Thermal radiation catalytic reaction device and mass spectrometry system
By designing a thermal radiation catalytic reaction device and mass spectrometry analysis system, combined with vacuum ultraviolet photoionization and ultrasonic molecular beam sampling technology, the problem of difficulty in real-time capture and analysis of gas-phase intermediates of thermal radiation catalytic reactions in the prior art is solved, and efficient and rapid reaction product detection is achieved.
Patent Information
- Application Number
- CN202421772577.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-24
- Publication Date
- 2025-03-28
- Estimated Expiration
- 2034-07-24
AI Technical Summary
The prior art is difficult to capture gas-phase intermediates of thermal radiation catalytic reactions in real time and online, and combine them with mass spectrometry analysis methods based on photoionization, resulting in inconvenience in studying the mechanism of thermal radiation catalytic reactions.
A thermal radiation catalytic reaction device is designed, including a transparent reaction tube and radiation source, mass spectrometry analysis is performed through a vacuum ultraviolet photoionization source, and combined with ultrasonic molecular beam sampling technology, in-situ on-site detection of reaction products is achieved.
Real-time, online capture and mass spectrometry analysis of gas-phase intermediates of thermal radiation catalytic reactions is achieved, and the problems of many fragments and slow chromatographic separation in traditional GC-MS methods are overcome, and the multi-component system can be detected quickly and accurately.
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Figure CN222678064U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the technical field of detection and analysis, and specifically relates to a thermal radiation catalytic reaction device and a mass spectrometry analysis system. Background Art
[0002] Photothermal catalytic reaction is a new technology that integrates photocatalytic reaction with thermal catalytic reaction. This technology has been proven to have considerable advantages in reactor engineering and catalytic performance.
[0003] Thermal radiation catalytic reaction is a method of coupling photocatalysis to thermal reaction using thermal radiation. It emits thermal radiation in a specific spectral range through a heating module, and is absorbed by molecules with the corresponding thermal radiation spectrum absorption capacity to catalyze the reaction. According to Planck's law, the blackbody radiation spectrum with a temperature between 500℃ and 1000℃ is mainly located in the infrared region between 1000nm and 10000nm, and the higher the temperature, the higher the total energy radiated, and the more short-wave components. Therefore, it is expected that the spectral distribution of blackbody radiation can be controlled by temperature regulation, so that thermal radiation can be used for catalytic reactions.
[0004] In the process of thermal radiation catalytic reaction, reactants will produce a large number of stable or unstable products. Real-time and online acquisition of the composition and spatial distribution of these products is of great significance for studying the detailed reaction kinetic mechanism in the process of thermal radiation catalytic reaction. At present, the main analytical methods for detecting the molecular structure of reaction products are in-situ spectral diagnosis and sampling analysis. In-situ spectral diagnosis does not interfere with the reaction system, but can only measure a few species. Sampling analysis generally uses a capillary or sampling cone to sample the reaction products, and then uses mass spectrometry (MS) or gas chromatography-mass spectrometry (GC-MS) for analysis. Sampling analysis is currently an effective method for obtaining most of the intermediate information in the process of thermochemical reaction. However, traditional GC-MS uses an electron impact ionization source (EI-MS) in a "hard" ionization method to ionize the analyte, thereby generating a large number of fragment ion peaks, and even cannot obtain the molecular ion peak of the analyte, which brings difficulties to the qualitative analysis of the analyte.
[0005] In-situ molecular beam sampling-photoionization time-of-flight mass spectrometry can solve the problems of GC-MS in detection, and has been verified in the application of capturing gas-phase reaction intermediates in reactions such as pyrolysis and catalysis. Vacuum ultraviolet photoionization is a "soft" ionization method that produces almost no fragment ions, and the products do not need chromatographic separation. It overcomes the shortcomings of EI-MS ionization, which produces many fragments and slow chromatographic separation, and can achieve rapid, in-situ online detection of multi-component systems. The ionization source of in-situ molecular beam sampling-photoionization time-of-flight mass spectrometry is a vacuum ultraviolet lamp or synchrotron vacuum ultraviolet light. Synchrotron vacuum ultraviolet light has the advantages of high brightness, high energy resolution, and tunability, and is extremely suitable for the analysis of complex systems. Ultrasonic molecular beams can "cool" gas-phase molecules, which is very suitable for the detection of gas-phase intermediates in thermal radiation catalytic reactions, and then study their reaction mechanism. However, there is currently a lack of a device that can capture gas-phase intermediates in thermal radiation catalytic reactions in situ and combine it with a mass spectrometry analysis method based on photoionization, which brings inconvenience to the study of the mechanism of thermal radiation catalytic reactions. Utility Model Content
[0006] The utility model aims to provide a thermal radiation catalytic reaction device and a mass spectrometry analysis system.
