CN101900710B - Multi-channel reaction simple device for evaluating hydrogen production performance of photocatalyst and method adopting same for carrying out hydrogen production performance evaluation - Google Patents
Multi-channel reaction simple device for evaluating hydrogen production performance of photocatalyst and method adopting same for carrying out hydrogen production performance evaluation Download PDFInfo
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Abstract
The invention relates to a multi-channel reaction simple device for evaluating the hydrogen production performance of a photocatalyst and a method adopting the same for carrying out hydrogen production performance evaluation. The multi-channel reaction simple device can solve the problems of complicated structure, time-consuming assembly, high cost and difficult implementation of the existing multi-channel reaction device for evaluating the hydrogen production performance of the photocatalyst. The device consists of a light source and 4-8 reaction systems which are uniformly distributed around the light source, and each reaction system consists of a reactor, a gas storage device, a gas circuit circulation device, a valve, a closed circulation loop consisting of rubber hoses for connecting the parts and a magnetic stirrer. The evaluation method comprises the following steps: well assembling the reaction systems, starting the light source, starting the gas circuit circulation systems, and then periodically taking gas for testing. The device is simple, has simple assembly, strong maneuverability, low cost of parts and small occupied space and can save space. The adoption of the device for carrying out the photocatalysis hydrogen production performance evaluation can lead the testing result to be creditable and lead experimental data in the same group to have strong comparability.
Description
Technical field
The present invention relates to a kind of device and evaluation method of evaluating hydrogen production performance of photocatalyst.
Background technology
In the photocatalysis hydrogen production field, relate to a certain definite catalyzer is carried out various quantitative scientific researches, wish to search out the optimal conditions of catalyzer or find the scientific law that it is inherent, people are to the screening of multiple catalysts or a certain definite catalyzer is carried out quantitative scientific research carry out in a reactor traditionally, although it is effective to pass logical photocatalyst reactor, also there is following problem:
1, efficient is low, because a reactor can only carry out activity rating in a kind of reaction system to a kind of catalyzer, can be a time-consuming job to multiple catalysts or a certain catalyzer at the activity rating of differential responses system therefore.
2, reappearance is relatively poor, when subtle change occurs owing to reaction conditions changes in especially a certain catalytic activity, the temperature that multi-pass operations brings, stirring rate, the impact of the disturbance factors such as light, no matter day by day urgent along with energy problem, photocatalysis hydrogen production field are that the Large-scale Screening of multiple catalysts or the basic scientific research of single catalyzer are in the urgent need to the high reproducible evaluating apparatus of a kind of high-level efficiency.
China applies for a patent the device that " a kind of multi-channel reaction device of photocatalysis hydrogen production performance Fast Evaluation " (application number is 200710099875.1) reported a kind of multichannel light catalyst screening, this device has adopted the design of electrographite brush in the at the uniform velocity rotation of tubular type light source, effectively avoided when rotated power supply cabling of light source.And the rotation of light source and the rotation of magnetic stirring apparatus can be controlled by speed regulator, and gas detecting system as sampling pipe, is realized the online detection of chromatogram by the stainless-steel tube of six-way valve or four-way valve control or glass tube.But this device is too loaded down with trivial details, require the reactor opening portion closely to be connected (because the volume in the reactor is limited, if γ-ray emission is more, can back down lid) with Photoreactor, the device that need to vacuumize will realize that preparation requires high to reactor to the online detection of gas.That is to say that material cost and the processing cost of installing in this are higher.
Summary of the invention
The objective of the invention is in order to solve the multi-channel reaction device complex structure of existing photocatalysis hydrogen production performance evaluation, assemble time-consumingly, cost is high and be difficult for the problem of realization.The invention provides a kind of multi-channel reaction simple device and evaluation method thereof of evaluating hydrogen production performance of photocatalyst.
The multi-channel reaction simple device of evaluating hydrogen production performance of photocatalyst of the present invention, formed by light source and 4～8 reactive systems being evenly distributed on around the light source, wherein reactive system is comprised of two parts, the first is by quartz reactor, accumulator unit, gas circuit circulating device, the first valve, second valve, the 3rd valve, seal rubber plug, the first escape pipe, the first draft tube, the second escape pipe, the second draft tube and be connected the sealing and circulating loop that the first sebific duct, the second sebific duct and the 3rd sebific duct of above each parts form, and it two is magnetic stirring apparatuss; Wherein, quartz reactor is over against light source, and the distance of quartz reactor and light source is 10～20cm, and sealing is fixed with the second escape pipe and the second draft tube on the accumulator unit; Quartz reactor is sealed by seal rubber plug, the first escape pipe and the sealing of the first draft tube are fixed on seal rubber plug inside, the port of the first draft tube is positioned at the 5～10mm place, bottom apart from quartz reactor, the first escape pipe is communicated with the second draft tube by the 3rd sebific duct, the second escape pipe is communicated with by the second sebific duct with the inlet end of gas circuit circulating device, and the outlet side of gas circuit circulating device is communicated with the first draft tube by the first sebific duct; The first valve is arranged on the first sebific duct, and second valve is arranged on the second sebific duct, and the 3rd valve is arranged on the 3rd sebific duct, and quartz reactor places on the magnetic stirring apparatus; Described gas circuit circulating device is syringe or the electronic air extracting pump that is communicated with the glass three-way fixing seal, and wherein, syringe is communicated with the second sebific duct and the first sebific duct respectively by two ports of glass three-way.
Described light source is uviol lamp or xenon lamp; Wherein the power of uviol lamp is 125～250W, and the power of xenon lamp is 250～500W.Described quartz reactor can be used for carrying out the pulverulence hydrogen manufacturing performance of photocatalyst, also can be used for being fixed photocatalysis agent hydrogen manufacturing performance.When being used for the immobilization evaluating hydrogen production performance of photocatalyst, as long as in quartz reactor, place a fixedly specimen holder of immobilization photocatalyst.
