CN218036417U - In-situ Raman spectrum device for on-line monitoring electrocatalysis test of high-voltage system - Google Patents
In-situ Raman spectrum device for on-line monitoring electrocatalysis test of high-voltage system Download PDFInfo
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Abstract
The in-situ Raman spectrum device for monitoring the electrocatalysis test of the high-voltage system on line comprises a gas steel cylinder, a plunger pump, a Raman spectrometer, a computer, an electrochemical workstation and a high-voltage Raman cell component; the high-pressure Raman cell component comprises a cell body, a top cover, a lining, an air inlet valve, an outlet valve, a pressure display meter, a pressure safety valve, a working electrode, a reference electrode, a counter electrode and an optical window; a sealing washer is arranged between the top cover and the tank body and is fixed by screws; the optical window is arranged on the top cover by a sealing washer and a sealing clamping sleeve; a Raman lens on the Raman spectrometer is close to the optical window for focusing; the gas steel cylinder is connected with the gas inlet of the gas inlet valve through the plunger pump, the gas outlet of the gas inlet valve is respectively connected with the pressure gauge and the inlet of the tank body through the two-way valve, and the outlet of the tank body is sequentially connected with the pressure safety valve and the outlet valve; the Raman spectrometer and the electrochemical workstation are respectively connected with the computer, and the electrochemical workstation is respectively connected with the three electrodes of the cell body through three-electrode leads.
Description
Technical Field
The utility model relates to a high-tension electricity catalytic normal position raman characterization test field especially relates to on-line monitoring high voltage system electro-catalysis test's normal position raman spectroscopy device.
Background
Since the industrial revolution, CO 2 The emission of CO increases year by year 2 The concentration of the pesticide breaks through 420ppm, so that various environmental problems such as greenhouse effect and the like are caused. Thus, to CO 2 Capture and conversion to useful chemicals or fuels is of great interest. In which CO is electrocatalyzed 2 Reduction has been extensively studied by researchers in recent years as one of the most potential technologies. To solve CO 2 The problem of low solubility, resulting in inefficient mass transfer, etc., is solved by passing high pressure CO 2 The electrocatalytic reduction method can effectively solve the problem and simultaneously can inhibit CO 2 Competition for RR reflects HER. In addition, high pressure CO 2 Electrochemical reduction is more suitable for the treatment of industrial waste gases making it more potential in industrial applications, however high pressure CO is now available 2 Characterization tests for electrocatalytic reduction are still largely limited by the lack of in-situ testing devices, and difficulty in obtaining relevant in-situ data through in-situ characterization tests, thereby making it difficult to monitor the reaction process in situ for relevant mechanism studies.
Raman spectrum characterization is an important technology for researching chemical reaction mechanism, because of waterThe raman scattering of (a) is weak and raman spectroscopy is an ideal tool for studying compounds in aqueous solutions. Therefore, it is commonly used by researchers for atmospheric pressure electro-catalysis of CO 2 In-situ monitoring of the (CO) reduction process to obtain information on the dynamic changes of the catalyst and real-time detection of reaction intermediates, for the study of electrocatalytic CO 2 The reaction path of (CO) reduction and mechanism research provide great help. Patent CN 213875522U discloses an in-situ electrochemical Raman spectrum measuring system in a high-temperature high-pressure water fluid environment, which comprises a high-temperature high-pressure reaction vessel, an electrochemical measuring device and a Raman spectrum measuring device, wherein the device can be used for testing under high pressure, but a larger solution resistance exists between a working electrode and a reference electrode. In addition, it is difficult to satisfy the electrocatalytic high-pressure CO in the design and configuration of the structure 2 Test requirements for (CO) reduction. Therefore, the existing patent can not accurately realize the electrocatalytic high-pressure CO 2 In situ raman characterization test of (CO) reduction.
