CN114405438B - Photoelectrocatalysis reaction system - Google Patents
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- CN114405438B CN114405438B CN202210200437.4A CN202210200437A CN114405438B CN 114405438 B CN114405438 B CN 114405438B CN 202210200437 A CN202210200437 A CN 202210200437A CN 114405438 B CN114405438 B CN 114405438B
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Abstract
The invention relates to the technical field of photoelectrocatalysis, in particular to a photoelectrocatalysis reaction system which comprises a cathode reactor and an anode reactor, wherein an air inlet of the cathode reactor is sequentially connected with a first air pump and a first air storage device used for providing reaction gas for the first air pump, and an air outlet of the cathode reactor is connected with a first back pressure valve; the air inlet of anode reactor has connected gradually the second air pump and is used for providing inert gas's second gas storage device to the second air pump, the gas outlet of anode reactor is connected with the second back pressure valve, the setting up of first back pressure valve and second back pressure valve can make cathode reactor and the inside even unanimity of pressure of anode reactor, thereby make the interior reaction gas's of cathode reactor solubility keep steady state, and then guaranteed that photoelectrocatalysis efficiency's stability is controlled, stable pressure also has decisive influence to gas chromatography test's stability and reproducibility in addition, the accurate assessment requirement to photoelectrocatalysis reaction efficiency has been satisfied.
Description
Technical Field
The invention relates to the technical field of photoelectrocatalysis, in particular to a photoelectrocatalysis reaction system.
Background
The photoelectrocatalysis technology takes clean solar energy as a driving force, efficiently carries out catalytic reaction under mild conditions (near atmospheric pressure and ambient temperature), and has important application in the fields of producing high value-added chemicals, decomposing harmful pollutants and the like. Compared with a photocatalytic technology, reduction and oxidation reactions are separated in space in the process of photoelectrocatalysis, so that a photon-generated carrier in a semiconductor photoelectrocatalysis material is prevented from being compounded on the surface of a photocatalyst; compared with an electro-catalysis technology, the photoelectrocatalysis directly converts light energy into chemical energy, and energy loss caused by multi-step conversion of solar energy, electric energy and chemical energy in an electro-catalysis process is avoided, so that the solar energy utilization efficiency of the photoelectrocatalysis technology is higher in theory.
Ammonia gas is an important basic chemical and has important application in the fields of clean fuel, nitrogen fertilizer production, protein synthesis and the like. At present, the main preparation method of ammonia gas is the habo method, high-temperature and high-pressure reaction conditions are needed, and hydrogen required by ammonia synthesis by the habo method is mainly prepared by a water-vapor conversion reaction or a natural gas reforming method, and is 'ash hydrogen' with high energy consumption and heavy carbon emission. Therefore, the habo method ammonia synthesis process does not meet the requirement of the current international society for realizing the goals of carbon neutralization and carbon peak reaching. The application of the photoelectrocatalysis technology to the synthesis of ammonia is a novel technology with extremely high potential, low energy consumption and zero carbon emission. The photoelectrocatalysis ammonia synthesis process is carried out under mild conditions, nitrogen and water are used as raw materials to synthesize ammonia, and a byproduct is only oxygen, so that the photoelectrocatalysis ammonia synthesis process completely meets the requirements of the targets of carbon neutralization and carbon peak reaching at present.
At present, nitrogen is injected into a cathode reactor through an air pump during photoelectrocatalysis ammonia synthesis, the nitrogen is dissolved in electrolyte in the cathode reactor and then adsorbed on a working electrode immersed in the electrolyte, and a light source is turned on to irradiate the working electrode, so that ammonium ions dissolved in the electrolyte are generated. However, the nitrogen flowing out from the air pump has a pulsation phenomenon, the pulsation phenomenon can cause the pressure change in the cathode reactor, and further cause the solubility of the nitrogen in the electrolyte to fluctuate, and the solubility fluctuation can cause the adsorption concentration of the nitrogen on the surface of the photoelectrode to change, so that the photoelectrocatalysis reaction efficiency is not controlled, and the photoelectrocatalysis reaction efficiency cannot be accurately evaluated.
Disclosure of Invention
The invention aims to provide a photoelectrocatalysis reaction system, and the technical problem to be solved by the invention is as follows: in the existing photoelectrocatalysis reaction system, the reaction gas is introduced into the cathode reactor through the air pump, and the pulsation phenomenon exists, so that the pressure in the cathode reactor is changed, and the photoelectrocatalysis reaction efficiency cannot be accurately evaluated.
In order to solve the technical problems, the invention provides a photoelectrocatalysis reaction system, which comprises a cathode reactor and an anode reactor, wherein an air inlet of the cathode reactor is sequentially connected with a first air pump and a first air storage device used for providing reaction gas for the first air pump, and an air outlet of the cathode reactor is connected with a first back pressure valve; the air inlet of the anode reactor is sequentially connected with a second air pump and a second air storage device used for providing inert gas for the second air pump, and the air outlet of the anode reactor is connected with a second back pressure valve.
Preferably, a first air washing and pressure stabilizing device is connected between the first air pump and the cathode reactor, and a second air washing and pressure stabilizing device is connected between the second air pump and the anode reactor.
Preferably, a first flow controller is connected between the first gas washing and pressure stabilizing device and the cathode reactor, and a second flow controller is connected between the second gas washing and pressure stabilizing device and the cathode reactor.
Preferably, the photoelectrocatalysis reaction system comprises a first airflow switching device, and the first airflow switching device is provided with a first port, a second port, a third port and a fourth port which can switch the communication state; the first port is communicated with the air outlet end of the first back pressure valve, the second port is communicated with the air inlet end of the first air pump, the air outlet of the first air storage device and the air outlet of the second air storage device are communicated with the third port, and the fourth port is connected with a first one-way valve for exhausting air;
switching the communication state of the first airflow switching device may enable the first port to communicate with the fourth port and the second port to communicate with the third port, or the first port to communicate with the second port and the third port to communicate with the fourth port.