Described accumulator unit is that the container of volume more than 500mL gets final product, when playing the effect of storage of hydrogen, also play the effect of dilution hydrogen, when making each extraction detect gaseous sample, the intrasystem hydrogen total amount of gas flow relative response that extracts, very little, can not affect the concentration of hydrogen in the reactive system.The introducing of accumulator unit has solved the device of existing evaluating hydrogen production performance of photocatalyst because of narrow space in the reactor, the hydrogen that produces is gathered in the reactor, every extraction once for detection of gas, all can make the content of hydrogen produce very large variation, the a large amount of minimizing, thus the detection of ensuing hydrogen content affected, cause occurring the light-catalyzed reaction time longer, the phenomenon that the amounts of hydrogen that detects tails off on the contrary makes testing result inaccurate.The present invention utilizes the gas circuit circulating device gas that photocatalysis in the quartz reactor produces can be mixed in whole reactive system, can not affect testing result so that the gas detection is got in any position in reactive system, improve contrast property and the confidence level of testing result.
Described gas circuit circulating device is aspiration pump or syringe, and the effect of gas circuit circulating device is the density of hydrogen uniformity that makes in the reactive system everywhere; The air capacity of control electronic air extracting pump is 300～600mL/min; Syringe is the syringe that is communicated with the glass three-way fixing seal, and wherein syringe is communicated with the first sebific duct and the sealing of the second sebific duct respectively by two other port of glass three-way, and the volume of syringe is 50～100mL.The present invention adopts and very easily to buy on the market, and cheap syringe and glass three-way be as the gas circuit circulating device, and its design is very ingenious, is a bright spot of the present invention.
The effect of described the first valve, second valve and the 3rd valve is to guarantee that density of hydrogen does not change when getting detection gas, guarantees that hydrogen content is corresponding consistent with the height of photocatalysis hydrogen production time in the detected gas.The first valve and second valve need be arranged on as much as possible near on the two-port position of gas circuit circulating device, avoid introducing too much air when the gas circuit circulating device is assembled to the reactive system that is full of nitrogen, affect the catalytic activity of photocatalyst.
The effect of described magnetic stirring apparatus is that the reaction system in the quartz reactor is stirred, and guarantees that Powdered photocatalyst evenly is suspended in the target solution, guarantees that photocatalyst fully absorbs light, plays better catalytic action.When photocatalyst is the immobilization photocatalyst, magnetic stirring apparatus can be removed.
The method that adopts the multi-channel reaction simple device of evaluating hydrogen production performance of photocatalyst of the present invention to carry out evaluating hydrogen production performance is: one, be placed in the quartz reactor with photocatalyst and by the target solution of catalytic reduction, and seal with sealing-plug, one end that then will be provided with the 3rd sebific duct of the 3rd valve is communicated with the sealing of the first escape pipe, the another port of the 3rd sebific duct is communicated with the second draft tube sealing of accumulator unit, one end that then will be provided with the second sebific duct of second valve is communicated with the second escape pipe sealing of accumulator unit, one end that will be provided with again the first sebific duct of the first valve is communicated with the sealing of the first draft tube, then keep the first valve, second valve and the 3rd valve are open mode, then the another port by the first sebific duct continues to pass into nitrogen 10～20min to the first sebific duct, then the first valve and second valve are closed, inlet end with the gas circuit circulating device is communicated with the another port sealing of the second sebific duct again, the outlet side of gas circuit circulating device is communicated with the another port sealing of the first sebific duct, assembling obtains reactive system, and described gas circuit circulating device is electronic air extracting pump; Two, assemble 4～8 reactive systems by the described operation steps of step 1, then 4～8 reactive systems that assemble evenly being distributed is placed on around the light source, and wherein quartz reactor is over against light source, and the distance of quartz reactor and light source is 10～20cm; Three, open light source, start gas circuit circulating device electronic air extracting pump, carry out the photocatalysis hydrogen production reaction, then regularly get the detection gaseous sample, carry out the gas chromatography spectrogram and detect; Wherein regularly getting the method that detects gaseous sample is every 0.5～1 hour, gets gaseous sample with the syringe of 5mL at the 3rd sebific duct at the second draft tube place of each accumulator unit and gets final product, and namely finishes the evaluation of hydrogen manufacturing performance of photocatalyst.
Above-mentioned employing electronic air extracting pump can also operate as follows as regularly getting the method that detects gaseous sample in the step 3 in the method for the evaluating hydrogen production performance of gas circuit circulating device: every 0.5～1 hour, gas circuit circulating device electronic air extracting pump is closed, then second valve and the 3rd valve of each reactive system are closed, then get gaseous sample at the 3rd sebific duct at the second draft tube place of each accumulator unit successively with the syringe of 5mL, after taking second valve and the 3rd valve are opened, restarted gas circuit circulating device electronic air extracting pump and get final product.
The method that the multi-channel reaction simple device of employing evaluating hydrogen production performance of photocatalyst carries out evaluating hydrogen production performance is: one, be placed in the quartz reactor with photocatalyst and by the target solution of catalytic reduction, and seal with sealing-plug, one end that then will be provided with the 3rd sebific duct of the 3rd valve is communicated with the sealing of the first escape pipe, the another port of the 3rd sebific duct is communicated with the second draft tube sealing of accumulator unit, one end that then will be provided with the second sebific duct of second valve is communicated with the second escape pipe sealing of accumulator unit, one end that will be provided with again the first sebific duct of the first valve is communicated with the sealing of the first draft tube, then keep the first valve, second valve and the 3rd valve are open mode, then the another port by the first sebific duct continues to pass into nitrogen 10～20min in the first sebific duct, then the first valve and second valve are closed, the two-port of gas circuit circulating device is communicated with the another port of the second sebific duct and the another port sealing of the first sebific duct respectively, assembling obtains reactive system, described gas circuit circulating device is the syringe that is communicated with the glass three-way fixing seal, wherein, syringe is communicated with the second sebific duct and the sealing of the first sebific duct respectively by two ports of glass three-way, and piston is positioned at the zero graduation place in the syringe; Two, assemble 4～8 reactive systems by the described operation steps of step 1, then 4～8 reactive systems that assemble evenly being distributed is placed on around the light source, and wherein quartz reactor is over against light source, and the distance of quartz reactor and light source is 10～20cm; Three, open light source, carry out the photocatalysis hydrogen production reaction, then regularly get the detection gaseous sample, carry out the gas chromatography spectrogram and detect; Wherein regularly getting the front 10～15min of test sample mixes the density of hydrogen in each reactive system, concrete operation method is: a, the first valve cuts out, gas circuit circulating device syringe is pulled to 50mL scale place by zero graduation, then the first valve is opened, again second valve is closed, syringe with the gas circuit circulating device is pushed into the zero graduation place again, finishes a circulation of a reactive system; B, successively remaining reactive system is finished a circulation according to the operation of above-mentioned steps a, finish a systemic circulation this moment, and then 4～8 systemic circulations are finished in repetitive operation, namely finishes mixing of density of hydrogen in the reactive system; Wherein regularly getting the method that detects gaseous sample is every 0.5～1 hour, gets gaseous sample with the syringe of 5mL at the 3rd sebific duct at the second draft tube place of each accumulator unit and gets final product, and namely finishes the evaluation of hydrogen manufacturing performance of photocatalyst.
