CN208239380U - A kind of photochemical catalyzing activity rating device - Google Patents

A kind of photochemical catalyzing activity rating device Download PDF

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Publication number
CN208239380U
CN208239380U CN201820881756.5U CN201820881756U CN208239380U CN 208239380 U CN208239380 U CN 208239380U CN 201820881756 U CN201820881756 U CN 201820881756U CN 208239380 U CN208239380 U CN 208239380U
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tube
grass
reactor body
shaped glass
air inlet
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CN201820881756.5U
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Chinese (zh)
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陈涛
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Dalian Ocean University
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Dalian Ocean University
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Abstract

The utility model discloses a kind of photochemical catalyzing activity rating devices, including magnetic agitation thermostatical circulating water bath cabinet, built-in optical catalytic reactor, U-shaped glass tube, the first grass tube, the second grass tube, unidirectional blow valve and glass three-way piston, the second grass tube is connected with U-shaped glass tube;Built-in optical catalytic reactor includes reactor body and Leng Jing;The inside of cold well is equipped with light source, and light source is one of mercury lamp or xenon lamp, and the upper end of cold well side wall is equipped with inlet and outlet, and inlet and outlet pass through hose and are connected with magnetic agitation thermostatical circulating water bath cabinet;The upper end of reactor body side wall is equipped with air inlet and air outlet, and gas outlet one end is connected with the first grass tube;The free end of U-shaped glass tube is connected with liquid storage ball;Second grass tube is equipped with spark discharger and branch pipe, and branch pipe is equipped with rubber sheet gasketing.The utility model is cheap, easy to operate, easy to use, small in size, good to the effect of catalyst activity evaluation.