Disclosure of Invention
An object of the utility model is to solve the above-mentioned problem among the prior art, provide the normal position raman spectroscopy device of on-line monitoring high voltage system electro-catalysis test, have easy operation, fill dress high pressure convenience, pressure resistance good and wash simple swift characteristics. The utility model discloses can realize high-tension electricity catalysis CO 2 Characterization test of in-situ Raman spectrum of (CO) experiment and mechanism research thereof.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
the in-situ Raman spectrum device for monitoring the electrocatalysis test of the high-voltage system on line comprises a gas steel cylinder, a plunger pump, a Raman spectrometer, a computer, an electrochemical workstation and a high-voltage Raman cell component;
the high-pressure Raman cell assembly comprises a cell body, a top cover, a lining, an air inlet valve, an outlet valve, a pressure display meter, a pressure safety valve, a working electrode, a reference electrode, a counter electrode and an optical window;
a sealing washer is arranged between the top cover and the pool body and is fixed by screws; the sealing washer and the sealing cutting sleeve for the optical window are arranged on the top cover; a Raman lens on the Raman spectrometer is close to the optical window for focusing;
the gas steel cylinder is connected with a gas inlet of a gas inlet valve through a plunger pump, a gas outlet of the gas inlet valve is respectively connected with a pressure gauge and an inlet of the tank body through a two-way valve, and an outlet of the tank body is sequentially connected with a pressure safety valve and an outlet valve;
the Raman spectrometer and the electrochemical workstation are respectively connected with a computer, and the electrochemical workstation is respectively connected with three electrodes in the cell body through three-electrode leads.
The pool body and the top cover are made of high-pressure resistant materials.
The lining is made of insulating materials.
The sealing washer is acid and alkali resistant and supercritical CO 2 Corrosion performance of (2).
And the working electrode, the reference electrode and the counter electrode are all packaged by adopting an insulating material.
The reference electrode and the counter electrode are inserted from the side edge of the cell body, the working electrode is inserted from the bottom of the cell body, and the three electrodes are fixed on the cell body through the threaded bayonet. The reference electrode is close to the working electrode, and the distance between the reference electrode and the working electrode is less than 5mm.
The distance between the working electrode and the optical window is controlled within 3 mm.
The thickness of the optical window is 1-3 mm, the diameter is 25-40 mm, and the optical window can be selected according to the requirements of test pressure and a Raman spectrum lens.
The pressure gauge adopts a digital display pressure gauge with the range of 0-20 MPa.
Application of in-situ Raman spectrum device for on-line monitoring of high-voltage system electro-catalysis test to on-line monitoring of high-voltage system electro-catalysis CO 2 (CO) in situ Raman Spectroscopy of reduction test.
Compared with the prior art, the utility model discloses technical scheme obtains beneficial effect is:
1. this device adopts high pressure resistant material as the cell body, adopts insulating material as the inside lining, is equipped with the visual window that has good optical transmission nature and pressure resistance, has fine resistance to pressure, and the seal, acid and alkali-resistance and corrosion resistance to the raman laser that sees through different wavelength that can be fine does not influence raman signal's detection.
2. The device can be fixed in a mode of connecting and combining the three electrodes packaged by insulating materials with the threaded bayonet inside and outside the Raman cell, and has good pressure resistance and corrosion resistance.
3. The device can be well used for electrocatalysis of high-pressure CO 2 Reduced in-situ Raman characterization test for realizing electrocatalysis high-pressure CO 2 In situ monitoring of reduction to obtain electrocatalytic CO in real time 2 Reduced raman data.
4. The utility model discloses in, reference electrode is close to working electrode (distance < 5 mm), has reduced solution resistance, improves the accuracy of test.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic diagram of the structure of a high pressure Raman cell assembly;
FIG. 3 shows example 1 at 25bar CO 2 Raman spectrograms acquired at different potentials under pressure;
FIG. 4 shows example 2 at 80bar CO 2 Raman spectra acquired at different potentials under pressure;
FIG. 5 shows the results of example 3 with different CO 2 Raman spectra taken at the same potential at pressures (1 bar, 25bar and 80 bar).
Reference numerals: the device comprises an air inlet valve 1, a two-way valve 2, a two-way valve 3, a pressure display meter 4, a top cover 5, an optical window 6, a sealing washer 7, a cell body 8, a reference electrode 9, a threaded bayonet 10, a working electrode 11, an inner lining 12, a counter electrode 13, a pressure safety valve 14, an outlet valve 15, a sealing clamping sleeve 16, a screw 17, a Raman lens 18, a reflecting mirror 19, laser 20, a Raman spectrometer 21, a plunger pump 22, a plunger pump display panel 23, a gas steel cylinder 24, a stainless steel connecting pipe 25, a computer 26 and an electrochemical workstation 27.
