Photocatalytic tester and testing method

Abstract

The application discloses a kind of photothermal catalysis testers and test methods, it is related to photothermal catalysis test technical field, including cavity, sealing cover, first shielding layer, second shielding layer, support plate, backing plate, shield, catalytic air inlet, sensor support, heating disc, object table, catalytic air transmission pipe, briquetting, porous air-permeable ceramic, electric signal interface, cavity cover, cavity cover nut, cavity cover screw, observation window, double sleeve joint, foot pad, sealing ring, atmosphere environment temperature measuring port, quartz cover temperature shielding layer, catalytic air outlet, high-temperature heating sample platform, temperature shielding layer, temperature control and temperature monitoring interface;Sealing cover is sealed at one end of cavity, cavity cover is assembled in the top opening of cavity;Backing plate and support plate are fixed in cavity inside bottom side in turn, heating disc is installed above support plate, and high-temperature heating sample platform is fixed on heating disc.The application uses the above-mentioned photothermal catalysis tester and test method, and the closed cavity is reliable in sealing, and gas circuit is stable in circulation.

Description

Technical Field

[0001] This invention relates to the field of photothermal catalysis testing technology, and in particular to a photothermal catalysis testing instrument and testing method. Background Technology

[0002] Gas-solid phase photocatalysis and thermocatalysis technologies are widely used in CO2 reduction, catalytic hydrogenation, VOCs degradation, nitrogen fixation, sulfur fixation, and other reaction scenarios, covering many fields such as energy and chemical engineering, environmental governance, chemical industry, materials science, and materials characterization. Studying the catalytic performance and phase structure evolution of catalytic materials under light, high temperature, and variable temperature conditions is an important research method for the development of new energy materials and the iteration of environmental pollutant treatment technologies.

[0003] Existing traditional photothermal catalysis testing devices suffer from numerous technical defects: Traditional equipment has a simple cavity sealing structure, poor sealing reliability between the cavity cover and the cavity, incomplete internal atmosphere replacement, and susceptibility to interference from external air, temperature, and humidity, failing to meet the environmental requirements for high-precision gas-solid phase catalytic reactions; conventional equipment lacks multi-layered heat insulation and light-shielding structures, allowing external heat radiation and stray light to easily penetrate the reaction cavity, causing internal temperature and light field disturbances, low temperature control accuracy, and severely affecting the accuracy and repeatability of catalytic reaction test data; traditional sample support structures are simple, lacking dedicated permeable support structures, resulting in poor uniformity of reaction gas flow across the sample surface, which is detrimental to steady-state catalytic reactions; temperature measuring components are mostly simply externally mounted, lacking dedicated sensor support and positioning structures, making it difficult to accurately locate the temperature measuring points near the sample reaction area, hindering precise monitoring and control under high-temperature and variable-temperature conditions; existing equipment has a simple gas path interface layout, with no independent, separate assembly structure for the gas inlet and external transmission pipeline, making pipeline disassembly and maintenance inconvenient and unable to meet the needs of long-term, multi-condition continuous catalytic testing. Summary of the Invention

[0004] The purpose of this invention is to provide a photothermal catalysis tester and test method to solve the defects of existing equipment such as poor sealing, photothermal interference, inaccurate temperature control, and unstable gas path, so as to achieve stable, accurate and repeatable testing of gas-solid phase photothermal catalysis.

[0005] This invention provides a photothermal catalysis testing instrument and method, comprising a cavity, a sealing cover, a first shielding layer, a second shielding layer, a support plate, a pad, a shielding cover, a catalytic inlet, a sensor support, a heating plate, a stage, a catalytic inlet transmission pipe, a pressure block, a porous permeable ceramic, an electrical signal interface, a cavity cover, a cavity cover nut, a cavity cover screw, an observation window, a double compression fitting, foot pads, a sealing ring, an ambient temperature measuring port, a quartz temperature shielding layer, a catalytic outlet, a high-temperature heating sample platform, a temperature shielding layer, and a temperature control and monitoring interface. The sealing cover is sealed at one end of the cavity and is assembled into the top opening of the cavity. The pad and support plate are sequentially fixed to the bottom side inside the cavity. The heating plate is installed above the support plate, the high-temperature heating sample platform is fixed on the heating plate, the stage is located on top of the high-temperature heating sample platform, and the porous permeable ceramic is placed on the stage.

