CN207091513U - A kind of stainless steel optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas - Google Patents
A kind of stainless steel optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas Download PDFInfo
- Publication number
- CN207091513U CN207091513U CN201720813070.8U CN201720813070U CN207091513U CN 207091513 U CN207091513 U CN 207091513U CN 201720813070 U CN201720813070 U CN 201720813070U CN 207091513 U CN207091513 U CN 207091513U
- Authority
- CN
- China
- Prior art keywords
- gas
- flange
- optical electro
- chemistry
- reaction chamber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 121
- 230000003287 optical effect Effects 0.000 title claims abstract description 58
- 230000005518 electrochemistry Effects 0.000 title claims abstract description 52
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 29
- 239000010935 stainless steel Substances 0.000 title claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000001816 cooling Methods 0.000 claims abstract description 23
- 238000004817 gas chromatography Methods 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims description 16
- 238000004458 analytical method Methods 0.000 claims description 15
- 238000005070 sampling Methods 0.000 claims description 13
- 238000005520 cutting process Methods 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 3
- 238000006073 displacement reaction Methods 0.000 claims description 2
- 238000003487 electrochemical reaction Methods 0.000 claims 1
- 239000000376 reactant Substances 0.000 claims 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 16
- 239000001569 carbon dioxide Substances 0.000 abstract description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 8
- 230000009467 reduction Effects 0.000 abstract description 5
- 238000011160 research Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 66
- 239000001257 hydrogen Substances 0.000 description 19
- 229910052739 hydrogen Inorganic materials 0.000 description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 18
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 238000005259 measurement Methods 0.000 description 7
- 230000005693 optoelectronics Effects 0.000 description 7
- 238000006467 substitution reaction Methods 0.000 description 7
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 230000005611 electricity Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000000498 cooling water Substances 0.000 description 5
- 230000005622 photoelectricity Effects 0.000 description 5
- 229910052697 platinum Inorganic materials 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- 239000007832 Na2SO4 Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000013401 experimental design Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000036647 reaction Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Landscapes
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The utility model discloses a kind of optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas.The core texture of the device includes main reaction chamber, gas circulation loop and circulating water cooling system, is made of stainless steel, and has good air-tightness, temperature-controllable, advantage compact-sized, scalability is strong.And the device can be compatible with commercialization gas-chromatography, the online and offline analytic function of gas componant is provided simultaneously with, is expected to be widely used in the scientific research of optical electro-chemistry splitting water, carbon dioxide reduction etc..
Description
Technical field
The invention belongs to chemical reaction equipment technical field.More particularly, to one kind be provided simultaneously with gas it is online and from
The new type stainless steel. corrosion resistance optical electro-chemistry reaction unit of line analysis function.
Background technology
As the high speed development of society, people are increasing to energy demand.The non-renewable mineral energy such as oil, natural gas
The reserves in source are limited, one day can be exhausted with the continuous exploitation and consumption of the mankind.In addition, these fossil energies
Use can produce great amount of carbon dioxide gas, cause greenhouse effects, and a large amount of pernicious gases discharged, can cause serious
Environmental pollution.Therefore, it is most important and urgent to develop sustainable development of the new clean reproducible energy for human society
It is too late to treat.
The sun is the main source of earth energy.The energy that each second reaches the earth is about 1.73 × 1017Watt, it is complete
Mankind institute consumed energy（14 TW terawatts, 1.4 × 1013Watt）More than 10,000 times.Although the energy of solar energy is very huge, between existing
The adverse effect of having a rest property and unpredictability.It is effectively to utilize the sun to convert solar energy into storable renewable and clean energy resource
One of important channel of energy.Hydrogen is a kind of clean energy resource with heats of combustion value, and the exclusive product after burning is water.1972
Year, Fujishima and Honda et al. had found that water-splitting can be hydrogen and oxygen under sunshine irradiation by titanium dioxide photo anode.
Since since then, more and more scientists put into semiconductor photoelectrode in splitting water by energy is studied（Or carbon dioxide reduction）This
One scientific domain.Solar energy can be effectively utilized come light/photoelectricity splitting water production hydrogen using sunshine, to solve social development institute
The energy demand brought and problem of environmental pollution provide an effective way.