The syringe that above-mentioned employing is communicated with the glass three-way fixing seal can also operate as follows as regularly getting the method that detects gaseous sample in the step 3 in the method for the evaluating hydrogen production performance of gas circuit circulating device: every 0.5～1 hour, second valve and the 3rd valve of each reactive system are closed, then get gaseous sample at the 3rd sebific duct at the second draft tube place of each accumulator unit successively with the syringe of 5mL, after taking second valve and the 3rd valve opened and get final product.
The multi-channel reaction simple device of evaluating hydrogen production performance of photocatalyst of the present invention is simple, and is easily assembled, workable, and do not need complicated parts, and each parts easily obtains, and is cheap, and production cost is low.Multi-channel reaction simple device of the present invention separates with hydrogen gas detector (gas chromatograph), takes up an area to lack, and is conducive to conserve space.
Adopt the multi-channel reaction simple device of evaluating hydrogen production performance of photocatalyst of the present invention to carry out the testing result of evaluating hydrogen production performance of photocatalyst credible, the comparability of experimental data is strong on the same group.
The present invention utilizes gas chromatograph to detect the concentration (c of the hydrogen in the sample that obtains
H2) be the concentration of hydrogen in the reactive system, then the hydrogen output (representing with L) in corresponding sampling time is: L=c
H2* V
Reaction System, V wherein
Reactive systemVolume for the reactive system confined space.In practical operation, owing in the reactive system, comparing with the volume of accumulator unit is long-pending, the volume of quartz reactor, gas circuit circulating device, the first sebific duct, the second sebific duct and the 3rd sebific duct can be ignored, so V
Reactive system≈ V
Accumulator unit
Description of drawings
Fig. 1 is the schematic diagram of the multi-channel reaction simple device of evaluating hydrogen production performance of photocatalyst of the present invention; Fig. 2 is the structure diagram of reactive system in the multi-channel reaction simple device of evaluating hydrogen production performance of photocatalyst of the present invention; Fig. 3 is the structure diagram of reactive system in the multi-channel reaction simple device of evaluating hydrogen production performance of photocatalyst of embodiment eight; Fig. 4 is the schematic diagram of multi-channel reaction simple device of the evaluating hydrogen production performance of photocatalyst of embodiment 17; Fig. 5 is the structure diagram of reactive system in the multi-channel reaction simple device of evaluating hydrogen production performance of photocatalyst of embodiment 17; Fig. 6 is nano-TiO in the embodiment 18
2Meta-hydrogen output concerns histogram during the light-catalyzed reaction of film photocatalyst; Fig. 7 is nano-TiO in the embodiment 18
2Hydrogen output graph of a relation during film photocatalyst light-catalyzed reaction 3h.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the combination in any between each embodiment.
Embodiment one: the multi-channel reaction simple device of the evaluating hydrogen production performance of photocatalyst of present embodiment is comprised of light source 1 and 4～8 reactive systems 2 being evenly distributed on around the light source 1, wherein reactive system 2 is comprised of two parts, the first is by quartz reactor 2-1, accumulator unit 2-2, gas circuit circulating device 2-3, the first valve 2-4, second valve 2-5, the 3rd valve 2-6, seal rubber plug 2-11, the first escape pipe 2-12, the first draft tube 2-13, the second escape pipe 2-14, the second draft tube 2-15 and the first sebific duct 2-7 that is connected above each parts, the sealing and circulating loop that the second sebific duct 2-8 and the 3rd sebific duct 2-9 form, it two is magnetic stirring apparatus 2-10; Wherein, quartz reactor 2-1 is over against light source 1, and the distance of quartz reactor 2-1 and light source 1 is 10～20cm, and the upper sealing of accumulator unit 2-2 is fixed with the second escape pipe 2-14 and the second draft tube 2-15; Quartz reactor 2-1 is sealed by seal rubber plug 2-11, it is inner that the first escape pipe 2-12 and the first draft tube 2-13 sealing are fixed on seal rubber plug 2-11, the port of the first draft tube 2-13 is positioned at the 5～10mm place, bottom apart from quartz reactor 2-1, the first escape pipe 2-12 is communicated with the second draft tube 2-15 by the 3rd sebific duct 2-9, the second escape pipe 2-14 is communicated with by the second sebific duct 2-8 with the inlet end of gas circuit circulating device 2-3, and the outlet side of gas circuit circulating device 2-3 is communicated with the first draft tube 2-13 by the first sebific duct 2-7; The first valve 2-4 is arranged on the first sebific duct 2-7, and second valve 2-5 is arranged on the second sebific duct 2-8, and the 3rd valve 2-6 is arranged on the 3rd sebific duct 2-9, and reactor 2-1 places on the magnetic stirring apparatus 2-10; Described gas circuit circulating device 2-3 is syringe or the electronic air extracting pump that is communicated with the glass three-way fixing seal, and wherein, syringe is communicated with the second sebific duct 2-8 and the first sebific duct 2-7 respectively by two ports of glass three-way.