Description

A kind of photochemical catalyzing activity rating device
Technical field
The utility model belongs to photocatalyst activity evaluating apparatus technical field, is related to a kind of photochemical catalyzing activity and comments Valence device.
Background technique
In recent years, the research of photocatalytic hydrogen production by water decomposition is increasingly paid attention to by people.In the research in the field, evaluation The activity of catalyst photochemical catalyzing is an important job.The dress for the evaluation photocatalyst activity that laboratory uses at present It sets and is made of mostly photo catalysis reactor, vacuum system and online gas-chromatography.Reactor is connected with vacuum systems in the device, The H generated in photochemical catalyzing reaction process2And O2Vacuum systems are initially entered, are sampled later by vacuum sampler laggard Enter on-line gas chromatography to carry out quantitative analysis, finally obtains H in the unit time2And O2Production quantity, i.e. catalyst sample Photocatalytic activity.The advantages of this device is can be more accurate and sensitively to the product H of photochemical catalyzing2And O2It carries out Quantitative analysis.Its disadvantage mainly has: package unit volume is big, occupies biggish laboratory area;Price, only vacuum system portion The price divided is general just at 100,000 yuan or so;The front end of the mechanical pump vacuumized is equipped with cold well, and when work needs liquid nitrogen frozen, to prevent Sealing steam enters mechanical pump and damages to it, and the consumption of liquid nitrogen increases testing cost.For these reasons, it is domestic very Have to the work for postponing this respect because condition is limited in the laboratories for wishing to carry out photocatalytic hydrogen production by water decomposition research more.
Based on current status and actual needs, in conjunction with our some experiences obtained in experimental work, it is proposed that The photochemical catalyzing activity rating device of a kind of simple possible, the basic principle is that utilizing H2And O2It is insoluble in the property of water Matter directly collects the H generated in photochemical catalyzing reaction with drainage2And O2And its total volume is measured, later by perfect gas State equation calculates H2And O2The amount of total substance.
Utility model content
The purpose of the utility model is to provide a kind of photochemical catalyzing activity rating devices, to solve above-mentioned background technique Proposed in the problem of.
The utility model is the technical scheme adopted is that a kind of photochemical catalyzing activity rating device, including magnetic force stir Mix thermostatical circulating water bath cabinet, the built-in optical catalytic reactor in magnetic agitation thermostatical circulating water bath cabinet, for gas body Product test with graduated U-shaped glass tube, the first grass tube, the second grass tube, unidirectional blow valve and be separately connected the One grass tube, the second grass tube, unidirectional blow valve one end glass three-way piston, the first grass tube urges with built-in optical Change reactor to be connected, the second grass tube being connected with what is tested for gas volume with graduated U-shaped glass tube;
Built-in optical catalytic reactor includes the reactor body of simple glass material and inside reactor body The cold well of quartz material, reactor body and cold well are closely sealed by ground;
The inside of cold well is equipped with light source, and light source is one of mercury lamp or xenon lamp, and the upper end of cold well side wall is equipped with water inlet And water outlet, inlet and outlet pass through hose and are connected with magnetic agitation thermostatical circulating water bath cabinet;
The upper end of reactor body side wall is equipped with air inlet and air outlet, and the inside of reactor body is equipped with air inlet pipe, into One end of tracheae is connected with air inlet, and the other end of air inlet pipe is 2mm away from the distance of reactor body bottom, and gas outlet one end connects It is connected to the first grass tube;
The free end of U-shaped glass tube is connected with liquid storage ball;
Second grass tube is equipped with spark discharger and branch pipe, and spark discharger is connected to power supply by conducting wire, branch pipe It is equipped with rubber sheet gasketing.
Wherein cold well includes inner and outer tubes, and light source is equipped in inner tube, is equipped with water inlet pipe, water inlet pipe and water inlet in outer tube It is connected.
Wherein air inlet one end is equipped with connecting tube, and connecting tube is connected with gas bomb, and connecting tube is equipped with shut-off valve.
Wherein U-shaped glass tube is provided with distilled water.
The beneficial effects of the utility model are: it is cheap, it is easy to operate, it is easy to use, it is small in size, to catalyst activity The effect of evaluation is good;Reactor body air inlet and air outlet are each provided to the upper end of reactor body side wall, it on the one hand can be with So that reaction solution when reaction is almost full with entire reactor body to reduce the dead volume of device, is on the other hand conducive to generate gas Discharge;Glass three-way piston and unidirectional blow valve use the various operations for making gas circuit and control very convenient;Spark discharge The design of device can be used to very easily judge H in product2And O2Close to the degree of metering ratio;The design of rubber sheet gasketing can To be very easily sampled to gaseous product;Detachable U-shaped glass tube design, in favor of selecting different volumes in an experiment The U-shaped glass tube of size and accuracy of reading;The magnetic agitation thermostatical circulating water bath cabinet of high-power high-accuracy (± 0.5 DEG C) is configured, Entire reaction unit is put into magnetic agitation constant water bath box in reaction, while being with magnetic agitation constant water bath box recirculated water Cold well provides cooling water, it is ensured that reaction system constant temperature.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of photochemical catalyzing activity rating device of the utility model.
