CN106556637A - A kind of photoelectrocatalysis reaction experiment device - Google Patents

A kind of photoelectrocatalysis reaction experiment device Download PDF

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Publication number
CN106556637A
CN106556637A CN201611001326.1A CN201611001326A CN106556637A CN 106556637 A CN106556637 A CN 106556637A CN 201611001326 A CN201611001326 A CN 201611001326A CN 106556637 A CN106556637 A CN 106556637A
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China
Prior art keywords
electrode
chamber
mouth
experiment device
reaction experiment
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Pending
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CN201611001326.1A
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Chinese (zh)
Inventor
王平
杨姮妍
王现英
孙峰
李慧珺
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Priority to CN201611001326.1A priority Critical patent/CN106556637A/en
Publication of CN106556637A publication Critical patent/CN106556637A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416Systems
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416Systems
    • G01N27/4162Systems investigating the composition of gases, by the influence exerted on ionic conductivity in a liquid
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Molecular Biology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

Photoelectrocatalysis reaction experiment device of the invention, by being connected with electro-chemical systems and gas chromatograph simultaneously, so that the photoelectric current and gaseous products of synchronous detection photovoltaic reaction generation when pending gas is processed by photovoltaic reaction, can be realized, characterized in that, including:Reacting part, with all use quartz material into chamber and closure;Intake section, is arranged on chamber and is connected with chamber, and the inside for pending gas to be incorporated into chamber is reacted;Exhaust portion, is arranged on chamber and is connected with chamber, detected for gaseous products are drawn out to gas chromatograph within the chamber;And electrode oral area, reference electrode mouth on side wall with three directions for being separately positioned on chamber, to electrode ports and working electrode mouth, reference electrode mouth with electrode ports are oppositely arranged, be respectively mounted be connected with electro-chemical systems reference electrode post, to electrode column and working electrode post.