[0007] To achieve the above object, the utility model provides a thermal radiation catalytic reaction device, comprising:
[0008] The heat-insulating shell is a hollow structure having a first inner cavity;
[0009] A transparent reaction tube, at least partially inserted into the first inner cavity;
[0010] A radiation source is at least partially disposed in the first inner cavity; the radiation source is spaced apart from and arranged in parallel with the reaction tube, and comprises a radiation tube, an inner liner tube and a first heating wire, the inner liner tube is at least partially penetrated in the tube cavity of the radiation tube, and the first heating wire is at least wound around the outer circumference of the portion of the inner liner tube located in the tube cavity of the radiation tube.
[0011] Optionally, there are multiple radiation sources, and the multiple radiation sources are arranged at intervals in the circumferential direction of the reaction tube.
[0012] Optionally, the heat-insulating shell is provided with two mounting holes, which are arranged opposite to each other; the axial ends of the reaction tube respectively pass through the two mounting holes and extend to the outside of the heat-insulating shell;
[0013] The heat radiation catalytic reaction device further includes a second heating wire, which is wound at least around the outer circumference of the portion of the reaction tube located in the first inner cavity and the mounting hole.
[0014] Optionally, the thermal radiation catalytic reaction device also includes a temperature monitoring component, which includes a first temperature monitoring element and a second temperature monitoring element. The first temperature monitoring element is arranged in the tube cavity of the inner lining tube, and the second temperature monitoring element is arranged on the outer surface of the part of the second heating wire located in the insulation shell.
[0015] Optionally, the thermal radiation catalytic reaction device further includes an ultrasonic molecular beam injection component, which includes a joint shell and a nozzle; the joint shell is a hollow structure having a second inner cavity, and the joint shell is provided with a first through hole and a second through hole communicating with the second inner cavity, the first through hole is arranged opposite to the second through hole, and the aperture of the first through hole is smaller than the aperture of the second through hole; the nozzle is connected to the second through hole, and is partially located in the second inner cavity, and is coaxially arranged with the first through hole; the inner diameter of the nozzle gradually increases in a direction away from the first through hole;
[0016] The reaction tube is sealed and connected to the joint shell at the first through hole, and the reaction tube is communicated with the second inner cavity.
[0017] Optionally, the ultrasonic molecular beam injection assembly further includes a third heating wire, which is located in the second inner cavity and is wound around at least a portion of the outer side wall of the nozzle.
[0018] Optionally, the joint shell is further provided with a third through hole communicating with the second inner cavity, the third through hole is provided with an air extraction pipeline, and the air extraction pipeline is provided with a valve.
[0019] Optionally, the reaction tube includes a first tube and a second tube, the first tube includes a tube body and a coupling ring, the coupling ring is connected to one end of the tube body and is located outside the thermal insulation shell; the coupling ring is sealed and connected to the coupling shell; the second tube is partially inserted into the tube cavity of the first tube and is coaxially arranged with the first through hole; the outer peripheral surface of one end of the second tube away from the first through hole is sealed and connected to the first tube.
[0020] To achieve the above-mentioned purpose, the utility model also provides a mass spectrometry analysis system, comprising a mass spectrometer and the thermal radiation catalytic reaction device as described above, wherein the mass spectrometer is connected to the reaction tube.
[0021] Optionally, the mass spectrometer comprises an ionization source joint, wherein the ionization source joint is used to connect to an ionization source; the ionization source is a vacuum ultraviolet photoionization source.
