CN1307416C - Multichannel rapid evaluating device for photolysis hydrogen making catalyst performance - Google Patents
Multichannel rapid evaluating device for photolysis hydrogen making catalyst performance Download PDFInfo
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- CN1307416C CN1307416C CNB2004100261027A CN200410026102A CN1307416C CN 1307416 C CN1307416 C CN 1307416C CN B2004100261027 A CNB2004100261027 A CN B2004100261027A CN 200410026102 A CN200410026102 A CN 200410026102A CN 1307416 C CN1307416 C CN 1307416C
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Abstract
The present invention discloses a multiple-channel device for rapidly evaluating the performance of a hydrogen catalyst prepared by photodecomposition, which comprises a cylindrical light reactor, wherein the center of the light reactor is provided with a light source driven to rotate by an asynchronous motor, a plurality of quartz reactors are uniformly distributed around the light source, each quartz reactor is provided with a magnetic stirring motor, and all the quartz reactors are led out of the light reactor by pipelines. The inner volumes of the pipelines corresponding to all the quartz reactors are the same. Each of the pipelines is provided with a nitrogen bottle and a vacuum pump. The outlets of all the pipelines are in one-to-one correspondence with corresponding points on a film glass plate coated with Pd/WO3. the device of the present invention has the advantages that the hydrogen catalyst prepared by photodecomposition is sieved and photodegraded with a combined chemical method, multiple groups of hydrogen catalysts are simultaneously prepared by photodegrading water under the same condition, and the hydrogen production quantity of each reactor is rapidly detected. The device can be combined with a chromatograph or an ultraviolet spectrograph, and is used for evaluating and researching the performance of the photodecomposition pollutant of a photochemical catalyst.
Description
Technical field
The invention belongs to the photochemistry experimental provision, relate to, the quick evaluating apparatus of particularly a kind of hyperchannel photodissociation catalyst for preparing hydrogen performance photodissociation catalyst for preparing hydrogen performance detection.
Prior art
In photocatalysis field, produce hydrogen etc. as photocatalysis degradation organic contaminant, photocatalysis decomposing water with solar energy, all relate to the development and the screening of high efficiency photocatalyst, and the rapid screening of photocatalyst is significant for the researcher.In the compound of nature and synthetic, compound with photocatalytic activity is a lot, and owing to lack effective photocatalysis performance (particularly photolysis water hydrogen performance) valuator device fast, screening effeciency is not high, therefore the photocatalysis performance of most compounds can't be verified, and makes many compounds that might have fine photocatalytic activity not obtain exploitation.Being and not being between while selection of catalysts or the activity, the energy difference is very little, and (the transition state energy variation only is 4.19～8.37kJ/mol).Therefore when the factor generation subtle change such as structure, reaction conditions or substrate structure of catalyzer, be difficult for predicting the change of catalyst performance.Up to now, the method that the mankind are used for photocatalyst performance evaluation all needs to have no way of various potential possibilities are examined or check based on traditional like this catalyst performance evaluation mode through once carry out a kind of very long process of photocatalysis experimental study of photocatalyst at a reactor at all.Experimental technique in open source literature generally carries out in a reactor.As several photocatalysis treatment water systems that " to being used for the research of the reactor that various coupling light catalysis that water purifies and film handle " (the Studies on variousreactor configurations for coupling photocatalysis and membrane processes inwater purification) of " membrane science magazine " (J Membrane Science) 206 (2002) 399-415 report summarized, all be based on the reactive system of a reactor." the Cu of and for example " international inorganic material magazine " (Int J Inorg Mater) 2 (2000) 339-346 report
2+Synthetic and the photochemical properties of doping layered titanic acid hydrogen salt " (Synthesis andphotochemical properties of Cu
2+Doped layered hydrogen titanate) Photoreactor of Cai Yonging is also only used a reactor.The current experiments device of open report can only be evaluated and tested a kind of catalytic performance of photocatalyst owing to all only use a reactor at every turn in the world, and efficient is very low when photocatalyst is done screening.Therefore, press for the experimental provision that to estimate and to screen a large amount of compound photocatalysis performances fast,, select and find new photocatalyst significantly to increase work efficiency.
According to the data-searching that the applicant carried out, do not see as yet at present both at home and abroad has the report of organizing the reaction unit that catalyzer photocatalytic hydrogen production by water decomposition performances detect simultaneously and estimate can satisfy more.