Measure product composition and content in depth studying photoelectrochemical behaviour and the light-change of semiconductor photoelectrode
Transformation efficiency is essential.The product of optical electro-chemistry splitting water is hydrogen and oxygen, and the production of carbon dioxide reduction
Thing is mostly the fuel gas small molecule such as carbon monoxide, methane.Therefore, gas-chromatography is widely used in optical electro-chemistry reaction production
The detection of thing.It is very for the characteristic for studying semiconductor photoelectrode organically to combine Conventional electrochemical electrolytic cell and gas-chromatography
Important.At present, it is domestic just like the fewer companies production and supply correlation optical electro-chemistry reaction such as luxuriant and rich with fragrance Lay (PerfectLight) of pool
System.However, the optical electro-chemistry reaction system of most commercializations at present is made using optical glass.In order to realize
Gas componant on-line analysis, gas-chromatography usually require to be connected with electrolytic cell by a set of complicated glass sampling pipe.For
Expensive, frangible, complicated, processing difficulties, poor expandability, maintenance process be present in the glass pipe of gas on-line analysis
The shortcomings of complicated, air-tightness is difficult to ensure that.In addition, glass pipe and the stainless steel pipes Joining Technology of gas-chromatography are relative multiple
It is miscellaneous.
The content of the invention
The technical problem to be solved in the present invention is the defects of overcoming above-mentioned prior art and deficiency, there is provided a kind of air-tightness
Good, temperature-controllable, compact-sized, function expansibility is strong, processing cost is low, easy to maintain, and can be with commercialization gas-chromatography
Compatibility, it is provided simultaneously with the new type stainless steel. corrosion resistance optical electro-chemistry reaction unit of the online and offline analytic function of gas componant.This device
Be expected to optical electro-chemistry splitting water, carbon dioxide reduction scientific research in be widely used.
It is an object of the invention to provide a kind of stainless steel optical electro-chemistry for being provided simultaneously with the online and offline analytic function of gas
Reaction unit.
Above-mentioned purpose of the present invention is achieved through the following technical solutions：
A kind of optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas, mainly by main reaction chamber
Room, gas circulation loop and circulating water cooling system composition（As shown in Figure 1）.
Specifically, each part composition is as follows：
（1）Main reaction chamber：Main structure is a cavity room of stainless steel 9, and two flanges distinguish portion and bottom disposed thereon,
Other 6 flanges are located in the middle part of main reaction chamber and are welded in 60 degree of distributions, a cutting ferrule in the middle part of chamber；One optical window
It is connected by the flange on main reaction chamber top with main reaction chamber；One optical electro-chemistry electrolytic cell for possessing three-electrode system leads to
The flange seal of main reaction chamber lower portion is crossed in main reaction intracavitary（Whole optical electro-chemistry electrolytic cell is sealed in main reaction chamber）；
Air gauge is also associated with main reaction chamber, is also respectively provided with and electrochemical electrode, thermocouple, micro air pump（Vavuum pump）Even
The electrode ports connect.In testing, light is radiated on optoelectronic pole from top to down by the optical window on top.
（2）Gas circulation loop：By the micro air pump chamber, the six-way valve that pass sequentially through stainless steel tube connection
Door, a quantitative sampling ring and a flange composition；Gas circulation loop both ends are connected with reality by flange with main reaction chamber
The now circulation of whole reaction unit internal gas；, can be efficiently by the photoelectricity in main reaction chamber by gas circulation loop
Gas caused by chemical reaction is transported to quantitative sampling ring and gas-chromatography, realizes gas on-line analysis function, improves detection
Accuracy and reliability.
（3）Circulating water cooling system：By a stainless steel water inlet pipe and a stainless steel outlet pipe, and an open circles
Disk forms；Circulating water cooling system is connected by the flange of main reaction chamber lower portion with main reaction chamber, and hollow disk is fixed on master
In reaction chamber, and thermally contacted with optical electro-chemistry electrolytic cell.Recirculated water is successively after stainless steel water inlet pipe reaches hollow disk
Flowed out by outlet pipe.Stainless steel water inlet pipe and outlet pipe are welded on a blind plate, and hollow disk is sealed in into master to realize
In reaction chamber.Solution heating and the thermal evaporation caused by long-time illumination can be effectively avoided by circulating water cooling system.