[0022] Compared with the prior art, the thermal radiation catalytic reaction device and mass spectrometry analysis system of the utility model have the following advantages:
[0023] The aforementioned thermal radiation catalytic reaction device includes a heat-insulating shell, a transparent reaction tube and a radiation source; the heat-insulating shell is a hollow structure with a first inner cavity; the reaction tube is at least partially penetrated in the first inner cavity; the radiation source is at least partially penetrated in the first inner cavity; the radiation source is arranged in parallel with the reaction tube and includes a radiation tube, a liner tube and a first heating wire, the liner tube is at least partially penetrated in the tube cavity of the radiation tube, and the first heating wire is at least spirally wound on the outer circumference of the part of the liner tube located in the tube cavity of the radiation tube. When the first heating wire is energized, the first heating wire heats the radiation tube and causes the radiation tube to generate thermal radiation, and the thermal radiation generated by the radiation tube can be transmitted to the reaction tube, and catalyze the reaction of the reactants in the reaction tube through light and heat. By controlling the current applied to the first heating wire, the temperature of the radiation tube is controlled, and then the range of the radiation spectrum of the radiation tube is controlled. BRIEF DESCRIPTION OF THE DRAWINGS
[0024] The accompanying drawings are used to better understand the present invention and do not constitute an improper limitation on the present invention.
[0025] Figure 1 It is a structural schematic diagram of a thermal radiation catalytic reaction device provided by the utility model according to one embodiment;
[0026] Figure 2 It is a partial structural schematic diagram of a thermal radiation catalytic reaction device provided by the utility model according to an embodiment, and the figure mainly shows a radiation source;
[0027] Figure 3 It is a partial structural schematic diagram of a heat radiation catalytic reaction device provided by the utility model according to an embodiment, and the figure mainly shows a reaction tube;
[0028] Figure 4 It is a schematic diagram of a mass spectrometry analysis system formed by combining a thermal radiation catalytic reaction device and a mass spectrometer provided by the utility model according to an embodiment;
[0029] Figure 5 This is a mass spectrum obtained when a mass spectrometry analysis system provided by the utility model according to one embodiment performs a thermal radiation catalytic reaction and analysis on an ethane and argon system;
[0030] Figure 6 The mass spectrum is obtained when the mass spectrometry analysis system provided by the utility model according to one embodiment performs thermal radiation catalytic reaction and analysis on an ethane and carbon dioxide system.
[0031] [Description of reference numerals is as follows]:
[0032] 10-thermal radiation catalytic reaction device, 20-mass spectrometer;
[0033] 100-insulation shell, 101-first inner cavity, 200-reaction tube, 210-first tube, 211-tube body, 212-joining ring, 220-second tube, 300-radiation source, 310-radiation tube, 320-liner tube, 330-first heating wire, 400-temperature monitoring assembly, 410-first temperature monitoring element, 420-second temperature monitoring element, 500-second heating wire, 600-ultrasonic molecular beam injection assembly, 610-joining shell, 611-second inner cavity, 612-first through hole, 613-second through hole, 614-third through hole, 620-nozzle, 630-third heating wire, 640-valve, 20-mass spectrometer, 700-four-way connector, 800-sample introduction part, 810-introduction shell, 820-guide, 900-ionization source joint. DETAILED DESCRIPTION
[0034] The following describes the implementation of the present invention through specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific implementations, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention. It should be noted that the illustrations provided in this embodiment only illustrate the basic concept of the present invention in a schematic manner, so the diagram only shows the components related to the present invention rather than drawing according to the number, shape and size of the components in the actual implementation. The type, quantity and proportion of each component in the actual implementation can be a random change, and the component layout type may also be more complicated.
[0035] In addition, each embodiment of the following description has one or more technical features, but this does not mean that the user of the present invention must implement all the technical features in any embodiment at the same time, or can only implement part or all of the technical features in different embodiments separately. In other words, under the premise of being possible to implement, those skilled in the art can selectively implement part or all of the technical features in any embodiment according to the disclosure of the present invention and according to the design specifications or implementation requirements, or selectively implement a combination of part or all of the technical features in multiple embodiments, thereby increasing the flexibility of the implementation of the present invention.
