CN205484185U - Three electrode reactor - Google Patents

Three electrode reactor Download PDF

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Publication number
CN205484185U
CN205484185U CN201620220683.6U CN201620220683U CN205484185U CN 205484185 U CN205484185 U CN 205484185U CN 201620220683 U CN201620220683 U CN 201620220683U CN 205484185 U CN205484185 U CN 205484185U
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China
Prior art keywords
electrode
hole
sidewall
reactor
fixing
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Withdrawn - After Issue
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CN201620220683.6U
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Chinese (zh)
Inventor
王喜娜
童锐
许扬
周小龙
汪汉斌
王浩
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Hubei University
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Hubei University
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Abstract

The utility model provides a three electrode reactor, the whole leakproofness of this three electrode reactor is good, can effectively avoid the infiltration or inside gaseous the revealing of outside air, has both guaranteed the reliability of producing depressed fruit, also can realize high -purity H2's preparation, this three electrode reactor both can external electrochemistry workstation or the current -voltage table, can carry out the gas washing and produce the gas sample reactor portion again, therefore can realize smooth water electrolysis process's synchronous optical electro -Chemistry action and gas production analysis to further investigation photoelectrolysis water system intrinsic optical electro -Chemistry mechanism, and the brineelectrolysis efficiency evaluation of setting a camera.

Description

Three electrode reactors
Technical field
This utility model relates to sunlight electrolysis water field, particularly relates to a kind of three electrode reactors.
Background technology
In recent years, along with non-renewable Fossil fuels such as the development of World Economics, coal, oil, natural gass Acceleration consumption, traditional energy system changes the most step by step, and exploitation and the development work of new forms of energy are the most urgent At the eyebrows and eyelashes.Solar energy is a kind of new green power, utilizes sunlight decomposition water hydrogen making, at Fossil fuel Day by day exhausted and that environmental pollution is serious society receives much concern [[1] Guo Liejin, Liu Tao, Ji Jun, et al.Science&Technology Review,2005,23(2):29-33]。
It addition, in the energy system of 21 century, hydrogen is a kind of preferably energy, and hydrogen energy source is efficient, ring Protect, its energy density (140MJ/Kg2) it is solid fuel (50MJ/Kg2) twice many, the heat of releasing is about For homogenous quantities gasoline 3 times.Meanwhile, hydrogen is nontoxic, cleans most compared with other fuel during burning, except generating Such as carbon monoxide, carbon dioxide, Hydrocarbon, leaded thing and powder will not be produced outside water and a small amount of hydrogen chloride The environmental contaminants such as dirt granule.By this kind of the conception inspiration, convert solar energy into the Hydrogen Energy of high-energy-density, draw Play the broad interest of scientific research personnel.And hydrogenous material is mainly water in nature, it is to obtain by photoelectrolysis water Obtain a direct way of Hydrogen Energy.
When cell reaction is in acidity or neutral system, its electrode reaction equation is as follows, negative electrode: 4H++4e→2H2, Φ0=0V;Anode: 2H2O→O2+4H++4e,Φ0=1.23V, in water electrolysis reaction, It is an extremely complex electrode process that the anode of oxygen separates out, and this reaction relates to the electrification that four electronics are participated in Learn reaction, during be frequently accompanied by bigger overpotential, therefore the anode evolution reaction of oxygen needs than oxygen Could react under the current potential of equilibrium potential corrigendum, if it is possible to utilize the luminous energy in nature with open arms, utilize half The photoelectric conversion process of conductor material, is done directly the conversion of " photochemical energy ", thus can sufficiently improve The utilization ratio of energy.