The rough schematic of the multi-channel reaction simple device of present embodiment as shown in Figure 1.Reactive system 2 be evenly distributed on light source 1 around, according to concrete test needs, can evenly place 4～8 reactive systems 2.The structure diagram of the reactive system 2 of present embodiment as shown in Figure 2.
The multi-channel reaction simple device of present embodiment is simple, and is easily assembled, and do not need complicated parts, and each parts easily obtains, and is cheap, and production cost is low.The multi-channel reaction simple device volume is little simultaneously, takes up an area to lack, and is conducive to conserve space.
Embodiment two: what present embodiment and embodiment one were different is that light source 1 is uviol lamp or xenon lamp; Wherein the power of uviol lamp is 125～250W, and the power of xenon lamp is 250～500W.Other parameter is identical with embodiment one.
Embodiment three: what present embodiment was different from embodiment one or two is that accumulator unit 2-2 is the container of volume more than 500mL.Other parameter is identical with embodiment one or two.
Embodiment four: what present embodiment was different from embodiment one or two is that accumulator unit 2-2 is that volume is at the there-necked flask of 1L.Other parameter is identical with embodiment one or two.
Embodiment five: present embodiment is different from one of embodiment one to four is that the distance of quartz reactor 2-1 and light source 1 is 15cm.Other parameter is identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five is that the port of the first draft tube 2-13 is positioned at the 8mm place, bottom apart from quartz reactor 2-1.Other parameter is identical with one of embodiment one to five.
Embodiment seven: what present embodiment was different from one of embodiment one to six is that gas circuit circulating device 2-3 is electronic air extracting pump, and the air capacity of control electronic air extracting pump is 300～600mL/min.Other parameter is identical with one of embodiment one to six.
Embodiment eight: what present embodiment was different from one of embodiment one to six is the syringe of gas circuit circulating device 2-3 for being communicated with the glass three-way fixing seal, and wherein the volume of syringe is 50～100mL.Other parameter is identical with one of embodiment one to six.
Syringe and the fixing seal mode of communicating of glass three-way are that dispensing end with syringe is communicated with wherein arbitrary port fixing seal of glass three-way and gets final product in the present embodiment, the fixing seal mode can be by adhesive bonds together, also can mechanical fixing seal, as long as realize fixing seal.
The multi-channel reaction simple device of the evaluating hydrogen production performance of photocatalyst of present embodiment as shown in Figure 3, the piston of syringe 2-3 is placed on zero graduation line place.Syringe more is simple and easy in the multi-channel reaction simple device of present embodiment, and cheap, cost is low, has avoided because of the cost issues of electronic air extracting pump because regularly replacing serviceable life, and is more practical, consume energy low.And can play the gas circuit ringing the same with electronic air extracting pump.
Present embodiment adopts and very easily to buy on the market, and cheap syringe and glass three-way be as the gas circuit circulating device, and its design is very ingenious, is a bright spot of the present invention.
Embodiment nine: present embodiment adopts the evaluation method of the multi-channel reaction simple device of embodiment one described evaluating hydrogen production performance of photocatalyst, realize by following steps: one, be placed among the quartz reactor 2-1 with photocatalyst and by the target solution of catalytic reduction, and seal with sealing-plug 2-11, one end that then will be provided with the 3rd sebific duct 2-9 of the 3rd valve 2-6 is communicated with the first escape pipe 2-12 sealing, the another port of the 3rd sebific duct 2-9 is communicated with the second draft tube 2-15 sealing of accumulator unit 2-2, one end that then will be provided with the second sebific duct 2-8 of second valve 2-5 is communicated with the second escape pipe 2-14 sealing of accumulator unit 2-2, one end that will be provided with again the first sebific duct 2-7 of the first valve 2-4 is communicated with the first draft tube 2-13 sealing, then keep the first valve 2-4, second valve 2-5 and the 3rd valve 2-6 are open mode, then the another port by the first sebific duct 2-7 continues to pass into nitrogen 10～20min to the first sebific duct 2-7, then the first valve 2-4 and second valve 2-5 are closed, inlet end with gas circuit circulating device 2-3 is communicated with the another port sealing of the second sebific duct 2-8 again, the outlet side of gas circuit circulating device 2-3 is communicated with the another port sealing of the first sebific duct 2-7, assembling obtains reactive system 2, and described gas circuit circulating device 2-3 is electronic air extracting pump; Two, assemble 4～8 reactive systems 2 by the described operation steps of step 1, then 4～8 reactive systems that assemble 2 are evenly distributed and be placed on around the light source 1, wherein quartz reactor 2-1 is over against light source 1, and the distance of quartz reactor 2-1 and light source 1 is 10～20cm; Three, open light source 1, start gas circuit circulating device electronic air extracting pump 2-3, carry out the photocatalysis hydrogen production reaction, then regularly get the detection gaseous sample, carry out the gas chromatography spectrogram and detect; Wherein regularly getting the method that detects gaseous sample is every 0.5～1 hour, gets gaseous sample with the 3rd sebific duct 2-9 of syringe at the second draft tube 2-15 place of each accumulator unit 2-2 of 5mL and gets final product, and namely finishes the evaluation of hydrogen manufacturing performance of photocatalyst.
Embodiment ten: what present embodiment and embodiment nine were different was regularly to get the method that detects gaseous sample in the step 3 can also operate as follows: every 0.5～1 hour, gas circuit circulating device electronic air extracting pump 2-3 is closed, then second valve 2-5 and the 3rd valve 2-6 with each reactive system 2 closes, then get gaseous sample at the 3rd sebific duct 2-9 at the second draft tube 2-15 place of each accumulator unit 2-2 successively with the syringe of 5mL, after taking second valve 2-5 and the 3rd valve 2-6 are opened, restart gas circuit circulating device electronic air extracting pump 2-3 and get final product.Other step and parameter are identical with embodiment nine.
In the present embodiment get detect gaseous sample before, second valve 2-5 and the 3rd valve 2-6 with each reactive system 2 closes simultaneously, purpose is the corresponding consistance of height that guarantees hydrogen content and photocatalysis hydrogen production reaction time in the detected gas, prevents that the hydrogen that produced afterwards from entering accumulator unit.