Summary of the invention
The objective of the invention is to, provide a kind of hyperchannel photodissociation catalyst for preparing hydrogen performance quick evaluating apparatus, utilize Pd/WO
3Film comes rapid screening decomposition water photocatalyst to the variable color response difference of different hydrogen concentration, utilize quartzy chilled water unit to control the temperature of reaction unit, utilize quartz reactor to center on that light source evenly distributes, controls the light source rotating and the cylinder type shell makes each reactor be subjected to light even relatively, utilization makes the pipeline volume of each reactor correspondence identical to the control of pipeline, realized can relatively screen multiple candidate compound photolysis water hydrogen performance simultaneously, realized the miniaturization of reactor simultaneously, significantly reduced requirement tested compound.
To achieve these goals, the technical scheme that the present invention takes is, the quick evaluating apparatus of a kind of hyperchannel photodissociation catalyst for preparing hydrogen performance, it is characterized in that, the photoreaction system that comprises a cylinder type shape, central authorities at photoreaction system are provided with a light source by the asynchronous machine driven rotary, and filter the light of the following wavelength of 400nm in the light source; Light source places in the quartzy chuck, and this quartz chuck can lead to chilled water light source is cooled off, or logical 1molL
-1NaNO
2Solution is with the cooling light source; Be provided with a plurality of quartz reactors around evenly distributing of light source on every side, each quartz reactor disposes the magnetic agitation motor, each quartz reactor is drawn photoreaction system by pipeline, volume in the pairing pipeline of each quartz reactor is identical, pipeline is communicated with nitrogen cylinder and vacuum pump, and the outlet of each pipeline is one by one corresponding to being coated with Pd/WO
3Respective point on the film glass plate.
Some other characteristics of the present invention are that described asynchronous machine has relay, speed regulator and positive and negative rotating controller, with the positive and negative rotation of control asynchronous machine.
Described light source is arranged on the asynchronous machine top, makes each quartzy reactor be subjected to light even relatively by the rotation of controlling asynchronous machine.
Described light source is mercury lamp (or xenon lamp or halogen tungsten lamp or metal halid lamp).
The specification of described quartz reactor is 10ml～500ml.
Described Pd/WO
3Film is clipped in the organic glass clip hermetically.
The upper plate of described organic glass clip has ladder type body groove, can also place to be used for Pd/WO in groove
3The film glass plate heats the heating plate of temperature control.
Adopt assessment device of the present invention can improve compound photocatalysis hydrogen production performance evaluating efficient in unit interval and the unit space, and then improve the screening effeciency of photodissociation catalyst for preparing hydrogen.
Description of drawings
Fig. 1 is a device block diagram of the present invention;
Fig. 2 is an Electric Machine Control part block diagram of the present invention;
Fig. 3 is a photoreaction system structural representation of the present invention;
Fig. 4 is a gas detection part-structure synoptic diagram of the present invention;
Fig. 5 is an organic glass clip stereographic map of the present invention;
Fig. 6 is the vertical view of organic glass clip train wheel bridge of the present invention;
Fig. 7 is the vertical view of organic glass clip lower plate of the present invention;
Fig. 8 is the relation curve of film variable color degree (transmitance) and CdS amount;
Fig. 9 is a film variable color scintigram.
Embodiment
The present invention is described in further detail for the embodiment of the assessment device of finishing according to technical scheme of the present invention below in conjunction with accompanying drawing and inventor.
As shown in Figure 1, the quick evaluating apparatus of a kind of hyperchannel photodissociation catalyst for preparing hydrogen performance, the photoreaction system that comprises a cylinder type shape, central authorities at photoreaction system are provided with a light source by the asynchronous machine driven rotary, be provided with a plurality of quartz reactors around evenly distributing of light source on every side, each quartz reactor disposes the magnetic agitation motor, each quartz reactor is drawn Photoreactor by pipeline, volume in the pairing pipeline of each quartz reactor is identical, pipeline is communicated with nitrogen cylinder and vacuum pump, and the outlet of each pipeline is one by one corresponding to being coated with Pd/WO
3Respective point on the film glass plate.
The present invention mainly is divided into Electric Machine Control part, photoreaction system, gas detection part.
The Electric Machine Control part: as shown in Figure 2, comprise the magnetic agitation motor, it is used for the magnetic agitation of reactor; Asynchronous machine, it is used to make light source to rotate uniformly; Speed regulator, it is used for the speed governing of asynchronous machine, and speed adjustable range is 0-7r/min; Positive and negative rotating controller, it is used to regulate the rotating of asynchronous machine; Relay, it is used for cooperating the rotating of control asynchronous machine with positive and negative rotating controller.