As a preferred scheme, the photoelectrocatalysis reaction system further comprises a second gas flow switching device, the second gas flow switching device is provided with a fifth port, a sixth port, a seventh port and an eighth port which can be switched to be in a communication state, and a gas outlet of the second gas storage device is communicated with the fifth port;
the sixth port is communicated with the air inlet end of the second air pump, and the seventh port is communicated with the air outlet end of the second backpressure valve; the eighth port is connected with a second one-way valve for exhausting;
switching the communication state of the second airflow switching device may cause the fifth port to communicate with the sixth port and the seventh port to communicate with the eighth port, or the sixth port to communicate with the seventh port and the fifth port to communicate with the eighth port.
As a preferable scheme, the photoelectrocatalysis reaction system further comprises a gas detection system for detecting the content of generated gas and a third gas flow switching device, the gas detection system is provided with a first gas inlet pipe and a first gas outlet pipe, the third gas flow switching device is provided with a ninth port, a tenth port, an eleventh port and a twelfth port, the ninth port is communicated with a gas outlet of the cathode reactor, the tenth port is communicated with the first gas inlet pipe, the eleventh port is communicated with the first gas outlet pipe, and the twelfth port is communicated with a gas inlet end of the first back pressure valve;
switching the communication state of the third airflow switching device may cause the ninth port to communicate with the tenth port and the eleventh port to communicate with the twelfth port, or the ninth port to communicate with the twelfth port and the tenth port to communicate with the eleventh port.
As a preferred scheme, the gas detection system comprises a gas chromatograph, a sampling device and a third gas storage device for introducing inert gas into the sampling device;
the sampling device is provided with a first interface, a second interface, a third interface, a fourth interface, a fifth interface and a sixth interface which can switch the communication state, the first interface is communicated with the gas outlet of the third gas storage device, the second interface is connected with a first quantitative ring, the other end of the first quantitative ring is connected with the fifth interface, the third interface is communicated with the first gas inlet pipe, the fourth interface is communicated with the first gas outlet pipe, and the sixth interface is communicated with the gas inlet of the gas chromatograph;
the communication state of the sampling device is switched, so that the third interface, the second interface, the first quantitative ring, the fifth interface and the fourth interface are sequentially communicated, or the first interface, the second interface, the first quantitative ring, the fifth interface and the sixth interface are sequentially communicated.
Preferably, the photoelectrocatalysis reaction system comprises a fourth gas flow switching device, the fourth gas flow switching device is provided with a thirteenth port, a fourteenth port, a fifteenth port and a sixteenth port, the thirteenth port can switch the communication state, the thirteenth port is communicated with the gas inlet end of the second backpressure valve, and the fourteenth port is communicated with the gas outlet of the anode reactor;
the sampling device is also provided with a seventh interface, an eighth interface, a ninth interface and a tenth interface which can switch the communication state, the seventh interface is connected with a second quantitative ring, the other end of the second quantitative ring is connected with the tenth interface, the eighth interface is communicated with the sixteenth port, and the ninth interface is communicated with the fifteenth port;
switching the connection state of the sampling device to connect the ninth port, the tenth port, the second quantitative ring, the seventh port and the eighth port in sequence; or the first port, the tenth port, the second quantitative ring, the seventh port and the sixth port are communicated in sequence;
switching the communication state of the fourth airflow switching device may cause the thirteenth port to communicate with the sixteenth port and the fifteenth port to communicate with the fourteenth port, or the thirteenth port to communicate with the fourteenth port and the fifteenth port to communicate with the sixteenth port.
Preferably, a particle exchange membrane for preventing the generated gas in the cathode reactor from entering the anode reactor is interposed between the cathode reactor and the anode reactor.
Compared with the prior art, the invention has the beneficial effects that: according to the photoelectrocatalysis reaction system, the gas outlet of the cathode reactor is connected with the first back pressure valve, the gas outlet of the anode reactor is provided with the second back pressure valve, and the first back pressure valve and the second back pressure valve are arranged to enable the pressure inside the cathode reactor and the pressure inside the anode reactor to be uniform, so that the solubility of reaction gas in the cathode reactor is kept in a stable state, the photoelectrocatalysis efficiency is guaranteed to be stably controlled, and the accurate evaluation requirement on the photoelectrocatalysis reaction efficiency is met.