Description of symbols:
1. magnetic agitation thermostatical circulating water bath cabinet, 2. built-in optical catalytic reactors, 3.U type glass tube, 4. first glass Conduit, 5. second grass tubes, 6. unidirectional blow valves, 7. glass three-way pistons, 8. reactor bodies, 9. cold wells, 10. light sources, 11. water inlet, 12. water outlets, 13. air inlets, 14. gas outlets, 15. air inlet pipe, 16. liquid storage balls, 17. spark discharger, 18. Branch pipe, 19. rubber sheet gasketings, 20. inner tubes, 21. outer tubes, 22. water inlet pipes, 23. connecting tubes, 24. shut-off valves.
Specific embodiment
With reference to the accompanying drawing, a specific embodiment of the utility model is described in detail, it is to be understood that this The protection scope of utility model is not limited by the specific implementation.
A kind of photochemical catalyzing activity rating device, as shown in Figure 1, including magnetic agitation thermostatical circulating water bath cabinet 1, position Built-in optical catalytic reactor 2 in magnetic agitation thermostatical circulating water bath cabinet 1, for gas volume test with graduated U-shaped glass tube 3, the first grass tube 4, the second grass tube 5, unidirectional blow valve 6 and it is separately connected the first grass tube 4, Two grass tubes 5,6 one end of unidirectional blow valve glass three-way piston 7, the first grass tube 4 and built-in optical catalytic reactor 2 It is connected, the second grass tube 5 being connected with what is tested for gas volume with graduated U-shaped glass tube 3;Built-in optical catalysis is anti- Answering device 2 includes the reactor body 8 of simple glass material and the cold well 9 of the quartz material inside reactor body 8, reaction Device main body 8 and cold well 9 are closely sealed by ground;The inside of cold well 9 be equipped with light source 10, light source 10 be one of mercury lamp or xenon lamp, The upper end of cold 9 side wall of well is equipped with water inlet 11 and water outlet 12, and water inlet 11 and water outlet 12 pass through hose and magnetic agitation Thermostatical circulating water bath cabinet 1 is connected;The upper end of 8 side wall of reactor body is equipped with air inlet 13 and gas outlet 14, reactor body 8 Inside is equipped with air inlet pipe 15, and one end of air inlet pipe 15 is connected with air inlet 13, and the other end of air inlet pipe 15 is away from 8 bottom of reactor body The distance in portion is 2mm, and 14 one end of gas outlet is connected with the first grass tube 4;The free end of U-shaped glass tube 3 is connected with liquid storage ball 16;Second grass tube 5 is equipped with spark discharger 17 and branch pipe 18, and spark discharger 17 is connected to power supply by conducting wire, props up Pipe 18 is equipped with rubber sheet gasketing 19.
Spark discharger 17 can make by oneself, including the sheet metal that two panels is in close proximity and is placed in parallel, the one of every sheet metal End is equipped with metal bar, and the free end of each metal bar is equipped with conducting wire, and the other end of conducting wire is equipped with attaching plug.It will when work In the common socket with switch control of plug insertion, socket switch is pressed when needing to discharge and is unclamped rapidly, or is adopted With a kind of switch pressing rear transient switching and just disconnecting automatically.Electric spark will be generated when energization between two metal sheets, thus point Fire H2And O2.Spark discharger 17 and the connection relationship of the second grass tube 5 are to bore in the horizontal direction of the second grass tube 5 Two apertures, sheet metal are put into inside the second grass tube 5, and metal bar passes through aperture and is exposed at outside the second grass tube 5 and and leads Line is connected, and will be sealed at aperture with common 704 glue of commercialization.
8 air inlet 13 of reactor body and gas outlet 14 are each provided to the upper end of 8 side wall of reactor body, it on the one hand can be with So that reaction solution when reaction is almost full with entire reactor body 8 to reduce the dead volume of device, is on the other hand conducive to generate gas Discharge.N is used before reaction2Sufficiently purging reaction solution, to exclude dissolved oxygen and be further reduced H2And O2In reaction solution Dissolution.Glass three-way piston 7 and unidirectional blow valve 6 use the various operations for making gas circuit and control very convenient.Spark is put The design of electric appliance 17 can be used to very easily judge H in product2And O2Close to the degree of metering ratio.Rubber sheet gasketing 19 Design can very easily be sampled gaseous product.Sealing between spark discharger 17 and the second grass tube 5 and Sealing between rubber sheet gasketing 19 and branch pipe 18 is completed with common 704 glue bond of commercialization, through practice examining, the party Method is simple, reliable, practical.Detachable U-shaped glass tube 3 designs, in favor of selecting different volumes size and reading in an experiment The U-shaped glass tube 3 of precision.The magnetic agitation thermostatical circulating water bath cabinet 1 of high-power high-accuracy (± 0.5 DEG C) is configured, it will in reaction Entire reaction unit is put into magnetic agitation constant water bath box 1, while being that cold well mentions with 1 recirculated water of magnetic agitation constant water bath box Cooling Water, to guarantee reaction system constant temperature.
Wherein cold well 9 includes inner tube 20 and outer tube 21, and light source 10 is equipped in inner tube 20, is equipped with water inlet pipe 22 in outer tube 21, Water inlet pipe 22 is connected with water inlet 11.
Wherein 13 one end of air inlet is equipped with connecting tube 23, and connecting tube 23 is connected with gas bomb, and connecting tube 23, which is equipped with, cuts Only valve 24.
Wherein U-shaped glass tube 3 is provided with distilled water.
Lead to cooling water to cold well 9 when work to prevent the temperature of mercury lamp or xenon lamp excessively high.