At present, utilize sunlight electrolysis water research be concentrated mainly on various light (electric) catalysis material preparation, The aspects such as the sign of photoelectrochemical property and the exploration of phonons acoustical scattering, and to for three-electrode system photoelectricity Produce hydrogen or to produce the research of reactor assembly of oxygen the most less, also lack a kind of reasonable, can testing photoelectronic stream Again can synchronized sampling test hydrogen or the device of oxygen output.Although photocatalytic water reactor aspect has many reports at present Road, such as, the novel photoelectric solution pool structure of the invention such as Yu Hongmei in 2012 can by the excitation of light, By a kind of device [[2], and Chinese Academy of Sciences's Dalian Chemical Physics that water decomposition is hydrogen and oxygen in alkaline solution Institute is also prepared for a kind of photoelectrolytic cell decomposition water hydrogen production bioreactor, and [Chinese invention is special Profit, CN102336453A, 2012-02-01] etc., but these devices are mainly used in photocatalytic semiconductor powder body product The preparation and measurement of hydrogen, it is impossible to for three-electrode system.If the synchro measure of three-electrode system can not be realized, Just photocurrent characteristics cannot be connected one by one with hydrogen output, thus go further to evaluate photoelectrolysis water battery Coulombic efficiency and analysis oxygen, evolving hydrogen reaction dynamical mechanism.Therefore, exploitation one laboratory is feasible, sealing Well, can be connected with three-electrode electro Chemical work station, the photoelectrolysis of Tong Bu hydrogen or oxygen detection can be realized again Water reactor is extremely important.
Utility model content
The purpose of this utility model is to provide that a kind of laboratory is feasible, sealing good, can be with three electrode electrochemical Learn work station to be connected, can realize again synchronizing hydrogen or three electrode reactors of oxygen detection and application thereof.
In order to achieve the above object, this utility model provides a kind of three electrode reactors, and it includes that an electrode is solid Determining sealing device, and a reaction vessel, described reactor head offers main interface, sidewall is offered respectively There are the outlet of gas washing entrance, gas washing and aerogenesis sample tap;Described electrode fixing seal device includes sealing flange and electricity Pole support bar, sealing flange seals with main interface and surface offers three through holes, and described electrode supporting bar is worn Crossing through hole and seal therewith, fix, electrode supporting bar is conductive material, and bottom is fixed, is electrically connected with electrode.
Preferably, described reaction vessel is quartz glass material, and is provided with a flat sidewall.
Described gas washing entrance is oppositely arranged along reactor axis with gas washing outlet, and gas washing entrance extends to reaction Bottom device.
Described sealing flange includes running through public law orchid and rim of the mouth flange, runs through public law orchid and includes top cover portion and bottom Extension, top cover portion is provided with three through holes;Rim of the mouth flange base is provided with support ring, extension side Wall is threadeded with rim of the mouth flange sidewalls, and seals with support ring bottom extension.It is further preferred that it is described Be provided with circular rubber gaskets bottom extension and between main interface top, bottom described extension with support ring it Between be provided with half-round metal packing ring, be provided with rubber sealant bottom described half-round metal packing ring.Further Preferably, described through hole is internally provided with circumferential support step, and is positioned at the sidewall at circumferential support step two ends On be provided with screw thread, each electrode supporting bar is provided with two fixing nuts, and described fixing nut leads to through hole Cross described threaded and support with circumferential support step upper and lower end face and seal respectively.Concrete, also include O Circle, described O-ring is arranged between circumferential support step upper and lower end face and fixing nut.
It is provided with electrode clamp groove bottom described electrode supporting bar and runs through sidewall and electrode clamp groove Screwed hole and screw.
Also include that an altitude mixture control base, described altitude mixture control base include horizontal base, screw rod, slide block and Fixing screw, fix vertical with horizontal base of described screw rod is connected, and slide block is fixing with sealing flange to be connected, slide block Centre is provided with through hole, is provided with slide block screwed hole between sidewall and through hole, screw rod through through hole and with Fixing.
The beneficial effects of the utility model are: (1) this three electrode reactors overall tightness is good, can be effective Avoid the infiltration of outside air or the leakage of internal gas, both ensure that the reliability of aerogenesis result, it is also possible to be real Existing high-purity H2Preparation.(2) this three electrode reactor both can external electrochemical workstation or current voltmeter, Inside reactor can be carried out again gas washing and aerogenesis sampling, thus the synchronizable optical electrification of photoelectrolysis water process can be realized Scholarship and moral conduct is and gas production analysis, thus furthers investigate the Optical Electro-Chemistry mechanism that photoelectrolysis water system is inherent, and to light Electrolysis water efficiency is evaluated.