Drawings
FIG. 1 is a schematic structural diagram of a photoelectrocatalytic reaction system of the present invention;
FIG. 2 is a schematic, partially enlarged view of a first airflow switching device;
FIG. 3 is an enlarged view of a portion of the second airflow switching device;
FIG. 4 is an enlarged view of a portion of a third airflow switching device;
FIG. 5 is a schematic view of a fourth airflow switching device in a partially enlarged manner;
FIG. 6 is a schematic view of the sampling device in a first state;
FIG. 7 is an enlarged partial schematic view of the sampling device in a second state;
in the figure, 1, a cathode reactor; 2. an anode reactor; 3. a first air pump; 4. a first gas storage device; 5. a first back pressure valve; 6. a second air pump; 7. a second gas storage device; 8. a second back pressure valve; 9. a first gas washing pressure stabilizing device; 10. a second gas-washing pressure stabilizing device; 11. a first flow controller; 12. a second flow controller; 13. a first airflow switching device; 131. a first port; 132. a second port; 133. a third port; 134. a fourth port; 14. a second airflow switching device; 141. a fifth port; 142. a sixth port; 143. a seventh port; 144. an eighth port; 15. a first check valve; 16. a second one-way valve; 17. a third air flow switching device; 171. a ninth port; 172. a tenth port; 173. an eleventh port; 174. a twelfth port; 18. a first intake pipe; 19. a first outlet pipe; 20. a gas chromatograph; 21. a sampling device; 21-1, a first interface; 21-2, a second interface; 21-3, a third interface; 21-4, a fourth interface; 21-5, a fifth interface; 21-6 and a sixth interface; 21-7, a seventh interface; 21-8 and an eighth interface; 21-9 and a ninth interface; 21-10, tenth interface; 21-11, a first quantity of loops; 21-12, a second dosing ring; 22. a third gas storage device; 23. a fourth airflow switching device; 231. a thirteenth port; 232. a fourteenth port; 233. a fifteenth port; 234. a sixteenth port; 24. a second intake pipe; 25. a second air outlet pipe; 26. a fifth airflow switching device; 27. a first pressure reducing valve; 28. a first flow meter; 29. a second pressure reducing valve; 30. a second flow meter; 31. a gas washing bottle; 32. a first condenser pipe; 33. a second condenser pipe; 34. a third pressure reducing valve; 35. an electrochemical workstation.
Detailed Description
The following detailed description of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "left", "right", "top", "bottom", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the device or element referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. It should be understood that the terms "first", "second", etc. are used herein to describe various information, but the information should not be limited to these terms, which are only used to distinguish one type of information from another. For example, "first" information may also be referred to as "second" information, and similarly, "second" information may also be referred to as "first" information, without departing from the scope of the present invention.
As shown in fig. 1 to 7, a preferred embodiment of the photoelectrocatalysis reaction system of the present invention comprises a cathode reactor 1 and an anode reactor 2, wherein an air inlet of the cathode reactor 1 is sequentially connected with a first air pump 3 and a first air storage device 4 for providing reaction gas for the first air pump 3, and an air outlet of the cathode reactor 1 is connected with a first back pressure valve 5; the air inlet of the anode reactor 2 is sequentially connected with a second air pump 6 and a second air storage device 7 used for providing inert gas for the second air pump 6, and the air outlet of the anode reactor 2 is connected with a second backpressure valve 8. The arrangement of the first backpressure valve 5 and the second backpressure valve 8 can enable the pressure inside the cathode reactor 1 and the pressure inside the anode reactor 2 to be uniform, so that the solubility of reaction gas in the cathode reactor 1 is kept in a stable state, and the stability and the control of the photoelectrocatalysis efficiency are further ensured; on the other hand, when setting up gas chromatograph at the photoelectrocatalysis reaction system, stable pressure can guarantee that the volume of the gas volume of awaiting measuring and the pressure that get into the ration ring remain stable in the reactor to guarantee that the volume of the sample material that gets into gas chromatography is stable, above-mentioned two aspects help the system to realize the accurate aassessment requirement to photoelectrocatalysis reaction efficiency jointly.
Wherein, first air pump 3 with be connected with first washing gas voltage regulator device 9 between the cathode reaction ware 1, second air pump 6 with be connected with second washing gas voltage regulator device 10 between the anode reaction ware 2, it is specific, first washing gas voltage regulator device and second washing gas voltage regulator device are the surge tank in this embodiment, and the air inlet setting of surge tank is in the bottom of bottle inner chamber, and the gas outlet setting of surge tank is at the top of bottle inner chamber to realize the buffer memory to the air current that gets into in the surge tank, reduce the pulsation from first air pump 3 or the gas that second air pump 6 flows out, guarantee to let in the pressure stability of the gas in cathode reaction ware 1 and the anode reaction ware 2. Preferably, the acid liquid is contained in the pressure stabilizing bottle in the embodiment, an air inlet pipe and an air outlet pipe are hermetically inserted into the bottle mouth of the pressure stabilizing bottle, one end of the air inlet pipe, which is positioned outside the pressure stabilizing bottle, is communicated with the air outlet of the first air pump 3, and one end of the air inlet pipe, which is positioned inside the pressure stabilizing bottle, is inserted into the acid liquid; one end of the air outlet pipe, which is positioned in the pressure stabilizing bottle, is arranged above the liquid level of the acid liquid, and the other end of the air outlet pipe, which is positioned outside the pressure stabilizing bottle, is communicated with the air inlet of the cathode reactor; the arrangement of the acidic liquid not only can enable the pressure stabilizing function of the pressure stabilizing bottle to be better, but also can absorb soluble gas contained in the gas introduced into the cathode reactor, so as to avoid the soluble gas from polluting electrolyte in the cathode reactor; in other embodiments of the present invention, if the reaction atmosphere does not contain soluble gas pollutants, the first and second scrubber and pressure stabilizer devices 9 and 10 may be surge tanks or surge balloons.
In this embodiment, a first flow controller 11 is connected between the first gas washing and pressure stabilizing device 9 and the cathode reactor 1, and a second flow controller 12 is connected between the second gas washing and pressure stabilizing device 10 and the anode reactor 2. The arrangement of the first flow controller 11 and the second flow controller 12 can respectively control the flow of the air flow introduced into the cathode reactor 1 and the anode reactor 2, and the requirements for regulating and controlling the photoelectrocatalysis reaction parameters of the photoelectrocatalysis reaction system are improved.
It should be noted that the reaction speed of the photoelectrocatalysis reaction is slow, most of the reaction gas cannot be dissolved in the electrolyte of the cathode reactor after the reaction gas is introduced into the cathode reactor, and the reaction gas which is not dissolved in the electrolyte is discharged from the gas outlet of the cathode reactor.