[0006] Preferably, the cavity cover is locked and fixed to the cavity body by cavity cover screws and cavity cover nuts, and the sealing ring is sandwiched between the mating end faces of the cavity cover and the cavity body.

[0007] Preferably, the observation window is embedded in the middle of the cavity cover, and the quartz cover temperature shielding layer is fixed inside the cavity cover and arranged below the observation window.

[0008] Preferably, the second shielding layer is wrapped around the outside of the heating plate and the high-temperature heating sample platform, the first shielding layer is wrapped around the outside of the second shielding layer, and the temperature shielding layer is wrapped around the outside of the first shielding layer.

[0009] Preferably, the shielding cover is fixedly installed inside the cavity on the inner side of one end near the sealing cover.

[0010] Preferably, the catalytic inlet and catalytic outlet are respectively fixed to the side wall of the cavity, and the catalytic inlet transmission pipe is connected and assembled to the outer port of the catalytic inlet.

[0011] Preferably, the double-ferrule connectors are respectively assembled on the outer end of the catalytic intake transmission pipe and the outer end of the catalytic outlet.

[0012] Preferably, the ambient temperature measuring port is fixed to the side wall of the cavity, and the temperature control and temperature monitoring interface is fixedly installed on the outer end face of the sealing cover.

[0013] Preferably, the sensor support is horizontally inserted through the side wall of the cavity, the inner end of the sensor support extends to the side of the high-temperature heating sample platform, the pressure block is fixed to the outer wall of the cavity and covers the insertion position of the sensor support, the electrical signal interface is fixedly embedded in the sealing cover and communicates with the inside of the cavity, and a foot pad is fixedly installed at the bottom of the cavity.

[0014] A testing method for a photothermal catalysis tester includes the following steps: Step S1, Sample loading and sealing; Place the catalytic sample to be tested on the surface of the porous permeable ceramic and spread it evenly, and place the entire porous permeable ceramic on the stage; Close the chamber cover and lock it with the chamber cover screws and nuts, and use the sealing ring to achieve the chamber seal; Step S2, Gas Replacement: Inert gas is introduced into the cavity through the external pipeline via the catalytic intake transmission pipe and the catalytic intake port to purge and replace the air and impurity gas in the cavity. The waste gas is discharged from the catalytic outlet, so that the cavity reaches the preset pure atmosphere. Step S3: Temperature control and preheating; start the heating plate to heat the high-temperature heating sample platform, and regulate the heating conditions through the temperature control and temperature monitoring interface; use the sensor support and the ambient temperature measurement port to collect temperature parameters synchronously, so that the sample area is stabilized at the set catalytic reaction temperature; Step S4, photothermal coupling reaction: An external light source is incident on the sample surface through the observation window to carry out a photothermal synergistic catalytic reaction; external photothermal interference is isolated by the first shielding layer, the second shielding layer, the temperature shielding layer, and the quartz cover temperature shielding layer. Step S5: Steady-state data acquisition; Maintain a constant gas supply flow rate through the catalytic inlet and catalytic gas inlet to keep the reaction atmosphere in the chamber stable; Continuously acquire relevant test data on temperature, atmosphere, and catalytic reaction throughout the process to complete the steady-state catalytic test; Step S6: Stop and reset; stop the light source and heating plate from working, continuously purge and cool the chamber with inert gas through the catalytic gas inlet and catalytic gas inlet, and after the chamber returns to normal temperature and pressure, open the chamber cover and take out the sample to complete the test.

