CN109187410B - Infrared detection device of atmospheric reflection of a segmentation plasma catalysis normal position - Google Patents
Infrared detection device of atmospheric reflection of a segmentation plasma catalysis normal position Download PDFInfo
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Abstract
The invention relates to a one-section type plasma catalysis in-situ diffuse reflection infrared detection device. An in-situ infrared method is used to understand the role of plasma in the catalytic reaction mechanism, and a method for optimizing the operation parameters of the catalyst and the plasma is provided. The invention provides a detailed description of the design of the infrared diffuse reflection pool for the plasma synergistic heterogeneous catalytic reaction. The working gas is introduced into the gas chamber and discharged at the catalytic bed layer, the discharge tube and the window support are fixedly sealed by a PTFE screw, and the tail end of the high-voltage electrode is connected with an insulating pad, inserted from the bottom end of the discharge tube and leveled with the upper surface of the catalytic bed layer. The detection signal penetrates through the window and generates diffuse reflection on the surface of the sample to be detected, and then the detection signal is converged and transmitted to the detector through the concave lens. The invention can realize in-situ infrared on-line monitoring of the one-stage plasma catalytic reaction process, provides an important characterization means for reaction mechanism discussion, and has the advantages of simple operation and wide application range.
Description
Technical Field
The invention relates to a one-section type plasma catalysis in-situ diffuse reflection infrared detection device, which mainly comprises a related design for a reactor window and a one-section type plasma discharge reactor.
Background
From PM, VOCs and NOxThe problem of causing air pollution is increasingly prominent, so that the development of an efficient and convenient solution is urgent. The electrostatic dust removal method has already been developed in stages for the treatment of main industrial PM pollution sources in China, such as coal-fired power plants, heating boilers and the like, and the methods of catalytic combustion, microbial degradation and the like are adopted to purify trace VOCs waste gas in industrial waste gas, but the method has a primary effect on industrial NOxAt present, no effective treatment scheme exists, and research work is still in continuous exploration. The adoption of the hydrocarbon selective catalytic reduction method is considered to be one of the most promising effective means for solving the nitrogen oxides in the future. Currently, a three-way catalyst system NH is adopted in treatment of tail gas and waste gas of mobile source3SCR has been widely used for heavy-duty diesel truck tail gas remediation, but with the concomitant production of ammoniaThe problem of leakage and the like is still not negligible, and therefore, it cannot be used as a moving source NOxThe main technical means of removal.
With the continuous deepening of plasma research work of scientific research groups in various countries, the combination of hydrocarbon selective catalytic reduction and a plasma catalysis method has been proved to be capable of effectively improving NOxThe removal efficiency can delay the inactivation of the catalyst to a certain extent, so that the application of the low-temperature plasma technology to the treatment of industrial waste gas becomes possible. However, for the cooperative reaction, especially for the "packed bed type" plasma catalytic reaction, the whole reaction process is complicated due to the generation of a large amount of active particles such as electrons, free radicals, excited molecules, atoms and the like in the discharge process, and the important reaction process is difficult to be directly and effectively detected by the conventional technical means, so that the research on the cooperative mechanism of the plasma catalysis is challenged. Species change in the reaction process is detected by adopting an in-situ diffuse reflection Fourier transform infrared spectrum, so that the method is widely applied to the heterogeneous catalytic reaction process, and provides a plurality of important reference bases for researching the reaction mechanism. At present, the commercial in-situ diffuse reflection pool can not realize 'one-stage' plasma discharge, and a method for analyzing surface species in the plasma catalytic reaction process by adopting an in-situ infrared diffuse reflection spectrum method does not exist, so that the exploration of a plasma catalytic synergistic mechanism is limited to a great extent.
Disclosure of Invention
The invention provides a one-section type plasma catalysis in-situ diffuse reflection infrared generation device, which can realize the in-situ detection of the plasma catalysis synergistic process.
