in inner surface of silica tube and glass
Pearl outer surface lifts plated film, and finally sintering forms catalyst film.
Second step makes the small fluidized-bed reactor of airwater mist cooling photocatalysis.5 waterpower internal diameter of quartz ampoule is 6mm, wall
Thick 1mm, length 100mm, bead diameter are 150 μm.Micro-injection pump 1 is used to convey methylene blue (methylene
Blue, MB) solution, micro-injection pump 9 be used to convey air.Quartzy bottom of the tube has solution-air body distributor 7.Overflow weir 4 is arranged at top
To prevent catalyst granules to be carried over.A unidirectional stop valve 8 is connected between gas-liquid distribution device 7 and air syringe 9, is avoided
Make liquid reflux enter gas syringe due to misoperation, and keeps stable gas pressure in operating process syringe.Described
Gas-liquid distribution device 7 have the entrance of gas and liquid below, have the outlet of gas and liquid on overflow weir 4.
Third step carries out light-catalyzed reaction.
Fe-TiO will be coated under dark surrounds2Bead be put into the MB solution to be degraded of respective concentration and stir
30min, to reach adsorption equilibrium.This reaction is intermittently operated.The small fluidized-bed reactor of photocatalysis in the process of running, every time
Recycle feed amount is 20mL.The radiant power of Xe lamp source is 150,200,250W.The initial height of bed H of catalyst bead0Point
Not Wei 5,10 and 15mm, MB solution initial concentration C0It is 10,20,30mgL-1, the charging rate of MB solution is respectively
10.80,12.96,15.12,17.28,19.44mL min-1；The charging rate of air is respectively 4,5,6,7,8mL min-1.Three
Mutually small photocatalysis fluid bed interior typical flow pattern belongs to bubble dispersion stream flow pattern.
4th step estimates photocatalysis quantum efficiency.Generally in the immobilized photocatalysis microresponse device of catalyst, quantum effect
It is micro- that rate is distributed in 0.0162%-0.0262%LED light source microchannel photo catalysis reactor, 0.103%-0.378%UV-LED more
Between channel photo catalysis reactor, the board-like photo catalysis reactor in 0.25% microchannel.Apparent quantum efficiency under this example system
Between 0.1877%-0.4441%, such as Fig. 2, more general photo catalysis reactor quantum efficiency increases at multiple.
Under different superficial liquid velocities, the small three-phase fluid bed reactor of photocatalysis be used for degrade MB solution when degradation rate such as
Shown in Fig. 3.As can be seen that (19.44mL min when fluid flow or larger liquid speed-1), degradation rate is more than 90% after 12 minutes.?
In xenon lamp ultraviolet light content so it is low in the case where, show very high photocatalytic activity.
Mass tranfer coefficient matched curve is passed through gas as shown in figure 4, under the conditions of the identical initial height of bed and superficial liquid velocity
Small airwater mist cooling fluidisation passes the mass tranfer coefficient of bed, is that the small Fluid-particle two-phase flows fluidized bed photocatalytic that no gas is passed through is anti-
3.73-4.42 times or so for answering device (referring to Chinese patent CN106215827A)；In the identical initial height of bed and superficial gas velocity item
Under part, mass tranfer coefficient when liquid Reynolds number is 60.25 is 2.2 times that Reynolds number is 33.47.
Based on above-mentioned analysis, the small gas-liquid-solid three-phase fluidized bed photo catalysis reactor of more bubbles and small liquid-solid two
Phase fludized bed photoreactor and small vapor-liquid two phases bubble tower photo catalysis reactor are (referring to Chinese patent
CN106237953A it) compares, mass tranfer coefficient dramatically increases, and the performance of photo catalysis reactor is further improved.In this reality
Under the operating condition of example system, the Multiphase Flow in small triphsic fluidized bed shows bubble dispersion stream.It is more
Weight microbubble can not only increase the level of disruption of solution, while can also provide higher specific surface area and promote to pass between gas, liquid
Matter.
Claims (1)
1. the small fluidized-bed reactor of airwater mist cooling photocatalysis, the glass including quartz ampoule and in the quartz ampoule
Pearl, load has catalyst film on the outer surface of the quartzy inside pipe wall and bead, and source alignment quartz ampoule is arranged,
It is characterized by: the quartz ampoule waterpower internal diameter is 3-10mm, wall thickness 0.1-2.0mm, length 20-100mm, bead is straight
Diameter is 50-250 μm, and bottom is equipped with gas-liquid distribution device and the stone in the lower section of gas-liquid distribution device in the quartz ampoule
English bottom of the tube is provided with import, and the import is connected to conveyance conduit, is provided with overflow weir at the top of the quartz ampoule,
Liquid outlet is provided on the overflow weir, liquid stream weir crest portion is provided with gas discharge outlet, and the liquid outlet passes through liquid
Body discharge pipe is connected to the brown air-tight bottle being immersed in cooling water glass；
Connected for conveying the outlet of the first micro-injection pump of liquid by the liquid-inlet of the first connecting pipeline and conveyance conduit
It is logical, connected for conveying the outlet of the second micro-injection pump of gas by the gas feed of the second connecting pipeline and conveyance conduit
It is logical, a unidirectional stop valve is connected in second connecting pipeline.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110776048A (en) * | 2019-11-13 | 2020-02-11 | 上海理工大学 | Design of small-sized series packing type reaction device |
| CN111974314A (en) * | 2019-05-22 | 2020-11-24 | 天津西敦津洋环保科技有限公司 | Micro-fluidized bed reactor and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111974314A (en) * | 2019-05-22 | 2020-11-24 | 天津西敦津洋环保科技有限公司 | Micro-fluidized bed reactor and application thereof |
| CN110776048A (en) * | 2019-11-13 | 2020-02-11 | 上海理工大学 | Design of small-sized series packing type reaction device |
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