In order to improve the utilization efficiency of the reaction gas, in this embodiment, the photoelectrocatalysis reaction system comprises a first gas flow switching device 13, and the first gas flow switching device 13 is provided with a first port 131, a second port 132, a third port 133 and a fourth port 134 which can switch the communication state; the first port 131 is communicated with the air outlet end of the first backpressure valve 5, the second port 132 is communicated with the air inlet end of the first air pump 3, the air outlet of the first air storage device 4 and the air outlet of the second air storage device 7 are communicated with the third port 133, and the fourth port is connected with a first one-way valve (15) for exhausting air; the first air pump 3, the first gas washing and pressure stabilizing device 9, the first flow controller 11, the cathode reactor 1, the first back pressure valve 5 and the first gas flow switching device are sequentially communicated through a pipeline to form a cathode gas circulation pipeline, the second gas storage device is opened before the reaction starts, the communication state of the first gas flow switching device 13 is switched to enable the first port 131 to be communicated with the fourth port 134, the second port 132 is communicated with the third port 133, inert gas in the second gas storage device is introduced into the cathode circulation pipeline and is discharged from the fourth port 134, so that air in the cathode circulation pipeline is discharged from the first check valve 15, and the first check valve 15 can prevent external air from entering the cathode circulation pipeline; realizing gas washing of the cathode circulation pipeline; after the gas washing is finished, the second gas storage device is closed, the first gas storage device 4 is opened, and the reaction gas flows into the cathode gas circulation pipeline from the first gas storage device 4, so that the concentration of the reaction gas in the cathode gas circulation pipeline is increased, and the required amount of the reaction gas by the cathode reactor 1 in the process of carrying out the photoelectrocatalysis reaction is ensured; then, the communication state of the first airflow switching device 13 is switched, so that the first port 131 is communicated with the second port 132, and the third port 133 is communicated with the fourth port 144, at this time, the cathode gas pipeline forms a closed pipeline, under the driving of the first air pump 3, the gas in the cathode gas circulation pipeline is repeatedly introduced into the cathode reactor 1, and then flows out of the cathode reactor 1, along with the progress of the photoelectrocatalysis reaction, the content of the reaction gas in the cathode gas circulation pipeline can be reduced, at this time, the communication state of the first airflow switching device 13 is switched again, and the reaction gas is introduced into the cathode gas circulation pipeline, so that the effective utilization rate of the reaction gas is ensured.
In this embodiment, the photoelectrocatalysis reaction system further comprises a second gas flow switching device 14, the second gas flow switching device 14 is provided with a fifth port 141, a sixth port 142, a seventh port 143 and an eighth port 144 which can be switched to a communication state, and a gas outlet of the second gas storage device 7 is communicated with the fifth port 141; the sixth port 142 is communicated with the air inlet end of the second air pump 6, and the seventh port 143 is communicated with the air outlet end of the second backpressure valve 8; specifically, the second air pump 6, the second gas washing and pressure stabilizing device 10, the second flow controller 12, the anode reactor 2, the second back pressure valve 8 and the second gas flow switching device 14 are sequentially communicated through a pipeline to form an anode gas circulation pipeline, before the photoelectrocatalysis reaction starts, the communication state of the second gas flow switching device 14 is switched, so that the fifth port 141 is communicated with the sixth port 142 and the seventh port 143 is communicated with the eighth port 144, the inert gas in the second gas storage device 7 is introduced into the anode gas circulation pipeline, and thus the air in the anode gas circulation pipeline is exhausted, the eighth port 144 is connected with the second one-way valve 16 for exhausting, and the second one-way valve 16 can prevent the air from entering the anode gas circulation pipeline; thereafter, the communication state of the second gas flow switching device 14 is switched again, so that the sixth port 142 is communicated with the seventh port 143 and the fifth port 141 is communicated with the eighth port 144, thereby the anode gas circulation line is in a closed circulation state, and the inert gas waste caused by the inert gas flowing into the air is avoided.
Further, as shown in fig. 1, the photoelectrocatalysis reaction system further comprises a fifth gas flow switching device 26, the fifth gas flow switching device 26 is provided with a seventeenth port, an eighteenth port and a nineteenth port which can be switched to be in a communication state, the first gas storage device 4 and the second gas storage device 7 are both communicated with the seventeenth port, the eighteenth port is communicated with the third port 133, and the nineteenth port is communicated with the fifth port 141; switching the communication state of the fifth air flow switching device 26 can communicate the seventeenth port with the eighteenth port, or communicate the seventeenth port with both the eighteenth port and the nineteenth port; before the start of the photoelectrocatalysis reaction, the seventeenth port is communicated with the eighteenth port and the nineteenth port, inert gas is simultaneously introduced into the cathode gas circulation pipeline and the anode gas circulation pipeline through the second gas storage device 7, the cathode gas circulation pipeline and the anode gas circulation pipeline are exhausted, and after the exhaust is finished, the communication state of the fifth gas flow switching device 26 is switched, so that the seventeenth port and the eighteenth port are connected to the cathode gas selection pipeline to introduce reaction gas; the fifth gas flow switching device 26 is arranged to make the whole structure of the photoelectrocatalysis reaction system more compact.