Embodiment 11: present embodiment is different from embodiment nine or ten is that the air capacity of the gas circuit circulating device electronic air extracting pump 2-3 in the step 1 is 300～600mL/min.Other step and parameter are identical with embodiment nine or ten.
Embodiment 12: present embodiment adopts the evaluation method of the multi-channel reaction simple device of embodiment one described evaluating hydrogen production performance of photocatalyst, realize by following steps: one, be placed among the quartz reactor 2-1 with photocatalyst and by the target solution of catalytic reduction, and seal with sealing-plug 2-11, one end that then will be provided with the 3rd sebific duct 2-9 of the 3rd valve 2-6 is communicated with the first escape pipe 2-12 sealing, the another port of the 3rd sebific duct 2-9 is communicated with the second draft tube 2-15 sealing of accumulator unit 2-2, one end that then will be provided with the second sebific duct 2-8 of second valve 2-5 is communicated with the second escape pipe 2-14 sealing of accumulator unit 2-2, one end that will be provided with again the first sebific duct 2-7 of the first valve 2-4 is communicated with the first draft tube 2-13 sealing, then keep the first valve 2-4, second valve 2-5 and the 3rd valve 2-6 are open mode, then the another port by the first sebific duct 2-7 continues to pass into nitrogen 10～20min in the first sebific duct 2-7, then the first valve 2-4 and second valve 2-5 are closed, the two-port of gas circuit circulating device 2-3 is communicated with the another port of the second sebific duct 2-8 and the another port sealing of the first sebific duct 2-7 respectively, assembling obtains reactive system 2, described gas circuit circulating device 2-3 is the syringe that is communicated with the glass three-way fixing seal, wherein, syringe is communicated with the second sebific duct 2-8 and the first sebific duct 2-7 sealing respectively by two ports of glass three-way, and piston is positioned at the zero graduation place in the syringe; Two, assemble 4～8 reactive systems 2 by the described operation steps of step 1, then 4～8 reactive systems that assemble 2 are evenly distributed and be placed on around the light source 1, wherein quartz reactor 2-1 is over against light source 1, and the distance of quartz reactor 2-1 and light source 1 is 10～20cm; Three, open light source 1, carry out the photocatalysis hydrogen production reaction, then regularly get the detection gaseous sample, carry out the gas chromatography spectrogram and detect; Wherein regularly getting the front 10～15min of test sample mixes the density of hydrogen in each reactive system 2, concrete operation method is: a, the first valve 2-4 is closed, syringe 2-3 in the gas circuit circulating device is pulled to 50mL scale place by zero graduation, then the first valve 2-4 is opened, again second valve 2-5 is closed, again gas circuit circulating device syringe 2-3 is pushed into the zero graduation place, finishes a circulation of a reactive system 2; B, successively remaining reactive system 2 is finished a circulation according to the operation of above-mentioned steps a, finish a systemic circulation this moment, and then 4～8 systemic circulations are finished in repetitive operation, namely finishes mixing of density of hydrogen in the reactive system 2; Wherein regularly getting the method that detects gaseous sample is every 0.5～1 hour, gets gaseous sample with the 3rd sebific duct 2-9 of syringe at the second draft tube 2-15 place of each accumulator unit 2-2 of 5mL and gets final product, and namely finishes the evaluation of hydrogen manufacturing performance of photocatalyst.
Embodiment 13: what present embodiment and embodiment 12 were different was regularly to get the method that detects gaseous sample in the step 3 can also operate as follows: every 0.5～1 hour, second valve 2-5 and the 3rd valve 2-6 of each reactive system 2 are closed, then get gaseous sample at the 3rd sebific duct 2-9 at the second draft tube 2-15 place of each accumulator unit 2-2 successively with the syringe of 5mL, after taking second valve 2-5 and the 3rd valve 2-6 opened and get final product.Other step and parameter are identical with embodiment 12.
In the present embodiment get detect gaseous sample before, second valve 2-5 and the 3rd valve 2-6 with each reactive system 2 closes simultaneously, purpose is the corresponding consistance of height that guarantees hydrogen content and photocatalysis hydrogen production reaction time in the detected gas, prevents that the hydrogen that produced afterwards from entering accumulator unit.
Embodiment 14: present embodiment is different from embodiment 12 or 13 is that the volume of syringe is 50～100mL among the gas circuit circulating device 2-3 of the syringe that is communicated with the glass three-way fixing seal in the step 1.Other step and parameter are identical with embodiment 12 or 13.
Embodiment 15: what present embodiment was different from one of embodiment nine to 14 is to install 6 reactive systems 2 by the described operational group of step 1 in the step 2, and then 6 reactive systems that assemble 2 evenly being distributed is placed on around the light source 1.Other step and parameter are identical with one of embodiment nine to 14.
Embodiment 16: present embodiment is different from one of embodiment nine to 15 is that the distance of quartz reactor 2-1 and light source 1 is 15cm in the step 2.Other step and parameter are identical with one of embodiment nine to 15.