When test sample photocatalytic activity, by the catalyst ultrasonic disperse of certain mass in distilled water, by reaction solution It is placed in reactor body 8, reaction solution is made to be almost full with entire reactor body 8, small magneton is put into reactor body 8, It is passed through N into reaction solution under the conditions of magnetic agitation later2(logical N2Purpose be a small amount of oxygen that will be dissolved in reaction solution It drives away, and is further reduced H2And O2Solubility in reaction solution), glass three-way piston 7 is adjusted, is made from reactor body 8 N out2A part is vented by unidirectional blow valve 6, and another part purges U-shaped glass tube 3, is passed through N2After more than half an hour, to Distilled water is added in U-shaped glass tube 3 and adjusts its liquid level to zero point (at 0.00mL scale), it is logical to stop to close shut-off valve 24 N2, and rotary glass stop,threeway 7 makes the outlet gas circuit of reactor body 8 only be connected with U-shaped glass tube 3 without being vented with unidirectional Valve 6 is connected, and lights mercury lamp or xenon lamp to start light-catalyzed reaction, while the zero point that records the time.It is entire built-in in reaction process Photo catalysis reactor 2 is placed in the magnetic agitation thermostatical circulating water bath cabinet 1 that can accurately control temperature that (the magnetic agitation constant temperature follows Ring water bath 1 provides recirculated cooling water to cold well 9 simultaneously), since the volume of gas changes with temperature, to reaction in the experiment Accurately controlling for system temperature is particularly important, and reaction starts liquid level in rear every primary U-shaped glass tube 3 of record at regular intervals Reading obtains generating H2And O2Total volume VH2+O2, room temperature T and atmospheric pressure P when record is tested.Finally, calculating according to the following formula The H of generation2And O2The amount n of total substanceH2+O2:
P is atmospheric pressure in formula, and T be room temperature when testing, and R is gas constant, the saturated vapor of P* is temperature when being T water Pressure, ρ are the density of water, and g is gravity acceleration constant, and h is U-shaped glass tube or so when reading the reading of liquid level in U-shaped glass tube The difference in height of both ends liquid level.
The H generated due to water decomposition2And O2Metering compare for 2:1, so the H generated2And O2The amount of substance be respectively as follows:
The spark discharger 17 that the dress centers is mainly used for examining the H in product2And O2Whether the relationship of 2:1 is met. Concrete operations be after the end of the experiment rotary glass stop,threeway 7 with by the confined gas in U-shaped glass tube 3 in pipe, then Powering on makes 17 spark discharge of spark discharger, lights the H in pipe2And O2, etc. after systems are restored to room temperature, U-shaped glass tube 3 In liquid level return to zero point and then illustrate H in product2And O2The ratio of amount of substance be 2:1, otherwise then have certain gas excessive. H in product in most cases2And O2For 2:1, it is not 2:1 under a few cases, it is more illustrates that catalyst surface is adsorbed with Related intermediate species.It may determine that the H in product using the device2And O2Deviate the degree of metering ratio, but which kind of gas can not be known Body is excessive.The device is equipped with rubber sheet gasketing 19, and micro syringe can be used when needing and go forward side by side to gaseous product sampling Row chromatography or mass spectral analysis, to determine which kind of gas is excessive.U-shaped glass tube 3 is detachable in device, in this way can root in an experiment Different activities size according to sample be the gaseous product generated number and select the U-shaped glass tube 3 of different volumes size.Experiment Middle discovery, the device can be used to measure photochemical catalyzing hydrogen-producing speed greater than 50 μm of ol/h sample activity, but for There are also certain difficulties for the test of the very low sample of activity.
In conclusion a kind of photochemical catalyzing activity rating device provided by the embodiment of the utility model is by reactor master 8 air inlet 13 of body and gas outlet 14 are each provided at the upper end of 8 side wall of reactor body, on the one hand can make reaction when reaction solution almost The dead volume of device is reduced full of entire reactor body 8, is on the other hand conducive to generate the discharge of gas;N is used before reaction2It fills Divide purging reaction solution, to exclude dissolved oxygen and be further reduced H2And O2Dissolution in reaction solution;Glass three-way piston 7 Make the various operations of gas circuit and control very convenient with using for unidirectional blow valve 6;The design of spark discharger 17 can be used Very easily to judge H in product2And O2Close to the degree of metering ratio;The design of rubber sheet gasketing 19 can be very easily right Gaseous product is sampled;Sealing and rubber sheet gasketing 19 and branch between spark discharger 17 and the second grass tube 5 Sealing between pipe 18 is completed with common 704 glue bond of commercialization, and through practice examining, this method is simple, reliable, practical; Detachable U-shaped glass tube 3 designs, in favor of selecting the U-shaped glass tube 3 of different volumes size and accuracy of reading in an experiment; The magnetic agitation thermostatical circulating water bath cabinet 1 for configuring high-power high-accuracy (± 0.5 DEG C), by built-in optical catalytic reactor in reaction 2 are put into magnetic agitation constant water bath box 1, while being that cold well 9 provides cooling water with 1 recirculated water of magnetic agitation constant water bath box, To guarantee reaction system constant temperature.
Disclosed above is only specific embodiment of the utility model, and still, the utility model embodiment is not limited to This, the changes that any person skilled in the art can think of should all fall into the protection scope of the utility model.