Photoreaction system: as shown in Figure 3, constitute light source 36, and filter the light of the following wavelength of 400nm by mercury lamp (or xenon lamp or halogen tungsten lamp or metal halid lamp); It is placed in the quartzy cooling jacket 34, and this quartz chuck can lead to chilled water light source is cooled off, or logical 1molL
-1NaNO
2Solution is with the cooling light source, and its power lead inlet is 310, rotates under asynchronous machine 31 drives, and asynchronous machine is by motor controling part control rotating speed and rotating; Chilled water or 1molL
-1NaNO
2Entered by water inlet (38), enter the water inlet 35 of quartzy cooling jacket 34 by water delivering orifice 37 through emulsion tube then, the water delivering orifice 312 by quartzy cooling jacket 34 enters 311 through emulsion tube then, goes out from water delivering orifice 39 at last.
Quartz reactor (33 among the figure, 313) (other does not draw in order to be evenly distributed in a plurality of 10～500ml quartz reactors around the light source two, present embodiment is 6 quartz reactors), they are fixed on the cylinder made from the 1mm steel plate, and their bottoms are placed with magnetic agitation motor 32,314.
Gas detection part: as shown in Figure 4, at first 8 ball valve 44-411 are opened, with vacuum pump pipeline is vacuumized, close ball valve 411 then, open nitrogen cylinder, to the logical nitrogen of pipeline, close ball valve 410 then, open ball valve 411, again pipeline is taken out vacuum one time, fully to remove the oxygen in the pipeline, close ball valve 44-49 then; The gas that produces among the quartz reactor 1-6 is system 42 by the road, is imported into the Pd/WO of correspondence as shown in Figure 7 respectively independently
3On the film glass plate point.
First characteristics of assessment device of the present invention are: the Electric Machine Control part is made up of magnetic agitation motor, asynchronous machine, speed regulator, positive and negative rotating controller, relay, transformer, speed regulator is connected with asynchronous machine by relay, positive and negative rotating controller is connected with asynchronous machine by relay, and the magnetic agitation motor is connected with power supply by transformer; Asynchronous machine is connected with quartzy cold air water leg by rotating shaft.By such design, the present invention utilizes low cost equipment to realize carrying out simultaneously the reaction of many group photocatalytic hydrogen production by water decomposition under the condition of magnetic agitation.
Second characteristic of assessment device of the present invention are: photoreactive moiety is by light source, quartzy cooling water jecket, quartz reactor, circular housing, the round barrel cover of cylinder and band cooling water outlet and inlet and power lead inlet is formed, quartzy cooling water jecket is fixed in the asynchronous machine rotating shaft, mercury lamp (or xenon lamp or halogen tungsten lamp or metal halid lamp) places quartzy cooling water jecket the inside, mercury lamp (or xenon lamp or halogen tungsten lamp or metal halid lamp) power lead is inserted by round barrel cover, cooling water outlet and inlet above the round barrel cover is connected with cooling water outlet and inlet on the quartzy cooling water jecket by pipe, quartz reactor is placed on the reactor jacket that is fixed on the circular housing, and reactor jacket is evenly distributed on around the light source.Because the emitting space skewness of commercial mercury lamp (or xenon lamp or halogen tungsten lamp or metal halid lamp) itself and the photon absorbing intensity inequality of quartzy cooling water jecket, light distribution is different around the light source at one time, the present invention is by allowing quartzy cooling jacket rotate together and the design of circular housing with light source, solve the uneven problem of light distribution well, made each reactor be subjected to light identical; Because the light source rotation can make chilled water turnover pipe and power lead stranded, the present invention has solved this problem by controlling quartzy cooling jacket well with the design of light source rotating together and round barrel cover.
The 3rd characteristics of apparatus of the present invention are: the gas detection part is made up of pipe system 42 and organic glass clip 43, the pipe that comes out from quartz reactor 1-6 passes through bifurcated, one the tunnel is connected with hole 71-76 on the organic glass clip, another road is connected with ball valve 44-49, the ball valve 44-49 other end is connected with pipe 412, pipe 412 is connected with ball valve 410,411, ball valve 410 is connected with nitrogen cylinder, ball valve 411 is connected with vacuum pump, wherein the length of pipe is identical with the thickness degree in each pipeline, and is the same with the spatial volume that guarantees each quartz reactor correspondence.As shown in Figure 5, the organic glass clip is made up of train wheel bridge 51, lower plate 52, two logical 53, and shown in figure six, train wheel bridge 51 has a ladder type body groove, as shown in Figure 7, ladder type body groove not only helps the stressed of glass plate film, can also put heating plate in groove glass plate is heated temperature control, with convenient variable color situation of observing film, have six holes in the middle of the lower plate, be stained with O-ring seal on the hole, the hole is connected with two logical 53, and two logical 53 directly are connected with pipeline.Be coated with Pd/WO
3The glass plate of film just can be clipped in the organic glass clip hermetically, has realized detecting six kinds of photocatalysts simultaneously with a coated glass pane.The present invention has realized utilizing the few material of simple and easy amount to reach and can vacuumize pipe system by such design, and can make the pipeline of each quartz reactor correspondence independent, guarantees the same requirement of pipeline spatial volume of each quartz reactor correspondence simultaneously.