In the device, main reaction chamber upper flange is used to connect optical window, realizes light and is radiated at work from top to down
Make on electrode；Main reaction chamber lower portion flange is used to connect circulating water cooling system, realizes the temperature control to electrolytic cell.
In addition, in 6 flanges in the middle part of main reaction chamber, one of flange, which is used to connecting one, has 3 electricity
The blind plate of extreme mouth, for connecting the working electrode of three-electrode system, to electrode and reference electrode.
In 6 flanges in the middle part of main reaction chamber, one of flange, which is used for connection one, has 2 electrode ports
Blind plate, detect the temperature of solution for one thermocouple of connection.
The stainless steel water inlet pipe and stainless steel outlet pipe of circulating water cooling system are welded on a blind plate.
In 6 flanges in the middle part of main reaction chamber, two of which flange is used to connect gas circulation loop, realizes gas
Body on-line analysis function.
In 6 flanges in the middle part of main reaction chamber, one of flange is used to connect air gauge, to monitor main reaction
Air pressure in chamber.
In 6 flanges in the middle part of main reaction chamber, one of flange is used to connect vavuum pump.
Use a micro air pump in gas circulation loop, promote circulation of the gas inside reaction unit and can be effective
Ground reaches quantitative sampling ring.
In order to realize gas off-line analysis, a cutting ferrule has been welded in the middle part of main reaction chamber.The effect of cutting ferrule is to be used to fix
Sampling pad.By the sampling pad, directly it can take out gas from main reaction chamber using sampling probe and be expelled to gas-chromatography and realize gas
The off-line analysis of body composition.
Walked using the performance of Photoelectrochemicaldevice device research optoelectronic pole and the concrete operations of gas composition analysis of the present invention
It is rapid as follows：
（1）Being fixed electrolytic cell with circulating water cooling device with screw makes to thermally contact between it.
（2）By electrode terminal by the optoelectronic pole of electrolytic cell, to electrode and reference electrode and the electrochemistry outside main reaction chamber
Work station connects.
（3）It is by main reaction chamber lower portion flange that electrolytic cell and circulating water cooling device is close after electrode connects
It is encapsulated in main reaction chamber, ON cycle chilled water unit.
（4）The switching switch of six-way valve on rotary gas circulation loop so that gasometry samples ring and main reaction chamber
Room connects.
（5）Open vavuum pump and be filled with substitution gas and the air of optical electro-chemistry reaction unit intracavitary is thoroughly replaced into argon gas
Deng reacting gas such as inert gas or carbon dioxide.Vavuum pump and substitution gas are closed after completing the process.
（6）Micro air pump is opened, and keeps it to run always during the course of the reaction.
（7）Electrochemical workstation and light source are opened, starts optical electro-chemistry reaction.According to experimental design timing rotation six-way valve
Quantitative sampling ring is connected to detect the composition and content of produced gas in course of reaction with gas-chromatography.So repeatedly, directly
Untill the reaction of whole optical electro-chemistry is completed.
（8）Open main reaction chamber and take out photovoltaic reaction electrolytic cell, close micro air pump and recirculated cooling water device.
The invention has the advantages that：
The optical electro-chemistry reaction unit of the present invention is provided simultaneously with the online and offline analytic function of gas, is followed by using gas
Loop back path realizes gas on-line analysis；Meanwhile circulating water cooling system significantly avoid as molten caused by long-time illumination
The adverse effect such as liquid heating and evaporation.The applicable air pressure range of this optical electro-chemistry reaction unit is 10-3Pa to 3 × 105Pa, can
Applied to 10-3 Pa to 3x105 Optical electro-chemistry reaction under Pa air pressure.
Preparation technology of the invention based on stainless-steel vacuum/high-pressure chamber, having made one can be with commercialization gas-chromatography
Compatible optical electro-chemistry reaction unit, this device has good air-tightness, temperature-controllable, compact-sized, autgmentability is strong, processing cost
The advantages that low, easy to maintain, it is expected to be widely used in semiconductor photoelectrode in splitting water, the research of carbon dioxide reduction.