[0015] Therefore, the present invention adopts the above-mentioned photothermal catalysis tester and test method to solve the defects of existing equipment such as poor sealing, photothermal interference, inaccurate temperature control and unstable gas path, and realizes stable, accurate and repeatable testing of gas-solid phase photothermal catalysis.

[0016] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the overall structure of a photothermal catalysis tester according to the present invention; Figure 2 This is a cross-sectional view of a photothermal catalysis testing instrument according to the present invention; Figure 3 This is a schematic diagram of the sensor support structure in a photothermal catalysis tester according to the present invention; Figure 4 This is a schematic flowchart of the testing method of a photothermal catalysis tester according to the present invention.

[0018] Figure Labels 1. Chamber; 2. Sealing cap; 3. First shielding layer; 4. Second shielding layer; 5. Support plate; 6. Pad; 7. Shielding cover; 8. Catalytic inlet; 9. Sensor support; 10. Heating plate; 11. Stage; 12. Catalytic inlet transmission pipe; 13. Press block; 14. Porous permeable ceramic; 15. Electrical signal interface; 16. Chamber cover; 17. Chamber cover nut; 18. Chamber cover screw; 19. Observation window; 20. Double compression fitting; 21. Foot pad; 22. Sealing ring; 23. Atmosphere temperature measurement port; 24. Quartz cover temperature shielding layer; 25. Catalytic outlet; 26. High-temperature heating sample platform; 27. Temperature shielding layer; 28. Temperature control and temperature monitoring interface. Detailed Implementation

[0019] The technical solution of the present invention will be further described below with reference to the accompanying drawings and embodiments.

[0020] Unless otherwise defined, the technical or scientific terms used in this invention shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention pertains.

[0021] The terms "first," "second," and similar words used in this invention do not indicate any order, quantity, or importance, but are merely used to distinguish different components. Terms such as "comprising" or "including" mean that the element or object preceding the word encompasses the elements or objects listed after the word and their equivalents, without excluding other elements or objects. Terms such as "connected" or "linked" are not limited to physical or mechanical connections, but can include electrical connections, whether direct or indirect. Terms such as "upper," "lower," "left," and "right" are used only to indicate relative positional relationships; when the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0022] Example 1 like Figures 1-4 As shown, the present invention provides a photothermal catalytic testing instrument, comprising a cavity 1, a sealing cover 2, a first shielding layer 3, a second shielding layer 4, a support plate 5, a pad 6, a shielding cover 7, a catalytic air inlet 8, a sensor support 9, a heating plate 10, a stage 11, a catalytic air inlet transmission pipe 12, a pressure block 13, a porous permeable ceramic 14, an electrical signal interface 15, a cavity cover 16, a cavity cover nut 17, a cavity cover screw 18, an observation window 19, a double compression fitting 20, foot pads 21, a sealing ring 22, an ambient temperature measuring port 23, a quartz cover temperature shielding layer 24, a catalytic air outlet 25, a high-temperature heating sample platform 26, a temperature shielding layer 27, and a temperature control and monitoring interface 28.

[0023] A sealing cap 2 is sealed at one end of the cavity 1, and a cavity cover 16 is fitted to the top opening of the cavity 1; a pad 6 and a support plate 5 are fixed to the bottom inside the cavity 1 in sequence, and a heating plate 10 is installed above the support plate 5. A high-temperature heating sample platform 26 is fixed on the heating plate 10, a stage 11 is located on top of the high-temperature heating sample platform 26, and a porous permeable ceramic 14 is placed on the stage 11 to support the catalytic sample and ensure uniform permeation and flow of the reaction gas.

[0024] The cavity cover 16 is locked and fixed to the cavity 1 by the cavity cover screw 18 and the cavity cover nut 17. The sealing ring 22 is sandwiched between the cavity cover 16 and the mating end face of the cavity 1 to achieve a tight seal of the opening of the cavity 1, preventing leakage of internal reaction gas and intrusion of external environmental interference.