Accompanying drawing explanation
Fig. 1 is the front view of this utility model reaction vessel;
Fig. 2 is the top view of this utility model reaction vessel;
Fig. 3 is this utility model electrode fixing seal device and the explosive view of altitude mixture control base;
Fig. 4 is the oxygen time chart that this utility model embodiment 1 obtains;
Fig. 5 is the oxygen time chart that this utility model embodiment 1 obtains;
Fig. 6 is the oxygen time chart that this utility model embodiment 2 obtains;
Fig. 7 is the chromatographic result that this utility model embodiment 5 obtains.
Detailed description of the invention
As shown in Figure 1, Figure 2 and Figure 3, this utility model provides a kind of three electrode reactors, and it includes one Electrode fixing seal device 1, and a reaction vessel 2, described reactor 2 top offers main interface 21, Gas washing entrance 22, gas washing outlet 23 and aerogenesis sample tap 24 is offered respectively on sidewall.Wherein, main interface 21 are tightly connected sealing flange 11, and gas washing entrance 22 meets N2Or argon bottle, gas washing is gone out by gas washing via solution Mouthfuls 23 discharge, and aerogenesis sample tap 24 is for syringe sampling, it is possible to achieve in vacuum environment or noble gas Protect the solution gas washing in environment and subsequent hydrogen or oxygen measurement.Concrete, gas washing entrance 22 and gas washing Outlet 23 is standard interface, conveniently connects the trachea such as rubber tube, plastic tube, main interface 21 and aerogenesis sample tap 24 is cylindrical, in order to and sealing flange 11 is external.Preferably, described reaction vessel 2 is quartz glass material Matter, and it is provided with a flat sidewall 25, to reduce the reflection of light, improve its light transmittance.Preferably, described Gas washing entrance 22 is oppositely arranged along reactor 2 axis with gas washing outlet 23, and gas washing entrance 22 extends to Bottom reactor 2.So, the when of facilitating gas washing, the air in reaction vessel 2 is drained, it is to avoid cause reality Test error.
Described electrode fixing seal device 1 includes sealing flange 11 and electrode supporting bar 12, described sealing flange 11 include running through public law blue 112 and rim of the mouth flange 113, run through public law orchid 112 and include top cover portion 1121 He The extension 1122 of bottom, top cover portion 1121 is provided with three through holes 111;Bottom rim of the mouth flange 113 Being provided with support ring 1131, extension 1122 sidewall is connected with rim of the mouth flange 113 sidewall thread, described extension Circular rubber gaskets (114), described extension it is provided with bottom portion 1122 and between main interface (21) top (1122) it is provided with half-round metal packing ring 115, described half-round metal between bottom and support ring 1131 Rubber sealant 1151 it is provided with bottom packing ring 115.
Common, three through holes 111 are correspondingly arranged two electrode supporting bars 12 and a reference electrode respectively. Described electrode supporting bar 12 is through through hole 111 and seals therewith, fix.Concrete, described through hole 111 It is internally provided with circumferential support step 1111, and is positioned on the sidewall at circumferential support step 1111 two ends and is provided with Screw thread, each electrode supporting bar 12 is provided with two fixing nuts 13, described fixing nut 13 and through hole 111 by described threaded and support with circumferential support step 1111 upper and lower end face and seal respectively.So, On the one hand, two fixing nut 13 localizing electrode support bars 12 can be passed through and run through public law orchid 112;Second party Face, can effective enclosed electrode support bar 12 and run through public law orchid 112, it is preferred that also include O-ring 14, institute State O-ring 14 to be arranged between circumferential support step 1111 upper and lower end face and fixing nut 13.
Electrode supporting bar 12 is conductive material, bottom be provided with electrode clamp groove 121 and run through sidewall with The screwed hole 122 of electrode clamp groove 121 and screw 123.So, electrode can be clamped in clamp groove 121 In and fix with screw 123.Electrode supporting bar 12 top has contact conductor to pick out, in order to electrochemistry work Make the instrument such as station to connect.