The specific technical scheme of the invention is as follows:
the invention mainly comprises the following steps: observation window, insulating pad, discharge tube, heating ring and support frame. The conical supporting part is respectively provided with openings on three sides of a conical surface, a quartz window sheet is embedded on the front side of the conical supporting part and used as an observation window, the left side and the right side of the conical supporting part are symmetrically provided with openings and are embedded with zinc selenide window sheets and used as infrared windows, the upper end and the lower end of the conical supporting part are respectively provided with an opening, the upper end of the conical supporting part is connected with the air inlet pipe through threads, the lower end of the conical supporting part is fixed with the discharge tube through a tetrafluoro screw, and the opening on the side surface of the discharge tube is connected with an air outlet. The gas flows into the catalytic bed layer of the discharge chamber from the gas inlet pipe at the top of the observation window to be discharged and then flows out from the gas outlet pipe. The high-voltage electrode is inserted from the lower end of the discharge tube, the protection tube is sleeved on the outer side of the high-voltage electrode to prevent creepage, the high-voltage electrode is fixed at the center of the discharge tube by the fixing ring, the lower end of the high-voltage electrode is connected with the insulating pad, and the O-shaped ring is sleeved in the groove on the side surface of the insulating pad and inserted into the reaction tube. The grounding electrode is tightly wrapped on the periphery of the discharge tube, a heating ring is sleeved on the outer side of the grounding electrode, and a gap between the heating ring and the grounding electrode is filled with quartz cotton. One end of the supporting frame is opened and is provided with two movable knife-shaped sliding sheets for fixing the reactor, and the other end of the supporting frame is combined with the three-dimensional adjusting frame and is fixed on the experiment table.
In a preferred embodiment of the present invention, the window supporting portion and the air inlet pipe are made of an insulating material with good insulation, such as polytetrafluoroethylene or nylon.
In a preferred embodiment of the present invention, the high voltage electrode is made of a metal material with good electrical conductivity, such as a tungsten needle, a white steel needle, or a copper rod.
In a preferred embodiment of the present invention, the discharge tube, the protection tube, and the gas outlet tube are made of quartz glass, alumina ceramic, or corundum.
In a preferred embodiment of the present invention, the insulating pad is made of nylon or teflon.
The working process of the invention is as follows: the high-voltage electrode is inserted from the lower end of the discharge tube and fixed by the fixing ring, the catalyst is filled between the high-voltage electrode and the grounding electrode in the discharge tube, and the filling amount is ensured to be level to the top of the electrode and compacted. The air inlet pipes and the air outlet pipes at two ends of the reactor are connected and fixed on the support frame respectively, the support frame is connected with the three-dimensional adjusting frame and integrally fixed on the workbench, and the position of the reactor in the diffuse reflection pool is adjusted to enable the reactor to achieve measurable infrared signal intensity. Working gas is introduced, the temperature is raised to the temperature required by the reaction, the power supply provides proper discharge voltage and discharge frequency after the high-voltage electrode is connected with the power supply, plasma generated in the catalytic bed generates infrared absorption on adsorbed species generated on the surface of the catalyst under a detection signal, and the infrared absorption is acquired by an MCT detector and then transmitted to a computer to be drawn into an infrared spectrum.
Compared with the prior art, the invention has the following advantages:
at present, many reports and researches are carried out on the adoption of plasma to activate heterogeneous catalytic reaction, but few people use an in-situ infrared method to understand the combination mechanism of plasma and catalyst reaction in real time and on line so as to provide a method for optimizing the parameters of the catalyst and the plasma, the existing commercial diffuse reflection in-situ pool can only meet the discussion of a simple catalytic reaction process, and plasma discharge cannot be realized. In order to ensure the air tightness of the device, the air inlet pipe and the window support are both made of polytetrafluoroethylene made of the same material and are sealed through threaded connection, the trend of the air pipe cannot influence sampling signals due to the fact that the window sheet is shielded, and the window support made of polytetrafluoroethylene with good insulating property mainly aims to prevent the creepage phenomenon in the plasma generation process and enable the discharge process to be safer and more stable. The melting point of the polytetrafluoroethylene material is 327 ℃, which can meet the requirement of the upper limit of the temperature in the experimental process. In addition, the included angle between the embedded infrared window and the bottom surface is 45 degrees, so that the incident infrared light can vertically penetrate through the zinc selenide window sheet and irradiate on the sample bed layer, and the detector can receive a detection signal to the maximum extent.
The invention is different from the design of the existing 'two-stage method' discharge reactor for researching plasma catalysis by adopting in-situ diffuse reflection infrared, the discharge mode of the invention is still wire-cylinder dielectric barrier discharge, the catalyst is filled between the high-voltage electrode and the grounding electrode, and simultaneously the plasma can be ensured to act on the upper surface of the catalytic bed layer, so that the detection signal can detect the change of surface adsorption state species in the reaction process. Therefore, the invention most directly explains the 'one-stage' plasma and catalyst reaction process and reaction combination mechanism by using an in-situ method.
Drawings
Fig. 1 and 2 are schematic structural views of embodiment 1 of the present invention.
FIG. 3 is a diffuse reflectance infrared spectrum of example 2 of the present invention.
In the figure, 1, a conical shell, 2, an infrared window, 3, an infrared window, 4, an observation window, 5, an air inlet pipe, 6, a heating ring, 7, an air outlet pipe, 8, a high-voltage electrode, 9, a discharge tube, 10 a protection tube, 11, an insulating ring, 12, an insulating pad, 13, a polytetrafluoroethylene screw rod, 14, an air chamber, 15, a threaded port and 16, a grounding electrode are arranged.