[0025] An observation window 19 is embedded in the center of the cavity cover 16, allowing an external light source to be incident perpendicularly onto the sample surface inside the cavity 1. A quartz temperature shielding layer 24 is fixed inside the cavity cover 16 and positioned below the observation window 19. It can isolate stray light and external thermal radiation, stabilizing the light and temperature fields inside the reaction cavity.

[0026] The second shielding layer 4 is wrapped around the outside of the heating plate 10 and the high-temperature heating sample platform 26, the first shielding layer 3 is wrapped around the outside of the second shielding layer 4, and the temperature shielding layer 27 is wrapped around the outside of the first shielding layer 3. This forms a multi-layered composite shielding and heat insulation structure, effectively isolating the heat exchange and light interference between the inside and outside of the cavity 1. The shielding cover 7 is fixedly installed inside the cavity 1 near the inner side of the sealing cover 2. The shielding cover 7, together with each shielding layer, forms a comprehensive shielding protection system.

[0027] The catalytic inlet 8 and catalytic outlet 25 are respectively fixed to the side wall of the cavity 1. The catalytic intake transmission pipe 12 is connected to the outer port of the catalytic inlet 8 to form a split intake passage. The catalytic inlet 8 is used to connect to the internal chamber of the cavity 1, and the catalytic intake transmission pipe 12 is used to connect to the external gas pipeline to realize gas flow and transportation.

[0028] The double-ferrule connectors 20 are respectively fitted onto the outer ends of the catalytic inlet transmission pipe 12 and the catalytic outlet 25. This facilitates rapid external piping, enabling the introduction of inert gases and reactive gases, and the discharge of reaction tail gases. It is suitable for various gas-solid phase catalytic reaction tests, such as CO2 reduction, hydrogenation, VOCs degradation, and nitrogen and sulfur fixation. The ambient temperature measuring port 23 is fixedly installed through the side wall of the cavity 1 for real-time monitoring of the internal ambient temperature of the cavity 1. The temperature control and monitoring interface 28 is fixedly installed on the outer end face of the sealing cover 2. This is used to connect external temperature control equipment to achieve the regulation of heating conditions and the transmission of temperature data.

[0029] The sensor support 9 is horizontally inserted through the side wall of the cavity 1, and its inner end extends to the side of the high-temperature heating sample platform 26 to mount the temperature sensing component. The pressure block 13 is fixed to the outer wall of the cavity 1 and covers the insertion position of the sensor support 9, thus both positioning and fixing the sensor support 9 and ensuring the airtightness of the insertion position on the side wall of the cavity 1. The electrical signal interface 15 is fixedly embedded in the sealing cover 2 and communicates with the interior of the cavity 1 for transmitting various electrical signals from within the device. Foot pads 21 are fixedly installed at the bottom of the cavity 1 to provide support and prevent slippage, ensuring the equipment is placed stably.

[0030] The porous, permeable ceramic 14 is neatly packed with precious metal catalysts such as Pt and Pd, as well as oxide catalysts such as TiO2 and CeO2, making it suitable for typical photothermal catalytic reactions such as methanol water vapor reforming, ethanol water vapor reforming, and biomass water vapor reforming to produce green hydrogen. The observation window 19 in the middle of the cavity cover 16 can be connected to an external xenon lamp light source to provide a stable incident light source for the catalytic reaction. With the heating plate 10 and temperature control system, precise temperature control in the low-temperature range can be achieved to meet the working conditions of photothermal coupling low-temperature catalysis.

[0031] A testing method for a photothermal catalysis tester includes the following steps: Step S1: Sample loading and sealing; Place the catalytic sample to be tested on the surface of the porous permeable ceramic 14, and place the entire porous permeable ceramic 14 on the stage 11. Cover with the shielding cover 7, close the chamber cover 16, and lock it with the chamber cover screws 18 and the chamber cover nut 17, and use the sealing ring 22 to seal the chamber 1.