Embodiment 17: the multi-channel reaction simple device of the evaluating hydrogen production performance of photocatalyst of present embodiment is comprised of xenon source 1 and 6 reactive systems 2 being evenly distributed on around the xenon source 1, wherein reactive system 2 is comprised of two parts, the first is by quartz reactor 2-1, there-necked flask 2-2, gas circuit circulating device 2-3, the first valve 2-4, second valve 2-5, the 3rd valve 2-6, seal rubber plug 2-11, the first escape pipe 2-12, the first draft tube 2-13, the second escape pipe 2-14, the second draft tube 2-15 and the first sebific duct 2-7 that is connected above each parts, the sealing and circulating loop that the second sebific duct 2-8 and the 3rd sebific duct 2-9 form, it two is magnetic stirring apparatus 2-10; Wherein, quartz reactor 2-1 is over against xenon source 1, and the distance of quartz reactor 2-1 and xenon source 1 is 15cm, and the upper sealing of there-necked flask 2-2 is fixed with the second escape pipe 2-14 and the second draft tube 2-15; Quartz reactor 2-1 is sealed by seal rubber plug 2-11, it is inner that the first escape pipe 2-12 and the first draft tube 2-13 sealing are fixed on seal rubber plug 2-11, the port of the first draft tube 2-13 is positioned at the 8mm place, bottom apart from quartz reactor 2-1, the first escape pipe 2-12 is communicated with the second draft tube 2-15 by the 3rd sebific duct 2-9, the second escape pipe 2-14 is communicated with by the second sebific duct 2-8 with the inlet end of gas circuit circulating device 2-3, and the outlet side of gas circuit circulating device 2-3 is communicated with the first draft tube 2-13 by the first sebific duct 2-7; The first valve 2-4 is arranged on the first sebific duct 2-7, and second valve 2-5 is arranged on the second sebific duct 2-8, and the 3rd valve 2-6 is arranged on the 3rd sebific duct 2-9, and reactor 2-1 places on the magnetic stirring apparatus 2-10; Described gas circuit circulating device 2-3 is the syringe that is communicated with the glass three-way fixing seal, and syringe is communicated with the second sebific duct 2-8 and the first sebific duct 2-7 respectively by two ports of glass three-way; The volume of described there-necked flask 2-2 is 1L.
The schematic diagram of the multi-channel reaction simple device of the evaluating hydrogen production performance of photocatalyst of present embodiment has 6 reactive systems 2 as shown in Figure 4 among the figure, be labeled as respectively " I, II, III, IV, V and VI ".The structure diagram of the reactive system 2 of the multi-channel reaction simple device of the evaluating hydrogen production performance of photocatalyst of present embodiment as shown in Figure 5.Device is not before carrying out evaluating hydrogen production performance of photocatalyst in the present embodiment, and the piston of the syringe 2-3 of gas circuit circulating device is in the zero graduation place.
The syringe 2-3 of the gas circuit circulating device of present embodiment is that volume is the syringe of 50mL.
Embodiment 18: the method that present embodiment adopts the multi-channel reaction simple device of embodiment 17 described evaluating hydrogen production performance of photocatalyst to carry out evaluating hydrogen production performance is: one, with nano-TiO
2Film photocatalyst and be placed among the quartz reactor 2-1 by the target solution of catalytic reduction, and seal with sealing-plug 2-11, one end that then will be provided with the 3rd sebific duct 2-9 of the 3rd valve 2-6 is communicated with the first escape pipe 2-12 sealing, the another port of the 3rd sebific duct 2-9 is communicated with the second draft tube 2-15 sealing of accumulator unit 2-2, one end that then will be provided with the second sebific duct 2-8 of second valve 2-5 is communicated with the second escape pipe 2-14 sealing of accumulator unit 2-2, one end that will be provided with again the first sebific duct 2-7 of the first valve 2-4 is communicated with the first draft tube 2-13 sealing, then keep the first valve 2-4, second valve 2-5 and the 3rd valve 2-6 are open mode, then the another port by the first sebific duct 2-7 continues to pass into nitrogen 10～20min in the first sebific duct 2-7, then the first valve 2-4 and second valve 2-5 are closed, the two-port of gas circuit circulating device 2-3 is communicated with the another port of the second sebific duct 2-8 and the another port sealing of the first sebific duct 2-7 respectively, assembling obtains reactive system 2, described gas circuit circulating device 2-3 is the syringe that is communicated with the glass three-way fixing seal, wherein, syringe is communicated with the second sebific duct 2-8 and the first sebific duct 2-7 sealing respectively by two ports of glass three-way, and piston is positioned at the zero graduation place in the syringe; Two, assemble 6 reactive systems 2 by the described operation steps of step 1, then 6 reactive systems that assemble 2 are evenly distributed and be placed on around the xenon source 1, wherein quartz reactor 2-1 is over against xenon source 1, and the distance of quartz reactor 2-1 and xenon source 1 is 15cm; Three, open xenon source 1, carry out the photocatalysis hydrogen production reaction, then regularly get the detection gaseous sample, carry out the gas chromatography spectrogram and detect; 15min mixes the density of hydrogen in each reactive system 2 before wherein regularly getting test sample, concrete operation method is: a, the first valve 2-4 is closed, syringe 2-3 in the gas circuit circulating device is pulled to 50mL scale place by zero graduation, then the first valve 2-4 is opened, again second valve 2-5 is closed, again gas circuit circulating device syringe 2-3 is pushed into the zero graduation place, finishes a circulation of a reactive system 2; B, successively remaining reactive system 2 is finished a circulation according to the operation of above-mentioned steps a, finish a systemic circulation this moment, and then 4～8 systemic circulations are finished in repetitive operation, namely finishes mixing of density of hydrogen in the reactive system 2; Wherein regularly getting the method that detects gaseous sample is every 1 hour, gets gaseous sample with the 3rd sebific duct 2-9 of syringe at the second draft tube 2-15 place of each accumulator unit 2-2 of 5mL and gets final product, and namely finishes the evaluation of hydrogen manufacturing performance of photocatalyst.
Nano-TiO in the step 1 in the present embodiment
2The preparation method of film photocatalyst is: adopt anode oxidation method, consisting of the NaF of 5～6g/L and volumetric concentration at electrolytic solution is 2%～5% H
3PO
4In the electrolytic solution of solution, constant voltage anodic oxidation 30min under 20V voltage, the nano-TiO of the nano tube structure that obtains
2Film photocatalyst.Be the 0.1mol/LNa of 50mL by the target solution of catalytic reduction in the step 1
2S and 0.02mol/LNa
2SO
3Aqueous solution, nano-TiO
2The area of film photocatalyst is 2.5cm * 4cm;
Present embodiment adopts the method for parallel laboratory test, estimates the reliability of multi-channel reaction simple device of the evaluating hydrogen production performance of photocatalyst of embodiment 17, and present embodiment is with 6 nano-TiOs with identical catalytic performance of the same area
2Film photocatalyst places respectively 6 reactive systems 2, carries out parallel laboratory test, and the hydrogen output when photocatalysis hydrogen production reaction in each reactive system 2 carried out 1h, 2h and 3h detects, and testing result as shown in Figure 6.As seen from Figure 6, respectively the hydrogen output when corresponding 1h, 2h and 3h is basic identical in each reactive system 2, illustrates that the reliability of multi-channel reaction simple device of evaluating hydrogen production performance of photocatalyst of embodiment 17 is good.