Detailed Description
The invention is explained in more detail below with reference to the figures 1-3 and the examples.
Embodiment 1 a "one-stage" plasma catalysis in-situ diffuse reflection infrared detection device, as shown in fig. 1 and 2, a working gas enters a gas chamber 14 through an inlet pipe 5, the end of the inlet pipe is connected with the top of a window support 1 through a thread 15, 2 and 3 are zinc selenide windows 4 which are quartz windows, the lower end of an observation window is connected with a discharge tube 9 and fixed through a tetrafluoro screw 13, the end of a high voltage electrode 8 is inserted into an insulating pad 12, the top of the high voltage electrode 8 is inserted from the bottom to the top of the discharge tube 9 and fixed to be level with the top of a ground electrode, the protection tube 10 is sleeved into the bottom of the high voltage electrode 8, the insulating ring 11 is sleeved into the high voltage electrode 8 and placed at the upper end of the protection tube 10, the right side of the discharge tube 9 is opened and connected with an outlet tube 7, the ground electrode 16 is tightly connected with the upper end of the discharge tube 9, the ground electrode 16 is externally connected with a ceramic heating ring 6, and the discharge tube, the protection tube, the ground electrode 16 is connected with a ceramic heating ring, The air outlet pipe is made of quartz glass, the air inlet pipe and the window support are made of polytetrafluoroethylene, the high-voltage electrode is made of tungsten needles and white steel needles, and the grounding electrode is made of white steel meshes and copper foils.
Example 2
A 'one-segment' plasma catalysis in-situ diffuse reflection infrared detection device is characterized in that one end of an air inlet pipe 5 is connected with a threaded port 15 in the center of the top end of a conical shell 1, three sides of the side surface of the conical shell 1 are open, a quartz window 4 is embedded in the front surface of the conical shell to serve as an observation window, two symmetrical openings are arranged on the left side and the right side of the conical shell, zinc selenide window sheets 2 and 3 are embedded in the two sides of the conical shell to serve as infrared windows, the bottom end of the conical shell 1 is in contact with the plane part of the top end of a discharge tube 9, the contact surfaces of the two parts are fixed through four tetrafluoro screws 13 penetrating through the two contact surfaces, the two parts are tightly connected, the end points of different tetrafluoro screws 13 in the same plane are sequentially connected to form a square, one end of the discharge tube 9 is connected with the bottom end of the conical shell 1, the other end of the discharge tube is provided with an insulating pad 12, a fixing ring 11 is arranged in parallel with a certain distance from the hollow interior of the discharge tube 9, one end of a high-voltage electrode 8 is in contact with the center of the insulating pad 12, the other end passes through the center of the fixing ring 11 and is exposed in the air, the high-voltage electrode 8 is vertical to the plane of the insulating pad 12, the high-voltage electrode 8 between the fixing ring 11 and the insulating pad 12 is sleeved with a protection tube 10, the outer end of the discharge tube 9 is wrapped with a ceramic heating ring 6 from the fixing ring 11 to the top end of the discharge tube 9, and a gap between the inner wall of the ceramic heating ring 6 and the outer surface of the discharge tube 9 is filled with quartz cotton. The outer side of the bottom end of the discharge tube 9 is tightly wrapped with a grounding electrode 16, the grounding electrode 16 is contacted with the ground, and the side surface of the discharge tube 9 is connected with the air outlet 7.
Example 2
Experimental parameters: a high-voltage alternating-current power supply is used as output, the discharge voltage is 12kV, and the discharge frequency is 6 kHz; the working gas is C2H2、NO、O2、N2As the balance gas, the total flow rate of the gas flow is 150mL/min, and the loading of the catalyst is 0.5 g.
Parameters such as gas flow, reaction temperature, reaction time, discharge voltage, frequency and the like are controlled to be unchanged in the experimental process. Comparison of different atmospheres C under the same conditions2H2+O2、NO+O2、C2H2+O2+ NO in Ag/Al2O3The influence of adsorbed species generated on the surface of the catalyst. FIG. 3 is a graph comparing the effect of generating adsorbed species on the surface of a catalyst with or without discharge. By comparison of C2H2+O2+ NO four-component Ag/Al without discharge2O3The experimental result shows that the plasma plays an important role in the activation reaction, and more surface intermediate species are generated compared with the surface intermediate species generated in the simple catalytic reaction process, especially for 2235 cm-1and-NCO species of (1) and 1336cm-1The enol form and the like of (A) have been widely regarded as important intermediate species for improving the activity, and the generation of the intermediate species plays a remarkable promoting role.