The 4th characteristics of assessment device of the present invention are: Pd/WO
3Open source literature is adopted in the preparation of film: Sensors and Actuators B 50 (1998) 234-245 report " with the Pd/WO of sol-gel processing preparation
3The gas-discoloration effect of film " (Gasochromic effect of palladium dopedperoxopolytungstic acid films prepared by the sol-gel route) prepare Pd/WO
3The method of film is 20ml H
2O
2(30%) add in the 5g tungsten powder, the room temperature lower magnetic force stirred 6 hours, and is dissolved entirely up to tungsten powder.Excessive H is removed in 40 ℃ of water-baths (or Pt net) then
2O
2, adding the 38ml absolute ethyl alcohol subsequently, 80 ℃ of water-baths heating becomes the green-yellow of emulsus up to colloidal sol from milky, suction filtration, centrifuging obtains bluish yellow look transparency liquid, adds 0.1152g PdCl
2, magnetic agitation allows PdCl
2Fully dissolving, the reactant liquor color becomes dark brown, is kept at then in-25 ℃ the refrigerator-freezer; The colloidal sol that extraction 3ml makes during plated film drops on the glass plate; glass plate was placed in the acid sonic oscillation earlier 20 minutes; sonic oscillation 20 minutes in alkali lye then; at last deionized water for ultrasonic vibration 20 minutes; be used for plated film after drying, wait film to do back coating one deck polyurethane diaphragm on the film surface.The present invention utilizes inexpensive method to prepare Pd/WO
3The quick film of hydrogen.
The 5th characteristics of assessment device of the present invention are: carry out a plurality of light-catalyzed reactions under the identical situation of experiment condition simultaneously, can evaluate and test simultaneously the photocatalytic hydrogen production by water decomposition performance of a plurality of different compounds simultaneously, because the compound of being evaluated and tested is in identical reaction conditions, so the comparability height of experimental result.The evaluation and test and the screening effeciency of the compound photocatalysis hydrogen production performance in the unit interval unit space have greatly been improved simultaneously.
The applicant adds 10～500mlNa in each quartz reactor
2S, Na
2SO
3Solution adds the different CdS that measure again, produces the hydrogen experiment.Found that device can accomplish the end in view and effect well; Fig. 8 is the relation curve of film variable color degree (transmitance) and CdS amount, and Fig. 9 is a film variable color scintigram.Experiment condition is as follows:
| The quartz reactor numbering | CdS(mg) | Na 2S●9H 2O | Anhydrous Na 2SO 3 | Light source | Ultrapure water |
| 1 | 2 | 0.735g | 0.479g | The 300W high-pressure sodium lamp | 300ml |
| 2 | 4 | ||||
| 3 | 6 | ||||
| 4 | 8 | ||||
| 5 | 10 | ||||
| 6 | 12 | ||||
| 1 and a half hours reaction time, 35 ℃ of film heating-up temperatures | |||||
Below be the embodiment that the inventor provides.
Fig. 1 is the block scheme of an embodiment of apparatus of the present invention.Electric Machine Control part, photoreactive moiety and gas detection part in Fig. 2, Fig. 3 and Fig. 4 difference corresponding diagram 1.By the gas detection part pipeline is vacuumized earlier, ball valve shown in Figure 4 44,45,46,47,48,49,410,411 is opened, with vacuum pump pipeline is vacuumized, close ball valve 411 then, logical nitrogen, then shut-off valve (410), open ball valve 411, take out vacuum again one time, at last ball valve 44-49 is closed, make the pipeline of each quartz reactor correspondence become vacuum state.Magnetic agitation motor in the control part and asynchronous machine carry out work under motor controling part control then, and the magneton in the magnetic agitation driven by motor quartz reactor stirs, and asynchronous machine drives the speed rotating of light source with 1r/min.Then, give quartzy cooling water jecket logical chilled water, the reaction beginning to the light source energising.The gas that produces in the quartz reactor is directed in the corresponding organic glass clip (Fig. 5) by pipeline and is coated with Pd/WO
3On the point of film glass plate.The final hydrogen that produces is because of the Pd/WO that do not coexist of its amount
3Form six Bluepoints that are of different shades on the film glass plate, by ultraviolet-visible pectrophotometer 6 Bluepoints are carried out absorbance measurement, determine the size of hydrogen output in each reactor according to the size of absorbance separately, and analyze the photocatalysis performance that obtains adding in each reactor catalyzer thus.