In this embodiment, in order to facilitate detection of the content of the reactant gas in the cathode gas circulation pipeline, the photoelectrocatalysis reaction system further comprises a gas detection system for detecting the content of the generated gas and a third gas flow switching device 17, the gas detection system is provided with a first gas inlet pipe 18 and a first gas outlet pipe 19, the third gas flow switching device 17 is provided with a ninth port 171, a tenth port 172, an eleventh port 173 and a twelfth port 174, the ninth port 171 is communicated with the gas outlet of the cathode reactor 1, the tenth port 172 is communicated with the first gas inlet pipe 18, the eleventh port 173 is communicated with the first gas outlet pipe 19, and the twelfth port 174 is communicated with the gas inlet end of the first back pressure valve 5; when the content of the reaction gas in the cathode gas circulation pipeline is detected, the communication state of the third gas flow switching device 17 is switched, so that the ninth port 171 is communicated with the tenth port 172 and the eleventh port 173 is communicated with the twelfth port 174, so that the gas in the cathode gas circulation pipeline flows into the gas detection system through the first gas inlet pipe 18 and then flows out of the gas detection system through the first gas outlet pipe 19, thereby detecting the content of the reaction gas in the cathode gas circulation pipeline, and then the communication state of the third gas flow switching device 17 is switched again, so that the ninth port 171 is communicated with the twelfth port 174 and the tenth port 172 is communicated with the eleventh port 173, thereby ensuring that the cathode gas circulation pipeline is in a closed circulation state. It should be noted that the third airflow switching device 17 is arranged to make the cathode gas circulation pipeline flow along the paths of the first air pump 3, the first scrubbing and pressure stabilizing device 9, the first flow controller 11, the cathode reactor 1, the third airflow switching device 17, the first back pressure valve 5 and the first airflow switching device all the time in a non-detection state, so as to eliminate the influence of the gas detection system caused by the pressure change in the cathode reactor during the sampling process; in other embodiments of the present application, the third gas flow switching device 17 is disposed between the gas outlet end of the first backpressure valve 5 and the gas inlet end of the first gas pump 3, so as to further avoid the influence of the switching process of the third gas flow switching device 17 on the fluctuation of the gas pressure in the cathode reactor 1.
Specifically, as shown in fig. 1, 6, and 7, the gas detection system includes a gas chromatograph 20, a sampling device 21, and a third gas storage device 22 for introducing an inert gas into the sampling device 21; the sampling device 21 is provided with a first interface 21-1, a second interface 21-2, a third interface 21-3, a fourth interface 21-4, a fifth interface 21-5 and a sixth interface 21-6 which can switch communication states, the first interface 21-1 is communicated with an air outlet of the third air storage device 22, the second interface 21-2 is connected with a first quantitative ring 21-11, the other end of the first quantitative ring 21-11 is connected with the fifth interface 21-5, the third interface 21-3 is communicated with the first air inlet pipe 18, the fourth interface 21-4 is communicated with the first air outlet pipe 19, and the sixth interface 21-6 is communicated with an air inlet of the gas chromatograph 20;
during sampling, firstly switching the communication state of the third gas flow switching device 17 to make the gas in the cathode gas circulation pipeline flow into the first gas inlet pipe 18, then switching the communication state of the sampling device 21 to make the sampling device 21 in the first state as shown in fig. 6, at this time, the third interface 21-3, the second interface 21-2, the first quantitative ring 21-11, the fifth interface 21-5 and the fourth interface 21-4 are sequentially communicated, and the reaction gas flowing into the gas inlet pipe 18 flows into the first quantitative ring 21-11 through the third interface 21-3 and the second interface 21-2 and flows to the first gas outlet pipe 19 through the fifth interface 21-5 and the fourth interface 21-4; after sampling, the communication state of the third airflow switching device 17 is switched, the introduction of the cathode reaction gas into the first air inlet pipe 18 is stopped, and the communication state of the sampling device 21 is switched, so that the sampling device 21 is in the second state as shown in fig. 7, at this time, the first interface 21-1, the second interface 21-2, the first quantitative ring 21-11, the fifth interface 21-5 and the sixth interface 21-6 are sequentially communicated, so that the inert gas in the third air storage device 22 is introduced into the first quantitative ring 21-11, and the cathode reaction gas remaining in the first quantitative ring 21-11 is discharged to the gas chromatograph 20.
Further, in order to detect the reactant gas in the anode gas circulation pipeline, in this embodiment, the photoelectrocatalysis reaction system includes a fourth gas flow switching device 23, the fourth gas flow switching device 23 is provided with a thirteenth port 231, a fourteenth port 232, a fifteenth port 233 and a sixteenth port 234 which can switch the communication state, the thirteenth port 231 is communicated with the gas inlet end of the second backpressure valve 8, and the fourteenth port 232 is communicated with the gas outlet of the anode reactor 2; the sampling device 21 is further provided with a seventh interface 21-7, an eighth interface 21-8, a ninth interface 21-9 and a tenth interface 21-10, which can be switched to a communication state, the seventh interface 21-7 is connected with a second quantitative ring 21-12, the other end of the second quantitative ring 21-12 is connected with the tenth interface 21-10, the eighth interface 21-8 is communicated with the sixteenth port 234, and the ninth interface 21-9 is communicated with the fifteenth port 233; specifically, as shown in fig. 1 and 5, the gas detection system is provided with a second gas inlet pipe 24 and a second gas outlet pipe 25, one end of the second gas inlet pipe 24 is connected to the ninth port 21-9, the other end of the second gas inlet pipe 24 is connected to the fifteenth port 233, one end of the second gas outlet pipe 25 is connected to the eighth port 21-8, and the other end of the second gas outlet pipe 25 is connected to the sixteenth port 234; when the content of the reactant gas in the anode gas circulation pipeline needs to be detected, firstly, the communication state of the fourth gas flow switching device 23 is switched, so that the thirteenth port 231 is communicated with the sixteenth port 234 and the fifteenth port 233 is communicated with the fourteenth port 232, so that the gas in the anode gas circulation pipeline flows into the second gas inlet pipe 24, then, the communication state of the sampling device 21 is switched, so that the sampling device 21 is in the second state shown in fig. 7, at this time, the ninth port 21-9, the tenth port 21-10, the second quantitative ring 21-12, the seventh port 21-7 and the eighth port 21-8 are sequentially communicated, and the anode reactant gas in the second gas inlet pipe 24 is introduced into the second quantitative ring 21-12; then, the communication state of the sampling device 21 is switched again, so that the sampling device 21 is in the first state as shown in fig. 6, and at this time, the first interface 21-1, the tenth interface 21-10, the second quantitative ring 21-12, the seventh interface 21-7 and the sixth interface 21-6 are sequentially communicated, so that the inert gas in the third gas storage device 22 is introduced into the second quantitative ring 21-12, and the anode reaction gas remaining in the second quantitative ring 21-12 is discharged to the gas chromatograph 20. The arrangement of the sampling device 21 enables the detection of the cathode gas product and the anode gas product to be satisfied by only using one gas chromatograph, greatly reduces the equipment cost of the photoelectrocatalysis reaction system, and enables the whole arrangement of the photoelectrocatalysis reaction system to be more compact. It should be noted that pressure fluctuation in the cathode reactor can cause pressure change in the first quantitative ring, pressure fluctuation in the anode reactor can cause pressure change in the second quantitative ring, pressure change in the first quantitative ring and the second quantitative ring can cause sample amount fluctuation entering the gas chromatograph at each time, and further cause poor evaluation reproducibility of the photoelectrocatalysis reaction efficiency.