Detailed Description
In order to make the technical problem, technical solution and beneficial effects to be solved by the present invention clearer and more obvious, the following description is made in detail with reference to the accompanying drawings and embodiments.
As shown in fig. 1-2, the in-situ raman spectroscopy apparatus for on-line monitoring of the electrocatalytic test of the high-voltage system in the present embodiment includes a pressurization system (a plunger pump 22, a plunger pump display panel 23, a gas steel cylinder 24 and a stainless steel connecting tube 25); a test system (high-voltage raman cell assembly (1-17), computer 26 and electrochemical workstation 27); a detection system (raman lens 18, mirror 19, laser 20 and raman spectrometer 21).
The high-pressure Raman cell component comprises an air inlet valve 1, a two-way valve 2, a two-way valve 3, a pressure display meter 4, a top cover 5, an optical window 6, a sealing washer 7, a cell body 8, a reference electrode 9, a threaded bayonet 10, a working electrode 11, a lining 12, a counter electrode 13, a pressure safety valve 14, an outlet valve 15, a sealing clamping sleeve 16 and a screw 17;
a sealing washer 7 is arranged between the top cover 5 and the tank body 8 and is fixed by a screw 17;
the optical window 6 is arranged on the top cover by a sealing gasket and a sealing cutting sleeve 16;
a Raman lens 18 on the Raman spectrometer is close to the optical window 6 for focusing;
the gas steel cylinder 24 is connected with the gas inlet of the gas inlet valve 1 through the plunger pump 22;
the air outlet of the air inlet valve 1 is respectively connected with the pressure display meter 4 and the inlet of the tank body 8 through a two-way valve, and the outlet of the tank body 8 is sequentially connected with a pressure safety valve 14 and an outlet valve 15;
the Raman spectrometer 21 and the electrochemical workstation 27 are respectively connected with a computer 26;
the electrochemical workstation 27 is respectively connected with three electrodes of the cell body 8 through three-electrode leads;
the tank body 8 and the top cover 5 have high pressure resistance;
the lining needs to be insulated, so that the lining has good voltage resistance;
the sealing gasket needs to be acid and alkali resistant and supercritical CO 2 The corrosion is not easy to deform, the tightness is good, the wear resistance is strong, and the sealing ring can be repeatedly used;
the working electrode 11, the reference electrode 9 and the counter electrode 13 can be packaged by adopting an insulating material;
the reference electrode 9 and the counter electrode 13 are inserted from the side edge of the cell body 8, the working electrode 11 is inserted from the bottom of the cell body 8, and the three electrodes are fixed on the cell body through the threaded bayonet 10;
the distance between the working electrode 11 and the optical window 6 is controlled to be within 3mm to ensure successful focusing of the raman laser.
The thickness of the optical window 6 is 1-3 mm, the diameter is 25-40 mm, and the optical window can be selected according to the size of the tested Raman lens and the required testing pressure. Before the test, the optical windows with different specifications are installed and then subjected to a pressure resistance test to ensure safety.
The pressure display meter 4 can adopt a digital display pressure meter with a range of 0-20 MPa, and has good sensing and real-time pressure display.
Example 1
Medicine preparation: 0.1M KHCO 3 Aqueous solution (national pharmaceutical group), catalyst ink, high purity CO 2 (99.999%, new aviation gas Co.)
Other devices: plunger pump, raman spectroscopy, computer, electrochemical workstation and stainless steel connecting pipe.
1. Three electrodes, namely a straight glassy carbon working electrode, an Ag/AgCl (saturated KCl) reference electrode and a platinum wire counter electrode are fixed on the cell body.
2. And coating the catalyst ink on a glassy carbon working electrode, and naturally drying.
3. Adding 0.1M KHCO into the lining 3 Water solution, locking pool body and top cover, pumping plunger pump and CO 2 The steel cylinder is connected, and the pool body is connected with the plunger pump.