Described altitude mixture control base 3 is used for fixing reaction vessel 2 and electrode fixing seal device 1, and regulates and controls it Highly.Concrete, described altitude mixture control base 3 includes horizontal base 31, screw rod 32, slide block 33 and solid Determining screw 34, fix vertical with horizontal base 31 of described screw rod 32 is connected, slide block (33) and sealing flange 11 fixing connections, are provided with through hole 331 in the middle of slide block (33), set between sidewall and through hole (331) Being equipped with slide block screwed hole 332 and slide block screw 333, screw rod 32 is through through hole 331 fixed thereto.
Below in conjunction with specific embodiment, of the present utility model three electrode reactors are discussed in detail.
Embodiment 1
Loading in through hole 111 by two electrode supporting bars 12, another through hole 111 is inserted into reference electrode, Seal with O-ring, inject a certain amount of electrolyte solution, wherein, electrolysis from the main interface 21 of reaction vessel 2 The liquid level of liquid, less than gas washing outlet 23 and aerogenesis sample tap 24, then accesses reaction vessel 2 sealing flange 11 Main interface 21, and be fixed on altitude mixture control base 3, close aerogenesis sample tap 24.
It is passed through high-purity N by gas washing entrance 222, open gas washing outlet 23, to reaction vessel 2 and inside simultaneously Electrolyte carry out gas washing, drive air therein away, after about 30 minutes, close gas washing entrance 22 and gas washing and go out Mouth 23, i.e. uses clamp rubber tube, makes reaction vessel 2 internal holding inert atmosphere.
Employing standard 1mL syringe takes gas 0.8mL by aerogenesis sample tap 24, and is injected into gas chromatogram H remaining in instrument analysis reactor2And O2Content, to detect the sealing of inside reactor, result such as Fig. 4 Shown in Fig. 5.Result shows, within 8h, is not detected by obvious H2Peak, and the leak rate of oxygen is about 1.1 μm ol/h, show that the air-tightness of this three electrode reactor is preferable, and the data that experiment is measured the most truly may be used Lean on.
Embodiment 2
Loading in through hole 111 by two electrode supporting bars 12, another through hole 111 is inserted into reference electrode, Seal with O-ring, inject a certain amount of electrolyte solution, wherein, electrolysis from the main interface 21 of reaction vessel 2 The liquid level of liquid, less than gas washing outlet 23 and aerogenesis sample tap 24, then accesses reaction vessel 2 sealing flange 11 Main interface 21, and be fixed on altitude mixture control base 3, close gas washing entrance 22 and aerogenesis sample tap 24.
By external with mechanical pump by angle valve for gas washing outlet 23, open angle valve and mechanical pump, evacuation 30min Rear closedown angle valve.
Employing standard 1mL syringe takes gas 0.8mL by aerogenesis sample tap 24, and is injected into gas chromatogram H remaining in instrument analysis reactor2And O2Content, to detect the sealing of inside reactor, result such as Fig. 6 Shown in.Result shows within 5h, is all not detected by the peak of hydrogen and oxygen, shows the gas of this test device Close property is preferable, and the data that experiment is measured are the most true and reliable.
Embodiment 3
Two electrode supporting bars 12 are loaded in through hole 111, tighten the screw 123 of electrode supporting bar 12 lower end, Fixing light anode, negative electrode respectively, light anode is semiconductor light electrolysis water material and the plane near reaction vessel 2 Sidewall 25, flat sidewall 25 is just to perpendicular light source;The top of anode electrode support bar 12 and electrochemical operation The working electrode stood be connected, the electrode clamp groove 121 of cathode electrode support bar 12 fix high-purity platinized platinum and with Light anode material is the most right, and electrode (CE) is connected by the other end be connected electrochemical workstation;By reference electrode Inserting in another through hole 111, seal with O-ring, reference electrode is by the corresponding interface of flange and electrochemistry work The reference electrode (RE) making to stand is connected.