In this embodiment, as shown in fig. 1, the gas outlet of the first gas storage device 4 is sequentially connected to a first pressure reducing valve 27 and a first flow meter 28, so as to monitor and adjust the pressure and the flow of the gas flowing out of the first gas storage device 4, thereby improving the accuracy of the evaluation of the photoelectrocatalysis reaction efficiency by the photoelectrocatalysis system of this embodiment; a gas washing bottle 31 is arranged between the fifth gas flow switching device 26 and the first gas flow switching device 13, and a solution for absorbing gas same as the cathode product or other soluble gas impurities is arranged in the gas washing bottle 31, so that the same type of products generated in the non-cathode reactor brought by the outside and mixed in the gas entering the cathode gas circulation pipeline from the first gas storage device 4 or the second gas storage device 7 are removed, and the evaluation precision of the photoelectrocatalysis system of the embodiment on the photoelectrocatalysis reaction efficiency is further improved; specifically, in this embodiment, the gas stored in the first gas storage device 4 is nitrogen, the gas generated after the nitrogen is introduced into the cathode reactor 1 is ammonia, and the solution in the first gas washing bottle is an acidic solution, so as to remove ammonia mixed in the gas introduced into the cathode gas circulation pipeline. The gas outlet of the second gas storage device 7 is sequentially connected with a second pressure reducing valve 29 and a second flowmeter 30, the gas outlet of the third gas storage device 22 is connected with a third pressure reducing valve 34, the gas outlet of the cathode reactor 1 is connected to a third gas flow switching device through a first gas pipe, a first condenser pipe 32 is wrapped outside the first gas pipe, the gas outlet of the anode reactor 2 is connected to a fourth gas flow switching device through a second gas pipe, and a second condenser pipe 33 is wrapped outside the second gas pipe.
In this embodiment, a particle exchange membrane for preventing the generated gas in the cathode reactor 1 from entering the anode reactor 2 is interposed between the cathode reactor 1 and the anode reactor 2. Specifically, an H-shaped structure is formed between the cathode reactor 1 and the anode reactor 2, the particle exchange membrane is arranged in the middle of the H-shaped structure, and the particle exchange membrane avoids the situation that ammonia gas generated in the anode reactor and oxygen gas generated in the cathode reactor are mixed in the same liquid phase and gas phase at the same time, so that a product reduced by the cathode is oxidized again at the anode, which is of great importance for ensuring the evaluation accuracy of the photoelectrocatalysis reaction efficiency.
In this embodiment, in order to further improve the accuracy of evaluating the efficiency of the photoelectrocatalysis reaction, the gas in the first gas storage device 4 is a pentadecane isotope gas, so as to avoid the influence of fourteen nitrogen in the air on the accuracy of evaluating the efficiency of the photoelectrocatalysis reaction system.
The following description will be made of the operation of the photoelectrocatalysis reaction system of the present invention, taking the photoelectrocatalysis reaction ammonia production as an example:
firstly, washing gas; specifically, the second gas storage device 7 is unscrewed, the pressure of argon gas flowing out of the second gas storage device 7 is adjusted to 0.3MPa through the second pressure reducing valve 29, the argon gas is divided into two paths after passing through the fifth gas flow switching device 26, the first path flows into the gas washing bottle 31 and further flows to the first gas flow switching device 13, the argon gas flows into the cathode gas circulation pipeline through the first gas flow switching device 13, air in the cathode gas circulation pipeline is exhausted, and the influence of the air in the cathode gas circulation pipeline on the photoelectrocatalysis reaction efficiency is avoided; the second flow flows to the second flow switching device 14, and flows into the anode gas circulation pipeline through the second flow switching device, so that air in the anode gas circulation pipeline is exhausted, and the influence of the air in the anode gas circulation pipeline on the photoelectrocatalysis reaction efficiency is avoided.