[0036] As used in this specification, the singular forms "one", "an", and "the" include plural objects, and the plural form "a plurality" includes more than two objects, unless the content clearly indicates otherwise. As used in this specification, the term "or" is generally used in a sense that includes "and / or", unless the content clearly indicates otherwise, and the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection. It can be a mechanical connection or an electrical connection. It can be directly connected or indirectly connected through an intermediate medium, and it can be a connection between two elements or an interactive relationship between two elements. Relational terms such as the terms "first", "second", etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations, nor do they indicate or imply relative importance or implicitly indicate the number of technical features indicated. It should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "axial", "radial", "circumferential" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0037] In order to make the purpose, advantages and features of the utility model clearer, the utility model is further described in detail below in conjunction with the accompanying drawings. It should be noted that the drawings are all in a very simplified form and are not in precise proportions, and are only used to conveniently and clearly assist in explaining the purpose of the embodiments of the utility model. The same or similar reference numerals in the drawings represent the same or similar components.
[0038] Figure 1 Schematic diagram of the structure of the thermal radiation catalytic reaction device provided by some embodiments of the utility model. Figure 1 As shown, the thermal radiation catalytic reaction device includes a heat-insulating shell 100, a transparent reaction tube 200 and a radiation source 300. The heat-insulating shell 100 is a hollow structure having a first inner cavity 101. The reaction tube 200 is at least partially disposed in the first inner cavity 101. The radiation source 300 is at least partially disposed in the first inner cavity 101 and is spaced apart from and arranged in parallel with the reaction tube 200. The structure of the radiation source 300 is as shown in FIG. Figure 2As shown, it includes a radiation tube 310, a liner tube 320 and a first heating wire 330. The liner tube 320 is at least partially inserted into the lumen of the radiation tube 310, and the first heating wire 330 is at least wound around the outer circumference of the liner tube 320 located in the lumen of the radiation tube 310.
[0039] When the thermal radiation catalytic reaction device is used, the reactants are preferably arranged in the lumen of the part of the reaction tube 200 located in the first inner cavity 101. By applying current to the heating wire 330, the first heating wire 330 generates heat, thereby heating the radiation tube 310, and causing the radiation tube 310 to be thermoluminescent and generate thermal radiation. In the first inner cavity 101, the thermal radiation generated by the thermal radiation tube 310 is transferred to the reaction tube 200 and further transferred to the lumen of the reaction tube 200 to act on the reactants in the reaction tube 200 and catalyze the occurrence of the reaction. It should be known that the spectral range of thermal radiation is related to temperature. Therefore, in the process of catalytic reaction, by controlling the value of the current applied to the first heating wire 330 according to the reaction conditions required by the reactants in the reaction tube 200, the temperature of the first heating wire 330 can be regulated, and then the temperature of the radiation tube 310 can be regulated, thereby regulating the spectral range of the thermal radiation generated by the radiation tube 310 to better catalyze the occurrence of the reaction.
[0040] It can be understood that the number of the radiation source 300 is one, or two, three, four, or even more, which is specifically set as needed. When the number of the radiation source 300 is multiple, the multiple radiation sources 300 are arranged at intervals in the circumferential direction of the reaction tube 200, preferably arranged at equal intervals. In addition, the distance between the thermal radiation source 300 and the reaction tube 200 is also set as needed.
[0041] The embodiment of the utility model has no special restrictions on the materials of the heat-insulating shell 100, the reaction tube 200, the inner lining tube 320 of the radiation source 300, and the radiation tube 310, as long as they can achieve the corresponding effect. In an optional embodiment, the heat-insulating shell 100 can be made of mullite, which has good heat-insulating effect and is easy to process. The material of the reaction tube 200 is quartz that is resistant to high temperature and has good transparency. Its infrared light transmittance cutoff value is about 5mm, which can adapt to the infrared absorption range of most reactants. The material of the radiation tube 310 can be alumina ceramic with high thermal radiation emissivity and high temperature resistance, and the material of the inner lining tube 320 can be high temperature resistance, such as alumina ceramic. The material of the first heating wire 330 can be iron-chromium-aluminum alloy. In addition, the embodiment of the utility model has no special restrictions on the specific sizes of the various components of the thermal radiation reaction device, and is specifically designed according to needs.
[0042] In the embodiment of the utility model, the radiation source 300 is preferably detachably connected to the heat-insulating shell 100, so as to increase or decrease the number of the radiation sources 300 according to actual needs and to perform maintenance on the radiation sources 300.