Certainly, the quartz reactor of choosing according to different demands can be a plurality of, evenly be arranged on light source around, can achieve the above object equally.
This device and chromatogram or ultraviolet spectrometer (UVS) coupling can also be used for the evaluation and test research of photocatalyst light degradation pollutant performance.
Claims (7)
1. the quick evaluating apparatus of hyperchannel photodissociation catalyst for preparing hydrogen performance is characterized in that, comprises the photoreaction system of a cylinder type shape, in the central authorities of photoreaction system one light source by the asynchronous machine driven rotary is set, and filters the light of the following wavelength of 400nm; Light source places in the quartzy chuck, feeds chilled water or 1molL at quartzy chuck
-1NaNO
2Solution cools off light source; Be provided with a plurality of quartz reactors around evenly distributing of light source on every side, each quartz reactor disposes the magnetic agitation motor, each quartz reactor is drawn photoreaction system by pipeline, volume in the pairing pipeline of each quartz reactor is identical, pipeline is communicated with nitrogen cylinder and vacuum pump, and the outlet of each pipeline is one by one corresponding to being coated with Pd/WO
3Respective point on the film glass plate.
2. the quick evaluating apparatus of hyperchannel photodissociation catalyst for preparing hydrogen performance as claimed in claim 1 is characterized in that described asynchronous machine has relay, speed regulator and positive and negative rotating controller, is used to control the rotation of asynchronous machine.
3. the quick evaluating apparatus of hyperchannel photodissociation catalyst for preparing hydrogen performance as claimed in claim 1 or 2 is characterized in that, described light source is arranged on the asynchronous machine top, makes each quartz reactor be subjected to light even relatively by the rotation of controlling asynchronous machine.
4. the quick evaluating apparatus of hyperchannel photodissociation catalyst for preparing hydrogen performance as claimed in claim 1 is characterized in that, described light source is mercury lamp or xenon lamp or halogen tungsten lamp or metal halid lamp.
5. the quick evaluating method of hyperchannel photodissociation catalyst for preparing hydrogen performance as claimed in claim 1 is characterized in that the specification of described quartz reactor is 10ml～500ml.
6. the quick evaluating apparatus of hyperchannel photodissociation catalyst for preparing hydrogen performance as claimed in claim 1 is characterized in that described Pd/WO
3The film glass plate holder and makes the outlet and the Pd/WO of each pipeline in the organic glass clip
3The sealing of film glass plate.
7. the quick evaluating apparatus of hyperchannel photodissociation catalyst for preparing hydrogen performance as claimed in claim 6 is characterized in that the upper plate of described organic glass clip has ladder type body groove, places to be used for Pd/WO in groove
3The film glass plate heats the heating plate of temperature control.
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| CNB2004100261027A CN1307416C (en) | 2004-05-10 | 2004-05-10 | Multichannel rapid evaluating device for photolysis hydrogen making catalyst performance |
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|---|---|---|---|
| CNB2004100261027A CN1307416C (en) | 2004-05-10 | 2004-05-10 | Multichannel rapid evaluating device for photolysis hydrogen making catalyst performance |
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| CN1307416C true CN1307416C (en) | 2007-03-28 |
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| CN104815597B (en) * | 2015-05-10 | 2016-11-09 | 福建师范大学泉港石化研究院 | Small-sized integrated photolysis water hydrogen reaction unit |
| CN105353070A (en) * | 2015-09-29 | 2016-02-24 | 北京泊菲莱科技有限公司 | Parallel irradiation reaction device |
| CN105277651A (en) * | 2015-10-30 | 2016-01-27 | 甘林 | Photocatalytic performance measuring device and photocatalytic performance measuring method |
| CN109374732B (en) * | 2018-08-14 | 2022-01-04 | 杭州超钜科技有限公司 | Portable rapid hydrogen measuring device for fault escape gas and monitoring method thereof |
| CN111929371B (en) * | 2020-06-22 | 2022-02-11 | 西安交通大学 | Visual continuous on-line measuring photoelectrocatalysis reaction unit |
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