Secondly, introducing nitrogen into a cathode gas circulation pipeline; specifically, the second gas storage device 7 is closed, the first gas storage device 4 is opened, nitrogen in the first gas storage device 4 sequentially flows into the cathode gas circulation pipeline through the first pressure reducing valve 27, the first flowmeter 28, the fifth gas flow switching device 26, the gas washing bottle 31 and the first gas flow switching device 13, the nitrogen exhausts argon in the cathode gas circulation pipeline, during the process of exhausting the argon in the cathode gas circulation pipeline, the nitrogen content in the cathode gas circulation pipeline is detected by switching the communication state of the third gas flow switching device 17 and the communication state of the sampling device 21, when the nitrogen content in the cathode gas circulation pipeline is higher than 90%, the cathode gas circulation pipeline is full of the nitrogen, and then the communication state of the first gas flow switching device 13 is switched, so that the cathode gas circulation pipeline is in a closed circulation state.
Thirdly, carrying out a photoelectrocatalysis reaction; specifically, the cathode reactor 1 is illuminated, the electrochemical workstation 35 is opened, and photoelectrocatalysis ammonia generation is started, and the combination of the first flow controller 11 and the second flow controller 12 can realize stable control of the flow rate of the reaction gas in the photoelectrocatalysis reaction process; the combination of the first backpressure valve 5 and the second backpressure valve 8 can realize the stable control of the pressure of the cathode reactor and the anode reactor, and the gas product in the cathode gas circulation pipeline and the gas product in the anode gas circulation pipeline can realize the on-line sampling through the sampling device 21 and carry out the real-time detection through the gas chromatograph 20. The gas chromatograph can only detect the gas composition of one gas path at the same time, and if the gas content in the cathode gas pipeline needs to be detected, the second gas inlet pipe 24 needs to be in a non-gas inlet state.
Fourthly, supplementing nitrogen; specifically, when the nitrogen content in the cathode gas circulation line decreases to 50%, it is necessary to supplement nitrogen to the cathode gas circulation line. At this time, the first pressure reducing valve 27 is opened, nitrogen flows to the first gas flow switching device through the first flow meter 28, the fifth gas flow switching device and the purge bottle 31, the communication state of the first gas flow switching device is switched, so that the first port 131, the second port 132 and the third port 133 are all communicated, and nitrogen flows into the cathode gas circulation pipeline, so that the concentration of the reactant gas in the cathode gas circulation pipeline is increased, and the required amount of the reactant gas in the cathode reactor 1 in the process of performing the photoelectrocatalysis reaction is ensured.
In conclusion, the invention provides a photoelectrocatalysis reaction system, wherein the arrangement of the first backpressure valve 5 and the second backpressure valve 8 can enable the pressure inside the cathode reactor 1 and the pressure inside the anode reactor 2 to be uniform, so that the solubility of reaction gas in the cathode reactor 1 is kept in a stable state, and the stability and control of photoelectrocatalysis efficiency are further ensured; on the other hand, the stable pressure in the reactor can ensure that the volume and the pressure of the gas to be detected entering the quantitative ring are kept stable, so that the quantity of the sample substance entering the gas chromatograph is ensured to be stable, and the two aspects together help the system to realize the accurate evaluation requirement on the photoelectrocatalysis reaction efficiency; the pressure of the gas introduced into the cathode reactor 1 and the anode reactor 2 is ensured to be stable through the first gas washing pressure stabilizing device and the second gas washing pressure stabilizing device; the flow of the air flow introduced into the cathode reactor 1 and the anode reactor 2 can be respectively controlled by arranging the first flow controller 11 and the second flow controller 12, so that the monitoring precision requirement on the photoelectrocatalysis efficiency of a photoelectrocatalysis reaction system is improved; the arrangement of the first airflow switching device 13 enables the cathode gas path circulation pipeline to keep closed circulation, and reaction gas can be introduced into the cathode gas path circulation system in time; through the arrangement of the second airflow switching device 14, the anode gas circulation pipeline can be kept in closed circulation, and the influence of outside air on the evaluation precision of the photoelectrocatalysis efficiency is avoided; through the matching of the sampling device 21, the third gas flow switching device 17 and the fourth gas flow switching device, the gas product in the cathode gas circulation pipeline and the gas product in the anode gas circulation pipeline can be sampled on line through the sampling device 21, and real-time detection is performed through the gas chromatograph 20; through the arrangement of the particle exchange membrane, the situation that the product of cathode reduction is oxidized again at the anode due to the fact that ammonia gas generated in the anode reactor and oxygen generated in the cathode reactor are mixed in the same liquid phase and gas phase at the same time is avoided; by setting the nitrogen as the isotope gas, the influence of the external gas on the evaluation of the photoelectric catalytic reaction efficiency is avoided; the photoelectrocatalysis system formed by the mutual matching of the above characteristics not only improves the effective utilization rate of nitrogen, but also ensures the accurate evaluation requirement on the photoelectrocatalysis reaction efficiency.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.
Claims (8)
1. The photoelectrocatalysis reaction system is characterized by comprising a cathode reactor (1) and an anode reactor (2), wherein an air inlet of the cathode reactor (1) is sequentially connected with a first air pump (3) and a first air storage device (4) used for providing reaction gas for the first air pump (3), and an air outlet of the cathode reactor (1) is connected with a first back pressure valve (5); the air inlet of the anode reactor (2) is sequentially connected with a second air pump (6) and a second air storage device (7) for providing inert gas for the second air pump (6), and the air outlet of the anode reactor (2) is connected with a second back pressure valve (8); the photoelectrocatalysis reaction system comprises a first gas flow switching device (13), wherein the first gas flow switching device (13) is provided with a first port (131), a second port (132), a third port (133) and a fourth port (134) which can be switched into a communication state; the first port (131) is communicated with the air outlet end of the first backpressure valve (5), the second port (132) is communicated with the air inlet end of the first air pump (3), the air outlet of the first air storage device (4) and the air outlet of the second air storage device (7) are communicated with the third port (133), and the fourth port (134) is connected with a first one-way valve (15) for exhausting air;
switching the communication state of the first airflow switching device (13) may cause the first port (131) to communicate with the fourth port (134) and the second port (132) to communicate with the third port (133), or the first port (131) to communicate with the second port (132) and the third port (133) to communicate with the fourth port (134).