[0043] For further information, please refer to Figure 1 The thermal radiation catalytic reaction device further includes a temperature monitoring component 400, and the temperature detection component 400 includes at least a first temperature monitoring element 410 (such as Figure 1 and Figure 2 As shown in the figure, the first temperature detection element 410 is arranged in the lumen of the inner liner tube 320 to indirectly monitor the temperature of the first heating wire 330 by monitoring the temperature of the inner liner tube 320. The first temperature monitoring element 410 can be a K-type armored thermocouple. Preferably, the first temperature monitoring element 410 is coaxially arranged in the lumen of the inner liner tube 320. The temperature of the first heating wire 330 is determined according to the reaction temperature required by the reactants in the reaction tube 200.
[0044] In practice, the heat-insulating shell 100 is provided with two mounting holes (not marked in the figure), both of which are connected to the first inner cavity 101, and the two mounting holes are arranged opposite to each other. The axial ends of the reaction tube 200 pass through the two mounting holes respectively and extend to the outside of the heat-insulating shell 100.
[0045] Since there is a certain gap between the heat radiation tube 310 and the reaction tube 200, there is a loss when the heat radiation generated by the heat radiation tube 310 is transferred to the reaction tube 200. In addition, due to the shielding of the wall of the heat-insulating shell 100, the heat radiation cannot be directly transferred to the part of the reaction tube 200 located in the mounting hole. This results in that when the current passed through the first heating wire 330 is controlled according to the reaction requirements of the reactants in the reaction tube 200, so that when the first heating wire 330 reaches the set temperature, the temperature of the reaction tube 200 may be lower than the required reaction temperature.
[0046] In view of this, if Figure 1 and Figure 3 As shown, the heat radiation catalytic reaction device preferably further includes a second heating wire 500, which is wound around at least the outer circumference of the reaction tube 200 located in the first inner cavity 101 and the mounting hole. In this way, the reaction tube 200 can be heated by the second heating wire 500 to compensate for the loss of heat radiation, so that the temperature of the reaction tube 200 can reach and be maintained at the required reaction temperature.
[0047] Accordingly, if Figure 1As shown, the temperature monitoring assembly 400 further includes a second temperature monitoring element 420, and the second temperature monitoring element 420 is disposed on the portion of the second heating wire 500 located in the heat-insulating shell 100 to monitor the temperature of the second heating wire 500. Here, “the portion of the second heating wire 500 located in the heat-insulating shell 100” includes the portion of the second heating wire 500 located in the first inner cavity 101 and / or the portion located in the mounting hole.
[0048] It is understandable that if Figure 1 and Figure 3 , Figure 4 As shown, the thermal radiation catalytic reaction device further includes a four-way joint 700, and the four-way joint 700 includes four joint parts. Among them, one of the joint parts is connected to the reaction tube 200, and the other three joint parts are connected to the reactant supply pipeline or the carrier gas pipeline according to actual needs, so as to introduce the reactant and / or the carrier gas into the reaction tube 200.
[0049] For further information, please refer to Figure 4 The thermal radiation catalytic reaction device is used to connect with the mass spectrometer 20, so as to use the mass spectrometer 20 to perform in-situ detection of the reaction products of the catalytic reaction carried out in the reaction tube 200. Therefore, one end of the reaction tube 200 can be connected with the mass spectrometer 20 to allow the reaction products to directly enter the mass spectrometer 20.
[0050] In a preferred embodiment, the thermal radiation catalytic reaction device further comprises an ultrasonic molecular beam injection assembly 600, which connects the reaction tube 200 and the mass spectrometer 20, so that the reaction product can enter the mass spectrometer 20 in the form of an ultrasonic molecular beam. Preferably, the mass spectrometer 20 uses vacuum ultraviolet light as ionization energy. The combination of ultrasonic molecular beam sampling and fragment-free soft ionization technology can detect the reaction product in situ without destroying the chemical structure or initial chemical inventory of the reaction product.
