Reactor and mass spectrometer apparatus

Abstract

The utility model provides a kind of reactor and double light source mass spectrum device for catalytic reaction gas phase species in situ detection, reactor includes control part, first pipe body and second pipe body;Control part includes first shell and switching element;First shell has the first passage and second passage along first direction arrangement;Switching element is located between first passage and second passage;First pipe body extends along first direction, and in switching element side away from second passage;First pipe body is communicated with first passage;Second pipe body extends along first direction, part in second passage;Second pipe body is connected with first shell, can be moved along first direction relative to first shell;Make switching element relative to first shell movement control first passage and second passage on-off;When first passage and second passage are communicated, allow second pipe body part to extend into second pipe body, when first passage and second passage are isolated, second pipe body is in switching element side away from first passage.The reactor carries out material replacement under the premise of not breaking vacuum.

Description

Technical Field

[0001] This invention belongs to the field of analytical chemistry technology, and specifically relates to a reactor and a mass spectrometry device. Background Technology

[0002] Catalysis technology, as a core driving force of modern chemical industry, achieves greener and more efficient production processes by reducing reaction activation energy and improving atom economy. Traditional methods for optimizing catalytic reaction processes and improving catalyst performance mainly rely on trial and error, involving numerous repeated experiments. This approach has limitations such as a vague understanding of catalytic mechanisms and lengthy research and development cycles. In catalytic reaction research, the study of gas-phase reaction mechanisms primarily focuses on the gas-phase intermediates desorbed from the catalyst surface to investigate the catalytic reaction kinetics. Therefore, real-time, in-situ capture and precise characterization of the dynamic evolution of active intermediates in catalytic reactions are the core scientific foundation for achieving catalytic reaction pathway analysis, rational catalyst design, and performance optimization.

[0003] Mass spectrometry (MS) is a crucial analytical tool in catalytic reaction kinetics research, operating under high vacuum. However, in current techniques for real-time in-situ capture and characterization of the dynamic evolution of active intermediates in catalytic reactions using MS, catalyst and / or reactant replacements are performed at atmospheric pressure. This means that whenever catalyst and / or reactant replacement is required, the reactor and MS must be restored to atmospheric conditions for sample loading and then re-evacuated to return to the high vacuum environment, resulting in significant waste of experimental time. Furthermore, the fixed relative positions of the catalytic reactor and MS in current techniques lead to a fixed sampling distance, preventing the study of the effects of different sampling distances on reactant concentration variations and reaction kinetic mechanisms. Utility Model Content

[0004] The purpose of this invention is to provide a reactor and a mass spectrometry device to solve the above-mentioned technical problems.

[0005] To achieve the above objectives, this utility model provides a reactor, comprising: The control unit includes a first housing and a switching element; the first housing has a first channel and a second channel arranged along a first direction; the switching element is partially disposed inside the first housing and located between the first channel and the second channel; the switching element is movably connected to the first housing. A first tube extends along the first direction and is disposed on the side of the switching member away from the second channel; one end of the first tube communicates with the first channel and is sealed to the first housing; and, The second tube extends along the first direction and partially passes through the second channel; the second tube is sealed to the first housing and is movable relative to the first housing along the first direction; The reactor is configured to control the connection and disconnection between the first channel and the second channel by the movement of the switching element relative to the first housing; when the first channel is connected to the second channel, the second tube is allowed to partially extend into the second tube, and when the first channel is isolated from the second channel, the second tube is located on the side of the switching element away from the first channel.

[0006] Optionally, the switching element is configured to rotate relative to the first housing, and the rotation axis of the switching element extends along a second direction, which is perpendicular to the first direction; the portion of the switching element located inside the first housing is provided with a through hole, the axis of which is perpendicular to the second direction; The control unit is configured such that when the switching member is rotated relative to the first housing to an axis extending along the first direction from the through hole, the first channel communicates with the second channel, and when the switching member is rotated relative to the first housing to an axis perpendicular to the first direction from the through hole, the first channel is isolated from the second channel.

[0007] Optionally, the walls of both the first tube and the second tube are transparent.

[0008] Optionally, the pipe wall of the first pipe and / or the pipe wall of the second pipe are provided with scales arranged along the first direction.

[0009] Optionally, the reactor further includes a sampling hood; the sampling hood is at least partially disposed on the side of the first tube body away from the control unit, and is a hollow structure with a first inner cavity; the sampling hood is sealed to the first tube body, and the lumen of the first tube body communicates with the first inner cavity; at least two sampling ports communicating with the first inner cavity are formed on the wall of the sampling hood, one of the sampling ports having an axis extending along the first direction, and the other sampling ports having an axis extending in a direction different from the first direction; On a plane perpendicular to the first direction, the projection of the sampling port, whose axis extends along the first direction, near the end of the first tube is located inside the projection of the second tube.