Brief description of the drawings
Fig. 1 is the integrally-built vertical view of optical electro-chemistry reaction unit that the present invention can be achieved to be connected with commercialization gas-chromatography
Figure.1-main reaction chamber, 2-gas circulation loop, 3-air gauge, the electrode ports for 4-1-be connected with electrochemical electrode, 4-
2-the electrode ports that are connected with thermocouple, the electrode ports for 4-3-be connected with micro air pump, 5-six-way valve, 6-quantitative
Compression ring, 7-micro air pump chamber, 8-substitution gas entrance, 9-cutting ferrule, 10-optical electro-chemistry electrolytic cell, 11-recirculated water cooling
But hollow disk, the dotted arrow in figure indicate gas in the flow direction of circulation loop.
Fig. 2 be without recirculated cooling water and in the case of having recirculated cooling water, solution temperature with light application time change.
Fig. 3 is the relation of the hydrogen peak area and electricity obtained using gas chromatographic measurement, and compares micro air pump
Run (a) and close the influence of (b) to measurement accuracy.
Fig. 4 is to use WO3The amount of hydrogen producing changes with time relation when carrying out photoelectricity splitting water as light anode.
Embodiment
The present invention is further illustrated below in conjunction with Figure of description and specific embodiment, but embodiment is not to the present invention
Limit in any form.Unless stated otherwise, the reagent of the invention used, method and apparatus routinely try for the art
Agent, method and apparatus.
Unless stated otherwise, following examples agents useful for same and material are purchased in market.
Embodiment 1
1st, a kind of optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas, mainly by main reaction chamber
Room, gas circulation loop and circulating water cooling system composition（As shown in Figure 1）.Flow direction of the gas in reaction unit is as schemed
Shown in 1 dotted arrow.
Specifically, each part composition of the device is as follows：
（1）Main reaction chamber：Main structure is a cavity room of stainless steel 9, and 2 flanges distinguish portion and bottom disposed thereon, 6
Individual flange is located in the middle part of main reaction chamber and is welded in 60 degree of distributions, 1 cutting ferrule in the middle part of chamber.One optical window passes through master
The flange on reaction chamber top is connected with main reaction chamber.One optical electro-chemistry electrolytic cell with three-electrode system is sealed in master
In reaction chamber.In testing, light is radiated on optoelectronic pole from top to down by the optical window on top.
（2）Gas circulation loop：By the micro air pump chamber, the six-way valve that pass sequentially through stainless steel tube connection
Door, a quantitative compression ring and a flange composition；Substitution gas entrance is provided with micro air pump chamber；Gas circulation loop
Both ends are connected the circulation for realizing whole reaction unit internal gas by flange with main reaction chamber.By gas circulation loop,
The gas of the optical electro-chemistry reaction generation in main reaction chamber can be transported to quantitative sampling ring and gas-chromatography, realize that gas exists
Line analysis function.
（3）Circulating water cooling system：By a stainless steel water inlet pipe and a stainless steel outlet pipe, and an open circles
Disk forms；Circulating water cooling system is connected by the flange of main reaction chamber lower portion with main reaction chamber, and hollow disk is fixed on master
In reaction chamber, and thermally contacted with optical electro-chemistry electrolytic cell.Recirculated water is successively after stainless steel water inlet pipe reaches hollow disk
Flowed out by outlet pipe.Stainless steel water inlet pipe and outlet pipe are welded on a blind plate.
In the device, main reaction chamber upper flange is used to connect optical window, realizes light and is radiated at work from top to down
Make on electrode；Main reaction chamber lower portion flange is used to connect circulating water cooling system, realizes the temperature control to electrolytic cell.
In addition, the effect of 6 flanges in the middle part of main reaction chamber is as follows：
One flange is used to connect a blind plate with 3 electrode ports, for connecting the work of three-electrode system
Electrode, to electrode and reference electrode.
One flange is used to connect a blind plate with 2 electrode ports, for connecting a thermocouple to detect
The temperature of solution.
The stainless steel water inlet pipe and stainless steel outlet pipe of circulating water cooling system are welded on a blind plate.
Two flanges are used to connect gas circulation loop, realize gas on-line analysis function.
One flange is used to connect air gauge, to monitor the air pressure in main reaction chamber.
One flange is used to connect vavuum pump.