[0051] In an optional embodiment, if Figure 1As shown, the ultrasonic molecular beam injection assembly 600 includes a joint shell 610 and a nozzle 620. The joint shell 610 is a hollow structure having a second inner cavity 611, and the joint shell 610 is also provided with a first through hole 612 and a second through hole 613 communicating with the second inner cavity 611, and the first through hole 612 and the second through hole 613 are arranged relative to each other, for example, the two are arranged coaxially. The aperture of the first through hole 612 is smaller than the aperture of the second through hole 613. The nozzle 620 is connected to the second through hole 613 and is partially located in the second inner cavity 611. The nozzle 620 is coaxially arranged with the first through hole 612, and the inner diameter of the nozzle 620 gradually increases in the direction away from the first through hole 612. Those skilled in the art can understand that the reaction product flowing out of the reaction tube 200 is formed into an ultrasonic molecular beam form after being insulated and expanded by the nozzle 620. The material of the nozzle 620 can be quartz.
[0052] The joint housing 610 is sealed and connected to the reaction tube 200 at the first through hole 612 , and preferably the reaction tube 200 is coaxially arranged with the first through hole 612 . Thus, the reaction tube 200 is connected to the second inner cavity 611 through the first through hole 612 .
[0053] For more details, please refer to Figure 1 and Figure 3 , Figure 4 The reaction tube 200 includes a first tube 210 and a second tube 220. The first tube 210 includes a tube body 211 and a coupling ring 212, wherein the coupling ring 212 is connected to one end of the tube body 211 and is located outside the heat-insulating shell 100. The second tube 220 is partially inserted into the tube cavity of the first tube 210, and preferably, the second tube 220 is coaxially arranged with the first tube 210. One end of the second tube 220 close to the coupling ring 212 is located in the tube cavity of the first tube 210, and one end of the second tube 220 away from the coupling ring 212 extends to the outside of the first tube 210, and at the end away from the coupling ring 212, the outer circumferential surface of the second tube 220 is sealed and connected to the first tube 210.
[0054] When the reaction tube 200 is connected to the supersonic molecular beam injection assembly 600, the second tube 220 is preferably coaxially arranged with the first through hole 612, and is sealed and connected with the joint housing 610 by the joint ring 212. After the connection, the second tube 220 can be coaxially arranged with the first through hole 612. The end of the second tube 220 away from the joint ring 212 is connected to the four-way joint 700, so that the reactants undergo a catalytic reaction in the second tube 220 and produce reaction products, and the reaction products flow out of the second tube 220 and flow into the mass spectrometer 20 through the supersonic molecular beam injection assembly 600.
[0055] In a further improvement, the ultrasonic molecular beam assembly 600 further includes a third heating wire 630, which is located in the second inner cavity 611 and is wound around at least a portion of the outer wall of the nozzle 620. The nozzle 620 is heated by the third heating wire 630, which, on the one hand, prevents the reaction product from condensing and adhering to the inner wall of the nozzle 620 due to the decrease in temperature, thereby reducing the amount of the reaction product that subsequently enters the mass spectrometer and causing low sensitivity of the detection result, and, on the other hand, prevents the reaction product from condensing and causing the nozzle 620 to be blocked.
[0056] In a further improvement, the joint housing 610 is further provided with a third through hole 614 communicating with the second inner cavity 611, and a gas extraction pipeline is provided at the third through hole 614, and a valve 640 is provided on the gas extraction pipeline, and the valve is, for example, a butterfly valve. The gas extraction pipeline is used to connect a gas extraction device to evacuate the second inner cavity 611 so that the pressure in the reaction tube 200 is at a set value.
[0057] Furthermore, an embodiment of the utility model also provides a mass spectrometry analysis system, comprising the thermal radiation catalytic reaction device and a mass spectrometer as described above, wherein the mass spectrometer is connected to the reaction tube 200 .
[0058] It can be understood that when the thermal radiation catalytic reaction device includes the ultrasonic molecular beam injection component 600 , the mass spectrometer 20 is connected to the reaction tube 200 through the ultrasonic molecular beam injection component 600 .