Description

A kind of photoelectrocatalysis reaction experiment device
Technical field
The present invention relates to a kind of photoelectrocatalysis reaction experiment device, the new photoelectrocatalysis reaction of more particularly to a kind of many work( Experimental provision.
Background technology
Used as the measuring apparatus that electrochemical research and teaching are conventional, its inside of electrochemical workstation occurs with data signal Device, data collecting system, multilevel signal gain, glucose current equation traffic filter, IR drop compensation circuits, galvanostat, constant potential Instrument, can complete the observing and controlling to some electrochemical parameters under different situations, using extremely wide in electrochemical measurement.And gas phase color Spectrometer is except for qualitatively and quantitatively analyzing in mixed gas in addition to each component, moreover it is possible to distribution system of the determination sample in fixing phase The physicochemical constants such as number, activity coefficient, molecular weight and specific surface area, thus in chemical industry, environmental protection, pharmaceutical sanitary field application very Extensively.It is worth noting that, as the analysis testing equipment that laboratory and scientific research institution are conventional, electrochemical workstation and gas-chromatography Instrument is all high to experimental situation requirement, repeats experiment difficulty very big.
Thus photoelectric current and photoelectrocatalysis gaseous products data how simultaneously and are accurately measured, lead in photocatalysis technology Compare stubborn problem in always one, domain.
The content of the invention
The present invention is proposed to solve the above problems, it is therefore intended that provide a kind of energy synchronous detection light electrocatalytic reaction The photoelectrocatalysis reaction experiment device of the photoelectric current and gaseous products of generation.
Present invention employs technical scheme below:
A kind of photoelectrocatalysis reaction experiment device, by being connected with electro-chemical systems and gas chromatograph respectively, is used for Carry out photovoltaic reaction to process pending gas and synchronously detect the photoelectric current and gaseous products of photovoltaic reaction generation, its feature exists In, including:Reacting part, in cylinder shape, with all use quartz material into chamber and closure, the chamber has opening, Closure is used to seal opening;Intake section, is arranged on chamber and is connected with chamber, for pending gas is incorporated into chamber Reacted the inside of room;
Exhaust portion, is arranged on chamber and is connected with chamber, for gaseous products are drawn out to gas phase color within the chamber Spectrometer is detected;And electrode oral area, it is reference electrode mouth on the side wall with three directions for being separately positioned on chamber, right Electrode ports and working electrode mouth, reference electrode mouth with electrode ports are oppositely arranged, wherein, reference electrode mouth, to electrode ports, work Be respectively mounted as electrode ports be connected with electro-chemical systems reference electrode post, to electrode column and working electrode post, for electrification System provides voltage to photovoltaic reaction, and forms the current loop of photoelectric current, and photoelectric current imports electrochemistry by current loop System is detected.
The photoelectrocatalysis reaction experiment device that the present invention is provided, also has the feature that:Wherein, reacting part is highly 130mm, chamber are in cylindrical, and its external diameter is 70mm, and opening inside diameter is 65mm.
The photoelectrocatalysis reaction experiment device that the present invention is provided, also has the feature that:Wherein, closure and opening all Frosted interface is provided with, and coordinates c-type to seal fastener by silicone gasket and sealed.
The photoelectrocatalysis reaction experiment device that the present invention is provided, also has the feature that:Wherein, intake section is air inlet Pipe, one end of air inlet pipe stretch into chamber and extend downwardly, and air inlet pipe is 6mm with the external diameter of exhaust portion.
The photoelectrocatalysis reaction experiment device that the present invention is provided, also has the feature that:Wherein, reference electrode mouth, right Polytetrafluoroethylsealed sealed packing ring is provided with electrode ports, working electrode mouth.
The photoelectrocatalysis reaction experiment device that the present invention is provided, also has the feature that:Wherein, to electrode using platinum electricity Pole, reference electrode is using silver or silver chloride electrode.
The photoelectrocatalysis reaction experiment device that the present invention is provided, also has the feature that:Wherein, reference electrode mouth, right Electrode ports, the external diameter of working electrode mouth are 10mm.
Invention effect and effect
Photoelectrocatalysis reaction experiment device of the invention, as electro-chemical systems and gas chromatograph can be connected, Institute has ensured experiment accuracy, while significantly under identical appointed condition in order to synchronous detection photoelectric current and gaseous products Experimental period has been saved, operating efficiency has been improve.
Description of the drawings
Fig. 1 is the structural representation of the photoelectrocatalysis reaction experiment device in the embodiment of the present invention.
Specific embodiment
Embodiment
The specific embodiment of embodiments of the invention is illustrated below in conjunction with accompanying drawing.
Fig. 1 is the structural representation of the photoelectrocatalysis reaction experiment device in the embodiment of the present invention.
As shown in figure 1, photoelectrocatalysis reaction experiment device 100 includes reacting part 10, intake section 20, exhaust portion 30 and electricity In highest terms portion 40.
Reacting part 10 is in cylinder shape, is highly 130mm, with chamber 11 and closure 12.
Chamber 11 is made using quartz material in cylinder, and for the container as photovoltaic reaction, its external diameter is 70m, is had There is opening, the opening inside diameter is 65mm.
Closure 12 is made using quartz material, and the opening with chamber 11 is frosted interface, and coordinates C by silicone gasket Type sealing fastener seals the opening.
Intake section 20 is air inlet pipe, and a diameter of 6mm of the air inlet pipe is arranged on chamber and is connected with chamber, one End is into chamber 11, and extends downwardly the bottom until chamber 11, for pending gas to be incorporated into the inside of chamber 11.
Exhaust portion 30 is arranged on the top of chamber 12, is connected above and with chamber 12, carries out for treating processing gas The gaseous products produced after photovoltaic reaction, are drawn out to gas chromatograph from chamber 12, at this moment can just be examined by gas chromatograph Survey the gaseous products.
Electrode oral area 40 is with reference electrode mouth 41, to electrode ports 42 and working electrode mouth 43, above three electrode ports Be separately positioned on three side walls of chamber 11, and reference electrode mouth 41 with electrode ports 42 are oppositely arranged, these three electrodes The external diameter of mouth is 10mm, and is all additionally provided with polytetrafluoroethylsealed sealed packing ring, so when electrode column is placed in electrode ports, Ke Yitong Cross the polytetrafluoroethylsealed sealed packing ring to be sealed.Platinum electrode is adopted to electrode 42, reference electrode 41 is using silver or silver chloride electrode.When making Used time, reference electrode post is placed in reference electrode mouth 41, placing electrode ports 42 to electrode column, and in working electrode mouth 43 Working electrode post is placed, and then each electrode column is connected with electro-chemical systems, photovoltaic reaction is pressurised into by electro-chemical systems Offer voltage, and the current loop of the photoelectric current of photovoltaic reaction generation is formed, such photoelectric current is returned by the current loop Electro-chemical systems and be detected.
The use step of electrocatalytic reaction experimental provision 100 is specifically described below:
Step one, weighs 10-200mg powdery photocatalysts, adds into 30-200ml electrolyte, pour chamber 11 into In, then by ultrasonic disperse 10 minutes.
Step 2, places reference electrode post, electrode ports 42 is being placed to electrode column, working electrode in reference electrode mouth 41 Mouth 43 places working electrodes, it is ensured that each electrode column is immersed under liquid level of electrolyte, and each electrode ports good seal.
Step 3, it is ensured that after 11 good seal of chamber, is continuously passed through high pure nitrogen as carrier gas from intake section 20, to chamber Purging cleaning is carried out in 11 30 minutes to 2 hours, until remaining without air in reactor, exhaust portion 30 is connected to into gas phase at this moment Chromatograph.
Step 4, starts light source prolonged exposure reactor, and by electro-chemical systems to working electrode post and to electrode Post applies certain voltage, while opening gas chromatograph, thus can detect photoelectric current by electro-chemical systems, moreover it is possible to pass through The gaseous products produced in gas chromatograph timing acquiring chamber 11 carry out qualitative and quantitative analysis.
The effect of embodiment and effect
According to photoelectrocatalysis reaction experiment device of the invention, as electro-chemical systems and gas-chromatography can be connected Instrument, institute have ensured experiment accuracy, while greatly under identical appointed condition in order to synchronous detection photoelectric current and gaseous products Experimental period has been saved greatly, operating efficiency has been improve;Simultaneously as manufacture craft is simple, and the material of reacting part is quartz, So cost of manufacture is relatively low and will not be to environment.
Further, as closure and opening are frosted interface, and c-type sealing fastener is coordinated to carry out by silicone gasket Sealing, and each electrode ports is provided with polytetrafluoroethylsealed sealed packing ring so that and air-tightness during reaction in cavity is greatly improved, and is ensured Experiment is accurate.
In addition, experiment of the photoelectrocatalysis reaction experiment device of the present embodiment for detection during photovoltaic reaction, as this , now only there is light reaction in the photoelectrocatalysis reaction experiment device of invention, it is also possible to the test experience being served only for during light reaction, only Gaseous products are detected by the gas chromatograph for connecting.
Although being described to the specific embodiment of description of the invention above, in order to the technology of the art Personnel understand the present invention, it should be apparent that the invention is not restricted to the scope of specific embodiment, the common skill to the art For art personnel, as long as various change is in appended claim restriction and the spirit and scope of the present invention for determining, these Change is it will be apparent that all utilize the innovation and creation of present inventive concept in the row of protection.