2. The photoelectrocatalysis reaction system according to claim 1, wherein a first washing and pressure stabilizing device (9) is connected between the first air pump (3) and the cathode reactor (1), and a second washing and pressure stabilizing device (10) is connected between the second air pump (6) and the anode reactor (2).
3. The photoelectrocatalysis reaction system according to claim 2, wherein a first flow controller (11) is connected between the first washing and pressure stabilizing device (9) and the cathode reactor (1), and a second flow controller (12) is connected between the second washing and pressure stabilizing device (10) and the anode reactor (2).
4. The photoelectrocatalysis reaction system according to claim 1, further comprising a second gas flow switching device (14), wherein the second gas flow switching device (14) is provided with a fifth port (141), a sixth port (142), a seventh port (143) and an eighth port (144) which can switch the communication state, and the gas outlet of the second gas storage device (7) is communicated with the fifth port (141);
the sixth port (142) is communicated with the air inlet end of the second air pump (6), and the seventh port (143) is communicated with the air outlet end of the second backpressure valve (8); a second one-way valve (16) for exhausting is connected to the eighth port (144);
switching the communication state of the second gas flow switching device (14) may cause the fifth port (141) to communicate with the sixth port (142) and the seventh port (143) to communicate with the eighth port (144), or the sixth port (142) to communicate with the seventh port (143) and the fifth port (141) to communicate with the eighth port (144).
5. The photoelectrocatalysis reaction system according to claim 1, further comprising a gas detection system for detecting the content of generated gas and a third gas flow switching device (17), wherein the gas detection system is provided with a first gas inlet pipe (18) and a first gas outlet pipe (19), the third gas flow switching device (17) is provided with a ninth port (171), a tenth port (172), an eleventh port (173) and a twelfth port (174) which can be switched to the communication state, the ninth port (171) is communicated with the gas outlet of the cathode reactor (1), the tenth port (172) is communicated with the first gas inlet pipe (18), the eleventh port (173) is communicated with the first gas outlet pipe (19), and the twelfth port (174) is communicated with the gas inlet end of the first backpressure valve (5);
switching the communication state of the third air flow switching device (17) may cause the ninth port (171) to communicate with the tenth port (172) and the eleventh port (173) to communicate with the twelfth port (174), or the ninth port (171) to communicate with the twelfth port (174) and the tenth port (172) to communicate with the eleventh port (173).
6. The photoelectrocatalytic reaction system according to claim 5, wherein the gas detection system comprises a gas chromatograph (20), a sampling device (21), and a third gas storage device (22) for introducing an inert gas into the sampling device (21);
the sampling device (21) is provided with a first interface (21-1), a second interface (21-2), a third interface (21-3), a fourth interface (21-4), a fifth interface (21-5) and a sixth interface (21-6) which can be switched to be in a communication state, the first interface (21-1) is communicated with an air outlet of the third air storage device (22), the second interface (21-2) is connected with a first quantitative ring (21-11), the other end of the first quantitative ring (21-11) is connected with the fifth interface (21-5), the third interface (21-3) is communicated with the first air inlet pipe (18), the fourth interface (21-4) is communicated with the first air outlet pipe (19), and the sixth interface (21-6) is communicated with an air inlet of the gas chromatograph (20);
the communication state of the sampling device (21) is switched, so that the third interface (21-3), the second interface (21-2), the first quantitative ring (21-11), the fifth interface (21-5) and the fourth interface (21-4) can be communicated in sequence, or the first interface (21-1), the second interface (21-2), the first quantitative ring (21-11), the fifth interface (21-5) and the sixth interface (21-6) are communicated in sequence.
7. The photoelectrocatalytic reaction system according to claim 6, comprising a fourth gas flow switching device (23), wherein the fourth gas flow switching device (23) is provided with a thirteenth port (231), a fourteenth port (232), a fifteenth port (233) and a sixteenth port (234) which are switchable in communication, the thirteenth port (231) is in communication with the gas inlet end of the second backpressure valve (8), and the fourteenth port (232) is in communication with the gas outlet of the anode reactor (2);
the sampling device (21) is further provided with a seventh interface (21-7), an eighth interface (21-8), a ninth interface (21-9) and a tenth interface (21-10) which can be switched to be in a communication state, the seventh interface (21-7) is connected with a second quantitative ring (21-12), the other end of the second quantitative ring (21-12) is connected with the tenth interface (21-10), the eighth interface (21-8) is communicated with the sixteenth port (234), and the ninth interface (21-9) is communicated with the fifteenth port (233);
switching the communication state of the sampling device (21) to enable the ninth interface (21-9), the tenth interface (21-10), the second quantitative ring (21-12), the seventh interface (21-7) and the eighth interface (21-8) to be communicated in sequence; or the first interface (21-1), the tenth interface (21-10), the second quantitative ring (21-12), the seventh interface (21-7) and the sixth interface (21-6) are communicated in sequence;
switching the communication state of the fourth airflow switching device (23) may cause the thirteenth port (231) to communicate with the sixteenth port (234) and the fifteenth port (233) to communicate with the fourteenth port (232), or the thirteenth port (231) to communicate with the fourteenth port (232) and the fifteenth port (233) to communicate with the sixteenth port (234).
8. Photoelectrocatalytic reaction system according to any one of claims 1 to 7, wherein an ion exchange membrane for preventing products inside the cathode reactor (1) from entering the anode reactor (2) is interposed between the cathode reactor (1) and the anode reactor (2).
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