[0059] For more details, please refer to Figure 4, the mass spectrometer 20 includes a sample introduction part 800, and the sample introduction part 800 includes an introduction housing 810 and a guide 820 disposed in the introduction housing 810. The introduction housing 810 is connected to the joint housing 610, and the introduction housing 810, the joint housing 610 and the nozzle 620 are enclosed together to form a third inner cavity (not marked in the figure). The guide 820 is disposed in the third inner cavity and connected to the introduction housing 810. The guide 820 is a hollow conical structure, and its inner diameter and outer diameter both increase in the direction away from the ultrasonic molecular beam injection assembly 600. The guide 820 is also preferably arranged coaxially with the nozzle 620, so that a differential chamber is formed between the guide 820 and the nozzle 620. The reason for setting the differential chamber here is that the mass spectrometer 20 is in a predetermined vacuum, and the reaction tube 200 has a set pressure, there is a pressure difference between the two, and the differential chamber plays a transitional role. Those skilled in the art will appreciate that, in practice, the nozzle 620 with a suitable inner diameter may be selected according to the pressure in the reaction tube 200 and the vacuum degree of the mass spectrometer 20. In other words, the nozzle 620 is preferably connected to the joint housing 610 in a detachable manner to facilitate replacement of the nozzle 620.
[0060] The mass spectrometer 20 further includes an ionization source joint 900, which is used to connect to an ionization source to introduce ionization energy into the mass spectrometer 20, thereby ionizing the reaction product entering the mass spectrometer 20. The ionization source is preferably a vacuum ultraviolet photoionization source, which includes but is not limited to any one of synchrotron radiation and vacuum ultraviolet lamps, and the energy range of the vacuum ultraviolet ionization source is 5eV to 24.5eV. In addition, the mass spectrometer 20 includes but is not limited to a time-of-flight mass spectrometer, such as a reflectron time-of-flight mass spectrometer.
[0061] Figure 5 The mass spectrum is obtained by using the thermal radiation catalytic reaction device of the mass spectrometry analysis system provided in the embodiment of the utility model to carry out a thermal radiation catalytic reaction on an ethane (C2H6) and argon (Ar) system, and using a time-of-flight mass spectrometer to perform in-situ detection and analysis of the reaction products. Figure 6 The mass spectrum is obtained by using the thermal radiation catalytic reaction device of the mass spectrometry analysis system provided in the embodiment of the utility model to perform a thermal radiation catalytic reaction on the ethane (C2H6) and carbon dioxide (CO2) system, and using a time-of-flight mass spectrometer to perform in-situ detection and analysis of the reaction products. Those skilled in the art know that argon (Ar) is an inert gas and actually has no catalytic effect on ethane (C2H6).
[0062] The inner diameter of the first tube 210 is 7.0 mm, the axial length of the portion of the reaction tube 200 located in the first inner cavity 101 is 350 mm, and during the reaction, the temperature of the reaction tube 200 is 1000 K, and the pressure in the reaction tube 200 is 10 Torr. In the axial direction of the reaction tube 200, the gap between the nozzle 620 and the reaction tube 200 is 10.0 mm, and the minimum inner diameter of the nozzle 620 is 1000 um.
[0063] The minimum inner diameter of the guide 820 is 2 mm. The resolution of the time-of-flight mass spectrometer is 2500@m / z128, that is, at a mass-to-charge ratio of 128, the resolution of the mass spectrum peak can reach 2500. The ionization source is synchrotron radiation with an energy range of 11 eV.
[0064] Figure 5 The signal intensities of ethyl and ethylene are both weak. Figure 6 The product ethylene in the reaction has obvious mass spectrometry peaks at (m / z=28) and the intermediate ethyl at (m / z=29). 13 The presence of C, the signal at m / z = 29 may also be 13 CCH4 and C2H5. 13 The natural abundance of C is 1.018%, but in the C2H6 / CO2 system, the ion count intensity of C2H4:C2H5 is 769:8.34, and in the C2H6 / Ar system, the ion count intensity of C2H4:C2H5 is 528:2.25. After deducting the isotope peak, the two systems still have a certain signal intensity at the position of m / z=29. It can be determined that when carbon dioxide is introduced, the output of C2H4 and C2H5 is increasing. In addition, the intensity ratios of C2H5 / C2H4 of the two systems are 0.0108 and 0.0043, respectively. The ratio of the former is more than 2.5 times that of the latter. Therefore, the experiment shows that carbon dioxide catalyzes the fission of CH in the C2H6 molecule under the action of thermal radiation, resulting in the generation of ethyl free radicals. That is, according to the above experimental results, it can be proved that the thermal radiation catalytic reaction device provided by the embodiment of the utility model can ensure the smooth progress of the thermal radiation catalytic experiment.