Injecting electrolyte solution from the main interface 21 of reaction vessel 2, wherein, the liquid level of electrolyte is less than gas washing Outlet 23 and aerogenesis sample tap 24, then access sealing flange 11 main interface 21 of reaction vessel 2, and It is fixed on altitude mixture control base 3, it is ensured that the lower half of electrolyte submergence above three electrode, spills electrode and prop up Electrode clamp groove 121 part of strut 12.Close aerogenesis sample tap 24.
It is passed through high-purity N by the gas washing entrance 22 of reaction vessel 22, open gas washing outlet 23, to reaction simultaneously The electrolyte of container 2 and inside carries out gas washing, i.e. drives air therein away, after about 30 minutes, closes gas washing Entrance 22 and gas washing outlet 23, make inside reactor keep inert atmosphere.
Open light source, adjust the optical power density arriving light anode material surface, after stablizing 5 minutes, pass through Electrochemical workstation provides a bias relative to reversible hydrogen electrode, with this test device to test photoelectrolysis water Produce the hydrogen oxygen-producing amount Changing Pattern with the response time, every half an hour with microsyringe from reaction vessel 2 Aerogenesis sample tap 24 takes out the gas of 0.8ml, is injected in gas chromatograph and is analyzed.
Embodiment 4
The present embodiment is substantially the same manner as Example 3, and difference is, light anode and negative electrode and constant current constant voltage source The both positive and negative polarity of table connects.
Embodiment 5
Two electrode supporting bars 12 are loaded in through hole 111, tighten the screw 123 of electrode supporting bar 12 lower end, Fixing light anode, negative electrode respectively, light anode is FTO/TiO2/BiVO4/ Co-Pi substrate and close reaction vessel 2 Flat sidewall 25, flat sidewall 25 just to perpendicular light source, time extremely Pt sheet;Anode electrode support bar The top of 12 is connected with the working electrode of electrochemical workstation, the electrode clamp groove of cathode electrode support bar 12 121 fix high-purity platinized platinum and the most right with light anode material, the other end be connected electrochemical workstation to electrode (CE) it is connected;Being inserted by reference electrode in another through hole 111, seal with O-ring, reference electrode uses full The Ag/AgCl of sum, is connected with the reference electrode (RE) of electrochemical workstation by the corresponding interface of flange.
Main interface 21 from reaction vessel 2 injects the KH of 40ml2PO4And Na2SO3Mixed solution, wherein, The liquid level of mixed solution, less than gas washing outlet 23 and aerogenesis sample tap 24, then accesses sealing flange 11 instead Answer the main interface 21 of container 2, and be fixed on altitude mixture control base 3, it is ensured that electrolyte submergence above three The lower half of electrode, spills electrode clamp groove 121 part of electrode supporting bar 12.Close aerogenesis sample tap 24。
Opening light source, the optical intensity density adjusting arrival light anode material surface is 100mW/cm2, stablize 5 points After clock, provide a bias relative to reversible hydrogen electrode 1.0V by electrochemical workstation, test with this Device to test TiO2/BiVO4The product hydrogen oxygen-producing amount of/Co-Pi light anode material is with the Changing Pattern in response time, often Every half an hour with microsyringe from the gas of reactor sample tap taking-up 0.8ml, it is injected into gas chromatograph In be analyzed, obtained result is as shown in Figure 7.
As seen from Figure 7, this three electrode reactor the TiO tested out2/BiVO4Light anode material Produce hydrogen and product oxygen speed is respectively 3.562 μm ol/cm2/ h and 1.570 μm ol/cm2/h.The linearly increasing theory of yield The air-tightness of this three electrode reactor bright is preferable, and experimental result is genuine and believable, can be used as three-electrode system photocatalytic water The test device of system.
The foregoing is only better embodiment of the present utility model, not in order to limit utility model, all at this Within the spirit of utility model and principle, any modification, equivalent substitution and improvement etc. done, should be included in Within protection domain of the present utility model.