Claims (7)

1. a kind of photoelectrocatalysis reaction experiment device, by being connected with electro-chemical systems and gas chromatograph respectively, be used for into Row photovoltaic reaction processes pending gas and synchronously detects the photoelectric current and gaseous products of the photovoltaic reaction generation, its feature It is, including:
Reacting part, in cylinder shape, with all use quartz material into chamber and closure, the chamber has opening, described Closure is used to seal the opening;
Intake section, is arranged on the chamber and is connected with the chamber, described for the pending gas is incorporated into Reacted the inside of chamber;
Exhaust portion, is arranged on the chamber and is connected with the chamber, for by the gaseous products from the within the chamber It is drawn out to the gas chromatograph to be detected;And
Electrode oral area, reference electrode mouth on the side wall with three directions for being separately positioned on the chamber, to electrode ports with And working electrode mouth, the reference electrode mouth is oppositely arranged to electrode ports with described,
Wherein, the reference electrode mouth, the reference being connected with the electro-chemical systems is respectively mounted to electrode ports, working electrode mouth Electrode column, to electrode column and working electrode post, voltage is provided to the photovoltaic reaction for the electro-chemical systems, and is formed The current loop of the photoelectric current, the photoelectric current import the electro-chemical systems by the current loop and are detected.
2. photoelectrocatalysis reaction experiment device as claimed in claim 1, it is characterised in that:
Wherein, the reacting part is highly 130mm,
The chamber is in cylindrical, and its external diameter is 70mm,
The opening inside diameter is 65mm.
3. photoelectrocatalysis reaction experiment device as claimed in claim 1, it is characterised in that:
Wherein, the closure is both provided with frosted interface with the opening, and coordinates c-type sealing fastener to enter by silicone gasket Row sealing.
4. photoelectrocatalysis reaction experiment device as claimed in claim 1, it is characterised in that:
Wherein, the intake section is air inlet pipe,
One end of the air inlet pipe is stretched into the chamber and is extended downwardly,
The air inlet pipe is 6mm with the external diameter of the exhaust portion.
5. photoelectrocatalysis reaction experiment device as claimed in claim 4, it is characterised in that:
Wherein, the reference electrode mouth, to being provided with polytetrafluoroethylsealed sealed packing ring on electrode ports, working electrode mouth.
6. photoelectrocatalysis reaction experiment device as claimed in claim 1, it is characterised in that:
Wherein, described that platinum electrode is adopted to electrode, the reference electrode is using silver or silver chloride electrode.
7. photoelectrocatalysis reaction experiment device as claimed in claim 1, it is characterised in that:
Wherein, the reference electrode mouth, the external diameter to electrode ports, working electrode mouth are 10mm.
CN201611001326.1A 2016-11-11 2016-11-11 A kind of photoelectrocatalysis reaction experiment device Pending CN106556637A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107366004A (en) * 2017-07-06 2017-11-21 中山大学 A kind of stainless steel optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas
CN109999743A (en) * 2019-04-22 2019-07-12 西安交通大学 A kind of experimental provision and experimental method of electrical enhanced photocatalysis carbon dioxide methanol