Claims (1)
1. A method for detecting by adopting a one-section type plasma catalysis in-situ diffuse reflection infrared detection device,
the device is characterized in that the detection device detects the plasma catalysis synergistic process on line under the in-situ condition and comprises an observation window (4), an infrared window, an air inlet pipe (5), an air outlet pipe (7), a high-voltage electrode (8), a grounding electrode (16), a discharge pipe (9), a protection pipe (10), a fixing ring (11), an insulation pad (12), a heating ring (6) and a support frame,
the observation window (4) and the conical shell (1) supporting the infrared window are of conical structures, window sheets are inlaid on the conical surface and are respectively used as the observation window and a transmission infrared window, the included angle between the infrared window and the bottom surface is 45 degrees, the upper end and the lower end of the infrared window are respectively provided with an opening, the upper end of the infrared window is connected with the air inlet pipe (5), the lower end of the infrared window is connected with the discharge tube (9), the top end of the high-voltage electrode (8) penetrates through a fixing ring (11) to the air chamber, the tail end of the high-voltage electrode (8) is connected with an insulating pad (12), a protection pipe (10) is sleeved on the outer side of the high-voltage electrode (8), a grounding electrode (16) is wrapped on the periphery of the discharge tube (9), a heating ring (6) is sleeved on the outer side of the grounding electrode, one end of the support frame is provided with an opening and is used for fixing the reactor through two movable knife-shaped slip sheets, and the other end of the support frame is connected with a three-dimensional adjusting frame;
the method comprises the following steps of:
inserting the high voltage electrode (8) from the lower end of the discharge tube (9) and fixing by the fixing ring (11), and Ag/Al2O3The catalyst is filled between a high-voltage electrode (8) and a grounding electrode (16) in a discharge tube (9) and the filling amount is ensured to be level to the top of the electrode and compacted;
connecting an air inlet pipe (5) and an air outlet pipe (7) at two ends of the reactor respectively and fixing the air inlet pipe and the air outlet pipe on a support frame, connecting the support frame with a three-dimensional adjusting frame and integrally fixing the support frame on a workbench, and adjusting the position of the reactor in a diffuse reflection pool to enable the reactor to achieve the purpose of measuring the infrared signal intensity;
working gas is introduced and the temperature is raised to the temperature required by the reaction, after the high-voltage electrode (8) is connected with a power supply, the power supply provides proper discharge voltage and discharge frequency, and plasma generated in the catalytic bed layer is Ag/Al2O3The adsorbed species generated on the surface of the catalyst generate infrared rays under the detection signalAbsorbing, collecting by MCT detector, and drawing into infrared spectrum by computer;
the experimental parameters were: a high-voltage alternating-current power supply is used as output, the discharge voltage is 12kV, and the discharge frequency is 6 kHz; the working gas is C2H2NO and O2， N2As balance gas, the total flow rate of the gas flow is 150mL/min, Ag/Al2O3The catalyst loading was 0.5 g;
the window supporting part is made of polytetrafluoroethylene, the observation window (4) is made of quartz glass, and the infrared window is made of zinc selenide;
the high-voltage electrode (8) is made of a white steel needle or a tungsten needle, and the grounding electrode (16) is made of a white steel net or a copper foil;
the discharge tube (9) and the protective tube (10) are both made of quartz glass;
the fixing ring (11) is made of ceramics, and the insulating pad (12) is made of nylon material or polytetrafluoroethylene material;
the heating ring (6) is mainly made of ceramic materials.
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| CN109682771B (en) * | 2019-02-21 | 2020-09-15 | 中国科学院力学研究所 | Gas detection device |
| CN109827924A (en) * | 2019-02-21 | 2019-05-31 | 中国科学院力学研究所 | A kind of gas-detecting device |
| CN110296938A (en) * | 2019-06-11 | 2019-10-01 | 江苏大学 | In-situ ft-ir reaction unit under a kind of freelymoving rats atmosphere |
| CN110296939A (en) * | 2019-06-11 | 2019-10-01 | 江苏大学 | A kind of Energetic Materials by In-Situ Diffuse Reflection reaction tank that plasma environment can be provided |
| CN110514593A (en) * | 2019-08-26 | 2019-11-29 | 江苏大学 | A kind of Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge |
| CN114199774A (en) * | 2021-11-12 | 2022-03-18 | 江苏大学 | In-situ transmission infrared reaction tank under action of jet plasma and testing method |
| CN114505978A (en) * | 2022-03-11 | 2022-05-17 | 聊城鲁西聚酰胺新材料科技有限公司 | Online index detection device, production system and method for nylon 6 dry slices |
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