Present embodiment is the reactive system 2 of II to label, when 3h is carried out in the photocatalysis hydrogen production reaction, extracts respectively continuously 3 and detects gaseous sample, is used for the hydrogen content of test reactive system 2 this moment, and its testing result as shown in Figure 7.As seen from Figure 7, the there-necked flask accumulator unit 2-2 of volume 1L, when playing the effect of storage of hydrogen, also play the effect of dilution hydrogen, when making each extraction detect gaseous sample, the intrasystem hydrogen total amount of gas flow relative response that extracts, very little, the concentration that can not affect hydrogen in the reactive system is the hydrogen content in the corresponding reactive system.The introducing of accumulator unit has solved the device of existing evaluating hydrogen production performance of photocatalyst because of narrow space in the reactor, the hydrogen that produces is gathered in the reactor, every extraction once for detection of gas, all can make the content of hydrogen produce very large variation, the a large amount of minimizing, thus the detection of ensuing hydrogen content affected, cause occurring the light-catalyzed reaction time longer, the phenomenon that the amounts of hydrogen that detects tails off on the contrary makes testing result inaccurate.
Claims (10)
1. the multi-channel reaction simple device of an evaluating hydrogen production performance of photocatalyst, by light source (1) be evenly distributed on light source (1) 4～8 reactive systems (2) on every side and form, it is characterized in that reactive system (2) is comprised of two parts, the first is by quartz reactor (2-1), accumulator unit (2-2), gas circuit circulating device (2-3), the first valve (2-4), second valve (2-5), the 3rd valve (2-6), seal rubber plug (2-11), the first escape pipe (2-12), the first draft tube (2-13), the second escape pipe (2-14), the second draft tube (2-15) and the first sebific duct (2-7) that is connected above each parts, the sealing and circulating loop that the second sebific duct (2-8) and the 3rd sebific duct (2-9) form, it two is magnetic stirring apparatus (2-10); Wherein, quartz reactor (2-1) is over against light source (1), the distance of quartz reactor (2-1) and light source (1) is 10～20cm, and the upper sealing of accumulator unit (2-2) is fixed with the second escape pipe (2-14) and the second draft tube (2-15); Quartz reactor (2-1) is sealed by seal rubber plug (2-11), the first escape pipe (2-12) and the first draft tube (2-13) sealing are fixed on seal rubber plug (2-11) inside, the port of the first draft tube (2-13) is positioned at the 5～10mm place, bottom apart from quartz reactor (2-1), the first escape pipe (2-12) is communicated with the second draft tube (2-15) by the 3rd sebific duct (2-9), the second escape pipe (2-14) is communicated with by the second sebific duct (2-8) with the inlet end of gas circuit circulating device (2-3), and the outlet side of gas circuit circulating device (2-3) is communicated with the first draft tube (2-13) by the first sebific duct (2-7); The first valve (2-4) is arranged on the first sebific duct (2-7), second valve (2-5) is arranged on the second sebific duct (2-8), the 3rd valve (2-6) is arranged on the 3rd sebific duct (2-9), and reactor (2-1) places on the magnetic stirring apparatus (2-10); Described gas circuit circulating device (2-3) is syringe or the electronic air extracting pump that is communicated with the glass three-way fixing seal, and wherein, syringe is communicated with the second sebific duct (2-8) and the first sebific duct (2-7) respectively by two ports of glass three-way.
2. the multi-channel reaction simple device of a kind of evaluating hydrogen production performance of photocatalyst according to claim 1 is characterized in that light source (1) is uviol lamp or xenon lamp; Wherein the power of uviol lamp is 125～250W, and the power of xenon lamp is 250～500W.
3. the multi-channel reaction simple device of a kind of evaluating hydrogen production performance of photocatalyst according to claim 1 and 2 is characterized in that accumulator unit (2-2) is the container of volume more than 500mL.
4. the multi-channel reaction simple device of a kind of evaluating hydrogen production performance of photocatalyst according to claim 3 is characterized in that the distance of quartz reactor (2-1) and light source (1) is 15cm.
5. according to claim 1, the multi-channel reaction simple device of 2 or 4 described a kind of evaluating hydrogen production performance of photocatalyst, the port that it is characterized in that the first draft tube (2-13) is positioned at the 8mm place, bottom apart from quartz reactor (2-1).
6. the multi-channel reaction simple device of a kind of evaluating hydrogen production performance of photocatalyst according to claim 5 is characterized in that gas circuit circulating device (2-3) is electronic air extracting pump, and the air capacity of control electronic air extracting pump is 300～600mL/min.