In addition, the cutting ferrule is used to install sampling pad on main reaction chamber, the function of gas off-line analysis is realized.
2nd, the performance of optoelectronic pole and the concrete operations of gas composition analysis are studied using the Photoelectrochemicaldevice device of the present invention
Step is as follows：
（1）Being fixed electrolytic cell with circulating water cooling device with screw makes to thermally contact between it.
（2）By electrode terminal by the optoelectronic pole of electrolytic cell, to electrode and reference electrode and the electrochemistry outside main reaction chamber
Work station connects.
（3）After electrode connects, by the flange of main reaction chamber lower portion, by electrolytic cell and circulating water cooling device
It is sealed in main reaction chamber.
（4）The switching switch of six-way valve on rotary gas circulation loop so that gasometry ring connects with main reaction chamber
It is logical.
（5）Open vavuum pump and be filled with substitution gas, the air of optical electro-chemistry reaction unit intracavitary is thoroughly replaced into argon
The inert gases such as gas or such as carbon dioxide reacting gas.Vavuum pump and substitution gas are closed after completing the process.
（6）Micro air pump is opened, and keeps it to run always during the course of the reaction.
（7）Electrochemical workstation and light source are opened, starts optical electro-chemistry reaction.It is logical according to experimental design timing rotation six
Valve, quantitative loop is connected to detect the composition and content of produced gas in course of reaction with gas-chromatography.So repeatedly, until
Untill whole optical electro-chemistry reaction is completed.
（8）Open main reaction chamber and take out photovoltaic reaction electrolytic cell, close micro air pump and recirculated cooling water device.
The effect of the circulating water cooling device of embodiment 2
, it is necessary to irradiate optoelectronic pole using powerful light source in optical electro-chemistry course of reaction.Caused by illumination
Solution heating can bring following several detrimental effects：
1) temperature of optical electro-chemistry reaction changes with light application time；
2) solution because of heating rapid evaporation so that solution concentration find significant change；
3) water of evaporation condenses on optical window, changes the intensity of illumination.
By using a thermocouple, the temperature of solution in electrolytic cell can be measured with the change of light application time.Such as Fig. 2 institutes
Show, after irradiation 140 minutes, the temperature of solution is increased to 33.2 DEG C from 20 DEG C.Meanwhile the solution in electrolytic cell reduces about
2 ml （About the 10% of original solution）.
In order to solve this problem, apparatus of the present invention are equipped with circulating water cooling device, can make in optical electro-chemistry electrolytic cell
The temperature of solution is basicly stable.By using 20 DEG C of recirculated cooling water, the temperature stabilization of solution is at 21 DEG C, and not in light
Learn window and main reaction cavity wall observes the globule of condensation.
Embodiment 3 demarcates the amount of hydrogen and the relation of the hydrogen peak area of gas chromatographic measurement
1st, experimental method
（1）By 20 ml 0.1 mol/L Na2SO4Solution is poured into electrolytic cell.Use a diameter of 0.5 mm platinum
Silk is used as working electrode, and the platinized platinum of a large area is used as to electrode and an Ag/AgCl/Cl-As reference electrode.When three
After electrode is connected with electrode terminal, electrolytic cell is sealed in main reaction intracavitary.
（2）Rotate the switching switch of six-way valve so that quantitative sampling ring is connected with main reaction chamber.
（3）Open vavuum pump and be filled with argon gas and inside reactor gas is thoroughly replaced.Closed after the completion of displacement true
Empty pump and substitution gas.
（4）Micro air pump is opened, and keeps it to run always during the course of the reaction.
（5）Electrochemical workstation is opened, by the control of Electric potentials of platinum filament (working electrode) in -1.2 V (relative to Ag/
AgCl).When the electricity passed through is 0.1 coulomb, stops at and apply voltage on platinum filament.
（6）Rotate the switching switch of six-way valve so that quantitative loop is connected with gas-chromatography, and the gas in quantitative loop is passed
It is defeated to arrive gas-chromatography, the peak area of hydrogen produced by obtaining cell reaction.
（7）Such repeat step 5 and 6, obtains hydrogen peak area and the relation by electricity and the amount of hydrogen.