[0032] Step S2, gas purging: Inert gas is introduced into the cavity 1 through the external pipeline via the catalytic intake transmission pipe 12 and the catalytic intake port 8 to purge and replace the air and impurity gas in the cavity 1. The waste gas is discharged from the catalytic outlet 25, so that the cavity 1 reaches the preset pure atmosphere.

[0033] Step S3: Temperature control and preheating; start the heating plate 10 to heat the high-temperature heating sample platform 26, and regulate the heating conditions through the temperature control and temperature monitoring interface 28; use the sensor support 9 and the ambient temperature measuring port 23 to synchronously collect temperature parameters, so that the sample area is stabilized at the set catalytic reaction temperature.

[0034] Step S4, photothermal coupling reaction: An external light source is incident on the sample surface through the observation window 19 to carry out a photothermal synergistic catalytic reaction; the external photothermal interference is isolated by the first shielding layer 3, the second shielding layer 4, the temperature shielding layer 27, and the quartz cover temperature shielding layer 24, which not only keeps the temperature, but also increases the residence time of the reaction gas inside the quartz cover temperature shielding layer, so that it will not diffuse directly.

[0035] When conducting the photothermal reforming experiment to produce green hydrogen, the xenon lamp light source is aimed at the observation window 19 to complete the lighting. Methanol vapor, ethanol vapor or biomass mixed water vapor are introduced into the cavity 1 as reaction raw materials. The heating plate 10 provides a low-temperature heat source. The catalyst undergoes a reforming reaction under the synergistic effect of light and low-temperature heating, continuously generating hydrogen-containing product gas. The product gas is discharged outward from the catalytic outlet 25 and can be connected to external detection equipment to complete component analysis.

[0036] Step S5: Steady-state data acquisition; Maintain a constant gas supply flow rate through the catalytic inlet transmission pipe 12 and the catalytic inlet 8 to keep the reaction atmosphere in the chamber 1 stable. Continuously acquire relevant test data on temperature, atmosphere, and catalytic reaction throughout the process to complete the steady-state catalytic test.

[0037] Step S6: Stop and reset; stop the operation of the light source and heating plate 10, continuously purge and cool the chamber with inert gas through the catalytic gas inlet transmission pipe 12 and catalytic gas inlet 8, and after the chamber 1 returns to normal temperature and pressure, open the chamber cover 16 to take out the sample and complete the test.

[0038] Therefore, the present invention employs the above-mentioned photothermal catalysis tester and test method, which features a reliable sealed cavity, stable flow of the split-type air inlet path, multi-layer shielding to isolate photothermal interference, precise temperature measurement and control, uniform sample loading, high integration, and the ability to stably complete gas-solid phase photothermal catalysis tests with accurate and repeatable data.

[0039] The above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the technical solutions of the present invention; and these modifications or equivalent substitutions cannot cause the modified technical solutions to deviate from the spirit and scope of the technical solutions of the present invention.

Claims

1. A photothermal catalysis testing instrument, characterized in that, The system includes a cavity, a sealing cap, a first shielding layer, a second shielding layer, a support plate, a pad, a shielding cover, a catalytic inlet, a sensor support, a heating plate, a stage, a catalytic inlet transmission pipe, a pressure block, a porous permeable ceramic, an electrical signal interface, a cavity cover, a cavity cover nut, a cavity cover screw, an observation window, a double compression fitting, foot pads, a sealing ring, an ambient temperature measuring port, a quartz cover temperature shielding layer, a catalytic outlet, a high-temperature heating sample platform, a temperature shielding layer, and a temperature control and monitoring interface. The sealing cap is sealed at one end of the cavity and is assembled into the top opening of the cavity. The pad and support plate are sequentially fixed to the bottom side inside the cavity. The heating plate is installed above the support plate, the high-temperature heating sample platform is fixed on the heating plate, the stage is located on top of the high-temperature heating sample platform, and the porous permeable ceramic is placed on the stage.