7. carry out the method for evaluating hydrogen production performance such as the multi-channel reaction simple device that adopts evaluating hydrogen production performance of photocatalyst claimed in claim 1, the method that it is characterized in that adopting the multi-channel reaction simple device of evaluating hydrogen production performance of photocatalyst to carry out evaluating hydrogen production performance is: one, be placed in the quartz reactor (2-1) with photocatalyst and by the target solution of catalytic reduction, and seal with sealing-plug (2-11), one end that then will be provided with the 3rd sebific duct (2-9) of the 3rd valve (2-6) is communicated with the first escape pipe (2-12) sealing, the another port of the 3rd sebific duct (2-9) is communicated with the second draft tube (2-15) sealing of accumulator unit (2-2), one end that then will be provided with second sebific duct (2-8) of second valve (2-5) is communicated with the second escape pipe (2-14) sealing of accumulator unit (2-2), one end that will be provided with again first sebific duct (2-7) of the first valve (2-4) is communicated with the first draft tube (2-13) sealing, then keep the first valve (2-4), second valve (2-5) and the 3rd valve (2-6) are open mode, then the another port by the first sebific duct (2-7) continues to pass into nitrogen 10～20min to the first sebific duct (2-7), then the first valve (2-4) and second valve (2-5) are closed, inlet end with gas circuit circulating device (2-3) is communicated with the another port sealing of the second sebific duct (2-8) again, the outlet side of gas circuit circulating device (2-3) is communicated with the another port sealing of the first sebific duct (2-7), assembling obtains reactive system (2), and described gas circuit circulating device (2-3) is electronic air extracting pump; Two, assemble 4～8 reactive systems (2) by the described operation steps of step 1, then 4～8 reactive systems that assemble (2) are evenly distributed and be placed on light source (1) on every side, wherein quartz reactor (2-1) is over against light source (1), and the distance of quartz reactor (2-1) and light source (1) is 10～20cm; Three, open light source (1), start gas circuit circulating device electronic air extracting pump (2-3), carry out the photocatalysis hydrogen production reaction, then regularly get the detection gaseous sample, carry out the gas chromatography spectrogram and detect; Wherein regularly getting the method that detects gaseous sample is every 0.5～1 hour, get gaseous sample with the 3rd sebific duct (2-9) that the syringe of 5mL is located in second draft tube (2-15) of each accumulator unit (2-2), again this gaseous sample is carried out the gas chromatography spectrogram and detect, namely finish the evaluation of hydrogen manufacturing performance of photocatalyst.
8. the multi-channel reaction simple device of employing evaluating hydrogen production performance of photocatalyst according to claim 7 carries out the method for evaluating hydrogen production performance, it is characterized in that regularly getting in the step 3 method that detects gaseous sample was: every 0.5～1 hour, gas circuit circulating device electronic air extracting pump (2-3) is closed, then second valve (2-5) and the 3rd valve (2-6) of each reactive system (2) are closed, then use the syringe of 5mL to get gaseous sample at the 3rd sebific duct (2-9) that second draft tube (2-15) of each accumulator unit (2-2) is located successively, after taking second valve (2-5) and the 3rd valve (2-6) are opened, restarted gas circuit circulating device electronic air extracting pump (2-3) and get final product.
9. carry out the method for evaluating hydrogen production performance such as the multi-channel reaction simple device that adopts evaluating hydrogen production performance of photocatalyst claimed in claim 1, the method that it is characterized in that adopting the multi-channel reaction simple device of evaluating hydrogen production performance of photocatalyst to carry out evaluating hydrogen production performance is: one, be placed in the quartz reactor (2-1) with photocatalyst and by the target solution of catalytic reduction, and seal with sealing-plug (2-11), one end that then will be provided with the 3rd sebific duct (2-9) of the 3rd valve (2-6) is communicated with the first escape pipe (2-12) sealing, the another port of the 3rd sebific duct (2-9) is communicated with the second draft tube (2-15) sealing of accumulator unit (2-2), one end that then will be provided with second sebific duct (2-8) of second valve (2-5) is communicated with the second escape pipe (2-14) sealing of accumulator unit (2-2), one end that will be provided with again first sebific duct (2-7) of the first valve (2-4) is communicated with the first draft tube (2-13) sealing, then keep the first valve (2-4), second valve (2-5) and the 3rd valve (2-6) are open mode, then the another port by the first sebific duct (2-7) continues to pass into nitrogen 10～20min in the first sebific duct (2-7), then the first valve (2-4) and second valve (2-5) are closed, the two-port of gas circuit circulating device (2-3) is communicated with the another port of the second sebific duct (2-8) and the another port sealing of the first sebific duct (2-7) respectively, assembling obtains reactive system (2), described gas circuit circulating device (2-3) is the syringe that is communicated with the glass three-way fixing seal, wherein, syringe is communicated with the second sebific duct (2-8) and the first sebific duct (2-7) sealing respectively by two ports of glass three-way, and piston is positioned at the zero graduation place in the syringe; Two, assemble 4～8 reactive systems (2) by the described operation steps of step 1, then 4～8 reactive systems that assemble (2) are evenly distributed and be placed on light source (1) on every side, wherein quartz reactor (2-1) is over against light source (1), and the distance of quartz reactor (2-1) and light source (1) is 10～20cm; Three, open light source (1), carry out the photocatalysis hydrogen production reaction, then regularly get the detection gaseous sample, carry out the gas chromatography spectrogram and detect; Wherein regularly getting the front 10～15min of test sample mixes the density of hydrogen in each reactive system (2), concrete operation method is: a, the first valve (2-4) cuts out, the syringe (2-3) of gas circuit circulating device is pulled to 50mL scale place by zero graduation, then the first valve (2-4) is opened, again second valve (2-5) is closed, again gas circuit circulating device syringe (2-3) is pushed into the zero graduation place, finishes a circulation of a reactive system (2); B, successively remaining reactive system (2) is finished a circulation according to the operation of above-mentioned steps a, finish a systemic circulation this moment, and then 4～8 systemic circulations are finished in repetitive operation, namely finishes mixing of density of hydrogen in the reactive system (2); Wherein regularly getting the method that detects gaseous sample is every 0.5～1 hour, get gaseous sample with the 3rd sebific duct (2-9) that the syringe of 5mL is located in second draft tube (2-15) of each accumulator unit (2-2), again this gaseous sample is carried out the gas chromatography spectrogram and detect, namely finish the evaluation of hydrogen manufacturing performance of photocatalyst.
10. the multi-channel reaction simple device of employing evaluating hydrogen production performance of photocatalyst according to claim 9 carries out the method for evaluating hydrogen production performance, it is characterized in that regularly getting in the step 3 method that detects gaseous sample was: every 0.5～1 hour, second valve (2-5) and the 3rd valve (2-6) of each reactive system (2) are closed, then use the syringe of 5mL to get gaseous sample at the 3rd sebific duct (2-9) that second draft tube (2-15) of each accumulator unit (2-2) is located successively, after taking second valve (2-5) and the 3rd valve (2-6) opened and get final product.
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| 崔文权等.纳米Pt/TiO2催化剂上气相CH3OH光催化分解制氢的研究.《化学学报》.2005,第63卷(第3期),203-209. * |
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