2nd, as shown in Figure 3, the hydrogen peak area that gas chromatographic detection obtains and the electricity passed through are linear.Pass through this
The slope of individual linear relationship, the magnitude relation that can demarcate hydrogen peak area and hydrogen is 13650/mol.If in addition, measuring
During close micro air pump, the amount of the gas of measurement is substantially lower than in reaction chamber amounts of hydrogen caused by reality
And cause great experimental error.Therefore, the present invention installs a micro air pump promotion reaction unit in gas circulation loop
The circulation of middle gas, this is very important for the accuracy of measurement.
Embodiment 4 studies application of the tungstic acid light anode in optical electro-chemistry splitting water hydrogen producing
Tungstic acid is the direct band-gap semicondictor that an energy gap is 2.7 eV, can absorb ultraviolet light and partially visible
Light.The fast light corrosive power of tungstic acid is strong, is a preferable light anode material.Reacted by using optical electro-chemistry of the present invention
Device, measurement tungstic acid light anode produce the speed and faradic efficiency of hydrogen during photoelectricity splitting water.
In optical electro-chemistry measurement, tungstic acid is used as to electrode as working electrode, platinum filament, and Ag/AgCl is as reference
Electrode.0.1 mol/l Na2SO4As electrolyte.Light is radiated on tungstic acid by optical window.Circulating water fills
Put and the temperature of solution is maintained 20 DEG C.By electrochemical workstation by the control of Electric potentials of tungstic acid in 1.2 V.Then, often
After reaction 1000 seconds, the amount of produced hydrogen is measured by the switching switch for rotating six-way valve.In gasmetry process
In, the reaction of photoelectricity splitting water persistently carries out interrupting.
Repeat operation, it is 1.1 that can accurately measure to obtain hydrogen output with the relation of time and the electricity passed through
mol/cm2/ h and faradic efficiency are 65%（As shown in Figure 4）.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas, it is characterised in that by main anti-
Answer chamber, gas circulation loop and circulating water cooling system composition；Each part composition is as follows：
Main reaction chamber：Main structure is a cavity room of stainless steel 9, and two flanges distinguish portion and bottom disposed thereon, 6 in addition
Flange is located in the middle part of the chamber and is welded in 60 degree of distributions, a cutting ferrule in the middle part of main chamber；One optical window passes through main anti-
The flange on chamber top is answered to be connected with main reaction chamber, an optical electro-chemistry electrolytic cell for possessing three-electrode system passes through main reaction
The flange seal of chamber lower portion is in main reaction intracavitary；
Gas circulation loop：By pass sequentially through a micro air pump chamber of stainless steel tube connection, a six-way valve, one it is fixed
Measure sample ring and a flange composition；The both ends of gas circulation loop are connected whole anti-to realize by flange with main reaction chamber
Answer the circulation of device internal gas；
Circulating water cooling system：By a stainless steel water inlet pipe and a stainless steel outlet pipe, and a hollow disk composition；
Circulating water cooling system is connected by the flange of main reaction chamber lower portion with main reaction chamber, and hollow disk is fixed on main reaction chamber
It is interior, and thermally contacted with optical electro-chemistry electrolytic cell.
2. optical electro-chemistry reaction unit according to claim 1, it is characterised in that it is fabricated by stainless steel, and device
Can be compatible with commercialization gas-chromatography, be provided simultaneously with gas componant online with off-line analysis function.
3. optical electro-chemistry reaction unit according to claim 1, it is characterised in that displacement is provided with micro air pump chamber
Gas access.
4. optical electro-chemistry reaction unit according to claim 1, it is characterised in that 6 in the middle part of main reaction chamber
In flange, one of flange is used to connect a blind plate with 3 electrode ports, for connecting optical electro-chemistry reactant
The working electrode of system, to electrode and reference electrode.
5. optical electro-chemistry reaction unit according to claim 1, it is characterised in that 6 in the middle part of main reaction chamber
In flange, one of flange is used to connect a blind plate with 2 electrode ports, for connecting a thermocouple to examine
Survey the temperature of solution.
6. optical electro-chemistry reaction unit according to claim 1, it is characterised in that 6 in the middle part of main reaction chamber
In flange, two of which flange is used to connect gas circulation loop.