4. Continuous introduction of CO 2 Introducing gas into the tank for 10min to discharge internal air, and introducing 25bar of CO 2 Gas, after pressure equalization, closes the inlet valve 1.
5. And placing the cell body on a Raman testing platform for focusing.
6. And correspondingly connecting the three electrodes of the electrochemical workstation with the three electrodes of the cell body, setting electrochemical test and Raman spectrum test conditions to perform electrochemical performance test and Raman spectrum acquisition test.
CO at 25bar 2 Pulling for collecting different electric potentials under pressureReferring to FIG. 3, it can be seen that the device can be used for high pressure CO 2 In situ raman characterization tests were performed in electrocatalytic reduction.
Example 2
This example was operated in the same manner as example 1, except that the set pressure was changed to CO 2 The gas pressure was 80bar. CO at 80bar 2 The Raman spectrogram acquired by different potentials under pressure is shown in figure 4, and the device can realize high-pressure CO 2 In situ raman characterization tests were performed in electrocatalytic reduction.
Example 3
This example was carried out in the same manner as in example 1, with CO at 1bar, 25bar and 80bar, respectively 2 And (3) closing the air inlet valve after the pressure is balanced, and carrying out electrochemical performance test and Raman spectrogram acquisition test.
Respectively at different CO 2 Raman spectra taken at the same potential for pressures (1 bar, 25bar and 80 bar) as can be seen from FIG. 5, the apparatus can be operated at high CO pressures 2 In situ raman characterization tests were performed in electrocatalytic reduction.
Claims (5)
1. The in-situ Raman spectrum device for on-line monitoring of the electrocatalysis test of the high-voltage system is characterized in that: comprises a gas steel cylinder, a plunger pump, a Raman spectrometer, a computer, an electrochemical workstation and a high-pressure Raman cell component;
the high-pressure Raman cell assembly comprises a cell body, a top cover, a lining, an air inlet valve, an outlet valve, a pressure display meter, a pressure safety valve, a working electrode, a reference electrode, a counter electrode and an optical window;
a sealing washer is arranged between the top cover and the pool body and is fixed by screws; the optical window is arranged on the top cover by a sealing washer and a sealing clamping sleeve; a Raman lens on the Raman spectrometer is close to the optical window for focusing;
the gas steel cylinder is connected with a gas inlet of a gas inlet valve through a plunger pump, a gas outlet of the gas inlet valve is respectively connected with a pressure gauge and an inlet of the tank body through a two-way valve, and an outlet of the tank body is sequentially connected with a pressure safety valve and an outlet valve;
the Raman spectrometer and the electrochemical workstation are respectively connected with a computer, and the electrochemical workstation is respectively connected with three electrodes in the cell body through three-electrode leads.
2. The in-situ raman spectroscopy device for online monitoring of electrocatalytic tests of high voltage systems of claim 1, wherein: the reference electrode and the counter electrode are inserted from the side edge of the cell body, the working electrode is inserted from the bottom of the cell body, and the three electrodes are fixed on the cell body through the threaded bayonet; the reference electrode is next to the working electrode, and the distance between the reference electrode and the working electrode is less than 5mm.
3. The in-situ raman spectroscopy device for on-line monitoring of electrocatalytic tests of high voltage systems according to claim 1, wherein: the distance between the working electrode and the optical window is controlled within 3 mm.
4. The in-situ raman spectroscopy device for on-line monitoring of electrocatalytic tests of high voltage systems according to claim 1, wherein: the thickness of the optical window is 1-3 mm, and the diameter is 25-40 mm.
5. The in-situ raman spectroscopy device for on-line monitoring of electrocatalytic tests of high voltage systems according to claim 1, wherein: the pressure gauge adopts a digital display pressure gauge with the range of 0-20 MPa.
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| CN115184329A (en) * | 2022-06-21 | 2022-10-14 | 厦门大学 | In-situ Raman spectrum device for on-line monitoring electrocatalysis test of high-voltage system and application |
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| CN115184329A (en) * | 2022-06-21 | 2022-10-14 | 厦门大学 | In-situ Raman spectrum device for on-line monitoring electrocatalysis test of high-voltage system and application |
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