[0065] Although the utility model is disclosed as above, it is not limited thereto. Those skilled in the art may make various modifications and variations to the utility model without departing from the spirit and scope of the utility model. Thus, if these modifications and variations of the utility model fall within the scope of the claims of the utility model and their equivalents, the utility model is also intended to include these modifications and variations.
Claims
1. A thermal radiation catalytic reaction device, characterized in that: include: The heat-insulating shell is a hollow structure having a first inner cavity; A transparent reaction tube, at least partially inserted into the first inner cavity; A radiation source is at least partially disposed in the first inner cavity; the radiation source is spaced apart from and arranged in parallel with the reaction tube, and comprises a radiation tube, an inner liner tube and a first heating wire, the inner liner tube is at least partially penetrated in the tube cavity of the radiation tube, and the first heating wire is at least wound around the outer circumference of the portion of the inner liner tube located in the tube cavity of the radiation tube.
2. The thermal radiation catalytic reaction device according to claim 1, characterized in that: There are multiple radiation sources, and the multiple radiation sources are arranged at intervals in the circumferential direction of the reaction tube.
3. The thermal radiation catalytic reaction device according to claim 1, characterized in that: The heat-insulating shell is provided with two mounting holes, which are arranged opposite to each other; the axial ends of the reaction tube respectively pass through the two mounting holes and extend to the outside of the heat-insulating shell; The heat radiation catalytic reaction device further includes a second heating wire, which is wound at least around the outer circumference of the portion of the reaction tube located in the first inner cavity and the mounting hole.
4. The thermal radiation catalytic reaction device according to claim 3, characterized in that: The thermal radiation catalytic reaction device also includes a temperature monitoring component, which includes a first temperature monitoring element and a second temperature monitoring element. The first temperature monitoring element is arranged in the tube cavity of the inner liner tube, and the second temperature monitoring element is arranged on the outer surface of the part of the second heating wire located in the insulation shell.
5. The thermal radiation catalytic reaction device according to claim 1, characterized in that: The thermal radiation catalytic reaction device further includes an ultrasonic molecular beam injection component, which includes a joint shell and a nozzle; the joint shell is a hollow structure having a second inner cavity, and the joint shell is provided with a first through hole and a second through hole communicating with the second inner cavity, the first through hole is arranged opposite to the second through hole, and the aperture of the first through hole is smaller than the aperture of the second through hole; the nozzle is connected to the second through hole, and is partially located in the second inner cavity, and is coaxially arranged with the first through hole; the inner diameter of the nozzle gradually increases in a direction away from the first through hole; The reaction tube is sealed and connected to the joint shell at the first through hole, and the reaction tube is communicated with the second inner cavity.
6. The thermal radiation catalytic reaction device according to claim 5, characterized in that: The ultrasonic molecular beam injection assembly further includes a third heating wire, which is located in the second inner cavity and is wound around at least a portion of the outer side wall of the nozzle.
7. The thermal radiation catalytic reaction device according to claim 5, characterized in that: The joint shell is also provided with a third through hole communicating with the second inner cavity, the third through hole is provided with an air extraction pipeline, and the air extraction pipeline is provided with a valve.
8. The thermal radiation catalytic reaction device according to claim 5, characterized in that: The reaction tube comprises a first tube and a second tube, the first tube comprises a tube body and a coupling ring, the coupling ring is connected to one end of the tube body and is located outside the heat-insulating shell; the coupling ring is sealedly connected to the coupling shell; the second tube is partially inserted into the tube cavity of the first tube and is coaxially arranged with the first through hole; the outer peripheral surface of one end of the second tube away from the first through hole is sealedly connected to the first tube.
9. A mass spectrometry system, characterized in that: It comprises a mass spectrometer and the thermal radiation catalytic reaction device according to any one of claims 1 to 8, wherein the mass spectrometer is connected to the reaction tube.
10. The mass spectrometry system according to claim 9, characterized in that: The mass spectrometer comprises an ionization source joint portion, and the ionization source joint portion is used to be connected to an ionization source; the ionization source is a vacuum ultraviolet photoionization source.