2. The photothermal catalysis testing instrument according to claim 1, characterized in that, The cavity cover is locked and fixed to the cavity body by cavity cover screws and cavity cover nuts, and the sealing ring is sandwiched between the mating end faces of the cavity cover and the cavity body.

3. The photothermal catalysis testing instrument according to claim 2, characterized in that, The observation window is embedded in the middle of the cavity cover, and the quartz cover temperature shielding layer is fixed inside the cavity cover and arranged below the observation window.

4. The photothermal catalysis testing instrument according to claim 3, characterized in that, The second shielding layer is wrapped around the outside of the heating plate and the high-temperature heating sample platform, the first shielding layer is wrapped around the outside of the second shielding layer, and the temperature shielding layer is wrapped around the outside of the first shielding layer.

5. A photothermal catalysis testing instrument according to claim 4, characterized in that, The shielding cover is fixedly installed inside the cavity, on the inner side of the end near the sealing cover.

6. The photothermal catalysis testing instrument according to claim 5, characterized in that, The catalytic inlet and catalytic outlet are respectively fixed to the side wall of the cavity, and the catalytic inlet transmission pipe is connected and assembled to the outer port of the catalytic inlet.

7. A photothermal catalysis testing instrument according to claim 6, characterized in that, The double-ferrule connectors are respectively assembled on the outer end of the catalytic intake transmission pipe and the outer end of the catalytic outlet.

8. The photothermal catalysis testing instrument according to claim 7, characterized in that, An ambient temperature measuring port is fixed to the side wall of the cavity, and a temperature control and monitoring interface is fixedly installed on the outer end face of the sealing cover.

9. A photothermal catalysis testing instrument according to claim 8, characterized in that, The sensor support is horizontally inserted through the side wall of the cavity, and the inner end of the sensor support extends to the side of the high-temperature heating sample platform. The pressure block is fixed to the outer wall of the cavity and covers the insertion position of the sensor support. The electrical signal interface is fixedly embedded in the sealing cover and connected to the inside of the cavity. The bottom of the cavity is fixedly installed with foot pads.

10. The testing method of the photothermal catalysis tester according to claim 9, characterized in that, Includes the following steps: Step S1, Sample loading and sealing; Place the catalytic sample to be tested on the surface of the porous permeable ceramic and spread it evenly, and place the entire porous permeable ceramic on the stage; Close the chamber cover and lock it with the chamber cover screws and nuts, and use the sealing ring to achieve the chamber seal; Step S2, Gas Replacement: Inert gas is introduced into the cavity through the external pipeline via the catalytic intake transmission pipe and the catalytic intake port to purge and replace the air and impurity gas in the cavity. The waste gas is discharged from the catalytic outlet, so that the cavity reaches the preset pure atmosphere. Step S3: Temperature control and preheating; start the heating plate to heat the high-temperature heating sample platform, and regulate the heating conditions through the temperature control and temperature monitoring interface; use the sensor support and the ambient temperature measurement port to collect temperature parameters synchronously, so that the sample area is stabilized at the set catalytic reaction temperature; Step S4, photothermal coupling reaction: An external light source is incident on the sample surface through the observation window to carry out a photothermal synergistic catalytic reaction; external photothermal interference is isolated by the first shielding layer, the second shielding layer, the temperature shielding layer, and the quartz cover temperature shielding layer. Step S5: Steady-state data acquisition; Maintain a constant gas supply flow rate through the catalytic inlet and catalytic gas inlet to keep the reaction atmosphere in the chamber stable; Continuously acquire relevant test data on temperature, atmosphere, and catalytic reaction throughout the process to complete the steady-state catalytic test; Step S6: Stop and reset; stop the light source and heating plate from working, continuously purge and cool the chamber with inert gas through the catalytic gas inlet and catalytic gas inlet, and after the chamber returns to normal temperature and pressure, open the chamber cover and take out the sample to complete the test.

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