7. optical electro-chemistry reaction unit according to claim 1, it is characterised in that 6 in the middle part of main reaction chamber
In flange, one of flange is used to connect air gauge.
8. optical electro-chemistry reaction unit according to claim 1, it is characterised in that 6 in the middle part of main reaction chamber
In flange, one of flange is used to connect vavuum pump.
9. optical electro-chemistry reaction unit according to claim 1, it is characterised in that the cutting ferrule is used to install sampling pad,
Realize the function of gas off-line analysis.
10. electrochemical reaction appts according to claim 1, it is characterised in that one is used in gas circulation loop
Micro air pump, promote circulation of the gas inside reaction unit and quantitative sampling ring can be effectively achieved.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720813070.8U CN207091513U (en) | 2017-07-06 | 2017-07-06 | A kind of stainless steel optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720813070.8U CN207091513U (en) | 2017-07-06 | 2017-07-06 | A kind of stainless steel optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN207091513U true CN207091513U (en) | 2018-03-13 |
Family
ID=61555808
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201720813070.8U Expired - Fee Related CN207091513U (en) | 2017-07-06 | 2017-07-06 | A kind of stainless steel optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN207091513U (en) |
Cited By (1)
| 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 |
-
2017
- 2017-07-06 CN CN201720813070.8U patent/CN207091513U/en not_active Expired - Fee Related
Cited By (2)
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Xing et al. | On the engineering part of solar hydrogen production from water splitting: photoreactor design | |
| CN103175876B (en) | Spectroelectrochemical in-situ pool and application thereof | |
| CN101586245A (en) | Hydrogen generating reactor, system and gas collection method, light-hydrogen energy conversion efficiency measuring system, and light-hydrogen energy / light-electricity conversion efficiency measuri | |
| CN107046139B (en) | A kind of nitrating carbon material and its preparation method and application based on metal organic framework | |
| CN107138111A (en) | A kind of carbon dioxide catalytic reduction reaction device | |
| CN112285173B (en) | Method and related device for optical/electrochemical in-situ Raman detection | |
| CN107366004A (en) | A kind of stainless steel optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas | |
| CN109112562A (en) | A kind of construction method of the photoelectro catalytic system of thermoelectricity auxiliary | |
| CN109507255A (en) | A kind of Preparation method and use of bismuth/carbonitride photoelectric material | |
| CN207091513U (en) | A kind of stainless steel optical electro-chemistry reaction unit for being provided simultaneously with the online and offline analytic function of gas | |
| CN116446000A (en) | Preparation method of palladium-copper-nickel catalytic material for hydrogen production by formic acid, component and system for hydrogen production by formic acid with photo-thermal interface | |
| CN110013763A (en) | A kind of device of carbon dioxide by photoelectric catalytic reduction | |
| Zhang et al. | Boosting solar-driven thermal-assisted photocatalytic hydrogen production through device thermal management | |
| CN114280026B (en) | In-situ Raman detection device and method for gas diffusion electrode | |
| Xiao et al. | Solar fuel production from CO2 reduction in a self-biased hybrid solar-microbial device | |
| CN109580732A (en) | A kind of universal three-electrode cell of the photoelectricity that system temperature is controllable | |
| CN110004456A (en) | A kind of photoelectrocatalysis complete solution water installations integrating carbon-based plane perovskite solar cell | |
| CN107084919A (en) | A kind of preparation method of metallic bipolar plate materials decay resistance test reference electrode | |
| CN108311131A (en) | A kind of alundum (Al2O3) ultrathin membrane passivation titanic oxide nanorod array composite material and preparation method | |
| CN105651839B (en) | Three electrode reactors and its application | |
| CN216117447U (en) | Electrolytic cell for photoelectrochemical analysis test and photoelectrode preparation | |
| ES2315077B1 (en) | DIDACTIC DEMONSTRATOR OF THE HYDROGEN SOLAR CYCLE. | |
| CN215828878U (en) | Electrolytic cell device for electrodeposition and photoelectrochemical test | |
| CN105016389A (en) | Carbon shell-coated lead molybdate nanocrystal and preparation method thereof | |
| CN218989417U (en) | Device and equipment for enhancing reduction efficiency of graphene oxide by liquid flow electrochemical reduction method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180313 Termination date: 20190706 |