Claims (4)

1. a kind of photochemical catalyzing activity rating device, which is characterized in that including magnetic agitation thermostatical circulating water bath cabinet (1), Built-in optical catalytic reactor (2) in the magnetic agitation thermostatical circulating water bath cabinet (1), for gas volume test Connect with graduated U-shaped glass tube (3), the first grass tube (4), the second grass tube (5), unidirectional blow valve (6) and respectively Connect first grass tube (4), the second grass tube (5), unidirectional blow valve (6) one end glass three-way piston (7), it is described First grass tube (4) is connected with built-in optical catalytic reactor (2), second grass tube (5) be used for gas volume Test is connected with graduated U-shaped glass tube (3);
The built-in optical catalytic reactor (2) include simple glass material reactor body (8) and be located at reactor body (8) the cold well (9) of internal quartz material, the reactor body (8) and cold well (9) are closely sealed by ground;
The inside of the cold well (9) is equipped with light source (10), and the light source (10) is one of mercury lamp or xenon lamp, the cold well (9) upper end of side wall is equipped with water inlet (11) and water outlet (12), and the water inlet (11) and water outlet (12) pass through hose It is connected with the magnetic agitation thermostatical circulating water bath cabinet (1);
The upper end of reactor body (8) side wall is equipped with air inlet (13) and gas outlet (14), the reactor body (8) Inside is equipped with air inlet pipe (15), and one end of the air inlet pipe (15) is connected with air inlet (13), the air inlet pipe (15) it is another Distance of the end away from reactor body (8) bottom is 2mm, and described gas outlet (14) one end is connected with the first grass tube (4);
The free end of the U-shaped glass tube (3) is connected with liquid storage ball (16);
Second grass tube (5) is equipped with spark discharger (17) and branch pipe (18), and the spark discharger (17) passes through Conducting wire connects to power supply, and the branch pipe (18) is equipped with rubber sheet gasketing (19).
2. a kind of photochemical catalyzing activity rating device as described in claim 1, which is characterized in that cold well (9) packet Inner tube (20) and outer tube (21) are included, light source (10) is equipped in said inner tube (20), is equipped with water inlet pipe (22) in the outer tube (21), The water inlet pipe (22) is connected with water inlet (11).
3. a kind of photochemical catalyzing activity rating device as described in claim 1, which is characterized in that the air inlet (13) One end is equipped with connecting tube (23), and the connecting tube (23) is connected with gas bomb, and the connecting tube (23) is equipped with shut-off valve (24)。
4. a kind of photochemical catalyzing activity rating device as described in claim 1, which is characterized in that the U-shaped glass tube (3) it is provided with distilled water.
CN201820881756.5U 2018-06-08 2018-06-08 A kind of photochemical catalyzing activity rating device Expired - Fee Related CN208239380U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108445143A (en) * 2018-06-08 2018-08-24 大连海洋大学 A kind of photochemical catalyzing activity rating device
CN109632611A (en) * 2019-01-14 2019-04-16 浙江大学 A kind of particulate matter moisture absorption simulator

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108445143A (en) * 2018-06-08 2018-08-24 大连海洋大学 A kind of photochemical catalyzing activity rating device
CN108445143B (en) * 2018-06-08 2023-07-18 大连海洋大学 Photocatalytic water splitting activity evaluation device
CN109632611A (en) * 2019-01-14 2019-04-16 浙江大学 A kind of particulate matter moisture absorption simulator

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Inventor after: Chen Tao

Inventor after: Ma Rui

Inventor after: Huang Qianyi

Inventor after: Zhang Xiaotong

Inventor after: Li Jiayin

Inventor after: Qin Huaying

Inventor before: Chen Tao

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Granted publication date: 20181214

Termination date: 20190608

CF01 Termination of patent right due to non-payment of annual fee