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CN2550615Y (en) * 2002-07-05 2003-05-14 陈阵 Steel-plastic composite pipe with protective device at end
CN1795534A (en) * 2003-03-31 2006-06-28 兰姆研究有限公司 Wafer clamping apparatus and method for operating the same
CN1982204A (en) * 2005-12-14 2007-06-20 湖南大学 Production of hydrogen by catalyzed decomposing magnesium and its mixture doped with other metals
CN201634417U (en) * 2009-09-14 2010-11-17 昆明理工大学 Multi-stage hydrogen producing device
CN101900710A (en) * 2010-07-07 2010-12-01 哈尔滨工业大学 Multi-channel reaction simple device for evaluating hydrogen production performance of photocatalyst and method adopting same for carrying out hydrogen production performance evaluation
CN102939486A (en) * 2010-04-30 2013-02-20 费希尔控制国际公司 Ball valve seal with dynamic c-seal and static c-seal
CN103529110A (en) * 2013-10-11 2014-01-22 南京大学 Photoinduced electrochemical photocurrent detection device
CN104437303A (en) * 2014-12-01 2015-03-25 上海师范大学 Photoelectrocatalysis reduction reaction device capable of operating under multi-factor variant condition
CN104498984A (en) * 2014-12-15 2015-04-08 天津大学 Photoelectric-catalytic water splitting hydrogen generation reaction analysis-detection system and application method of system
CN104711627A (en) * 2013-12-13 2015-06-17 中国科学院大连化学物理研究所 Method for preparing hydrogen through photoanode-photovoltaic battery coupled dual-illumination fully-photic-driven decomposition of water

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2550615Y (en) * 2002-07-05 2003-05-14 陈阵 Steel-plastic composite pipe with protective device at end
CN1795534A (en) * 2003-03-31 2006-06-28 兰姆研究有限公司 Wafer clamping apparatus and method for operating the same
CN1982204A (en) * 2005-12-14 2007-06-20 湖南大学 Production of hydrogen by catalyzed decomposing magnesium and its mixture doped with other metals
CN201634417U (en) * 2009-09-14 2010-11-17 昆明理工大学 Multi-stage hydrogen producing device
CN102939486A (en) * 2010-04-30 2013-02-20 费希尔控制国际公司 Ball valve seal with dynamic c-seal and static c-seal
CN101900710A (en) * 2010-07-07 2010-12-01 哈尔滨工业大学 Multi-channel reaction simple device for evaluating hydrogen production performance of photocatalyst and method adopting same for carrying out hydrogen production performance evaluation
CN103529110A (en) * 2013-10-11 2014-01-22 南京大学 Photoinduced electrochemical photocurrent detection device
CN104711627A (en) * 2013-12-13 2015-06-17 中国科学院大连化学物理研究所 Method for preparing hydrogen through photoanode-photovoltaic battery coupled dual-illumination fully-photic-driven decomposition of water
CN104437303A (en) * 2014-12-01 2015-03-25 上海师范大学 Photoelectrocatalysis reduction reaction device capable of operating under multi-factor variant condition
CN104498984A (en) * 2014-12-15 2015-04-08 天津大学 Photoelectric-catalytic water splitting hydrogen generation reaction analysis-detection system and application method of system

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107366004A (en) * 2017-07-06 2017-11-21 中山大学 A kind of stainless steel optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas
CN107366004B (en) * 2017-07-06 2023-09-26 中山大学 Stainless steel photoelectrochemical reaction device with gas on-line and off-line analysis functions
CN109999743A (en) * 2019-04-22 2019-07-12 西安交通大学 A kind of experimental provision and experimental method of electrical enhanced photocatalysis carbon dioxide methanol
CN109999743B (en) * 2019-04-22 2024-04-09 西安交通大学 Experimental device and experimental method for preparing methanol by photoelectrically and cooperatively catalyzing carbon dioxide

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Application publication date: 20170405