Claims (9)

1. three electrode reactor, it includes electrode fixing seal device (1), and a reaction vessel (2), It is characterized in that: described reactor (2) top offers main interface (21), sidewall offers respectively and washes Gas entrance (22), gas washing outlet (23) and aerogenesis sample tap (24);Described electrode fixing seal device (1) Including sealing flange (11) and electrode supporting bar (12), sealing flange (11) seals with main interface (21) And surface offers three through holes (111), described electrode supporting bar (12) through through hole (111) and Sealing therewith, fix, electrode supporting bar (12) is conductive material, and bottom is fixed, is electrically connected with electrode.
Three electrode reactors the most as claimed in claim 1, it is characterised in that: described reaction vessel (2) is stone English glass material, and it is provided with a flat sidewall (25).
Three electrode reactors the most as claimed in claim 1, it is characterised in that: described gas washing entrance (22) with wash Gas outlet (23) is oppositely arranged along reactor (2) axis, and gas washing entrance (22) extends to reactor (2) bottom.
Three electrode reactors the most as claimed in claim 1, it is characterised in that: described sealing flange (11) includes Run through public law blue (112) and rim of the mouth flange (113), run through public law blue (112) and include top cover portion (1121) With the extension (1122) of bottom, top cover portion (1121) is provided with three through holes (111);Rim of the mouth Flange (113) bottom is provided with support ring (1131), extension (1122) sidewall and rim of the mouth flange (113) Sidewall thread connects, and extension (1122) bottom seals with support ring (1131).
Three electrode reactors the most as claimed in claim 4, it is characterised in that: described extension (1122) bottom And it is provided with circular rubber gaskets (114), described extension (1122) end between main interface (21) top Half-round metal packing ring (115), described half-round metal packing ring it is provided with between portion and support ring (1131) (115) bottom is provided with rubber sealant (1151).
Three electrode reactors the most as claimed in claim 4, it is characterised in that: described through hole (111) is internal It is provided with circumferential support step (1111), and is positioned on the sidewall at circumferential support step (1111) two ends setting Screw thread, each electrode supporting bar (12) is had to be provided with two fixing nuts (13), described fixing nut (13) Threaded with through hole (111) by described and support with circumferential support step (1111) upper and lower end face respectively Hold and seal.
Three electrode reactors the most as claimed in claim 6, it is characterised in that: also include O-ring (14), described O-ring (14) is arranged between circumferential support step (1111) upper and lower end face and fixing nut (13).
Three electrode reactors the most as claimed in claim 1, it is characterised in that: described electrode supporting bar (12) end Portion is provided with electrode clamp groove (121) and runs through the screwed hole (122) of sidewall and electrode clamp groove (121) With screw (123).
Three electrode reactors the most as claimed in claim 1, it is characterised in that: also include an altitude mixture control base (3), Described altitude mixture control base (3) includes horizontal base (31), screw rod (32), slide block (33) and solid Determining screw (34), described screw rod (32) is vertical with horizontal base (31) fixing to be connected, slide block (33) and Sealing flange (11) is fixing to be connected, and is provided with through hole (331) in the middle of slide block (33), and sidewall is with through Be provided with slide block screwed hole (332) between hole (331), screw rod (32) through through hole (331) and with Fixing.
CN201620220683.6U 2016-03-22 2016-03-22 Three electrode reactor Withdrawn - After Issue CN205484185U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105651839A (en) * 2016-03-22 2016-06-08 湖北大学 Three-electrode reactor and application thereof
CN110461474A (en) * 2017-02-02 2019-11-15 艾卡工厂有限及两合公司 Closing means, electrochemical vessel and laboratory equipment for electrochemical vessel

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105651839A (en) * 2016-03-22 2016-06-08 湖北大学 Three-electrode reactor and application thereof
CN105651839B (en) * 2016-03-22 2018-12-25 湖北大学 Three electrode reactors and its application
CN110461474A (en) * 2017-02-02 2019-11-15 艾卡工厂有限及两合公司 Closing means, electrochemical vessel and laboratory equipment for electrochemical vessel
CN110461474B (en) * 2017-02-02 2022-03-04 艾卡工厂有限及两合公司 Closing mechanism for electrochemical container, electrochemical container and laboratory device

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Granted publication date: 20160817

Effective date of abandoning: 20181225