[0010] Optionally, the reactor further includes a heating wire wound around a portion of the outer circumferential surface of the first tube. The sampling hood is connected to the outer side of the first tube, and a sealing element is provided between the sampling hood and the outer side of the first tube; a medium flow channel is provided on the sampling hood near the sealing element, and the medium flow channel has a medium inlet and a medium outlet.

[0011] Optionally, the reactor further includes an air inlet, which includes at least two branch pipes and a manifold; one end of the manifold is connected to the end of the second pipe body away from the first pipe body, and the other end is connected to all the branch pipes; and / or, The first tube body is also provided with an air extraction port.

[0012] To achieve the above objectives, the present invention also provides a mass spectrometry device, including a first mass spectrometer and a reactor as described in any of the preceding claims, wherein the first mass spectrometer is sealed and connected to the end of the first tube away from the control unit.

[0013] Optionally, the first mass spectrometer includes a photoionization section, which includes a second housing, a synchrotron radiation optical interface, and a vacuum ultraviolet lamp; the second housing is a hollow structure with a second inner cavity, in which a photoionization region is formed; a connection hole is provided on the wall of the second housing, the axis of which passes through the photoionization region; the synchrotron radiation optical interface is disposed at the connection hole; the vacuum ultraviolet lamp is disposed in the second inner cavity, and the vacuum ultraviolet beam generated by the vacuum ultraviolet lamp can be transmitted to the photoionization region.

[0014] Optionally, the photoionization section further includes an electrode assembly disposed in the second inner cavity and including a cylindrical electrode. The cylindrical electrode is a hollow structure with a third inner cavity, which constitutes the photoionization region. The cylindrical electrode has a fourth, fifth, sixth, seventh, eighth, and ninth through-hole on its wall. The fourth and fifth through-holes are arranged opposite to each other along the first direction, with the fourth through-hole being closer to the reactor than the fifth through-hole. The fourth through-hole constitutes the sample inlet, and the fifth through-hole constitutes the sample outlet. The sixth and seventh through-holes are arranged opposite to each other on the axis of the connecting hole to allow the synchrotron radiation beam to pass through. The eighth and ninth through-holes are arranged opposite to each other on the transmission path of the vacuum ultraviolet beam generated by the vacuum ultraviolet lamp to allow the beam generated by the vacuum ultraviolet lamp to pass through; and / or, The first mass spectrometer further includes a mass analysis unit, which includes an ion introducer and a mass analyzer. The ion introducer and the mass analyzer are arranged along the first direction, and the ion introducer is closer to the photoionization unit than the mass analyzer.

[0015] Compared with the prior art, the reactor and mass spectrometry device of this invention have the following advantages: The aforementioned reactor includes a control unit, a first tube, and a second tube. The control unit includes a first housing and a switching element. The first housing has a first channel and a second channel arranged along a first direction. The switching element is partially disposed within the first housing and located between the first channel and the second channel. The switching element is movably connected to the first housing. The first tube extends along the first direction and is disposed on the side of the switching element away from the second channel. One end of the first tube communicates with the first channel and is sealed to the first housing. The second tube extends along the first direction and partially passes through the second channel. The second tube is sealed to the first housing and is capable of being positioned relative to the first housing along the first direction. The reactor is configured to control the connection and disconnection between the first channel and the second channel by the movement of the switching element relative to the first housing; when the first channel is connected to the second channel, the second tube is allowed to partially extend into the second tube; when the first channel is isolated from the second channel, the second tube is located on the side of the switching element away from the first channel. That is, the reactor has a first state and a second state. In the reactor in the first state, the first channel is connected to the second channel and the second tube is partially inserted into the first tube; in the reactor in the second state, the first channel is isolated from the second channel and the second tube is located on the side of the switching element away from the first channel. The reactor can be used in conjunction with a mass spectrometer to form a mass spectrometry device. The mass spectrometer is sealed to the end of the first tube away from the control unit and is in communication with the first tube. During the reaction, the catalyst and / or reactants are carried in the second tube, and the reactor is in the first state. This ensures a high vacuum environment in both the reactor and the mass spectrometer while the end of the second tube away from the mass spectrometer is not connected to the atmosphere. When it is necessary to replace the catalyst and / or reactants, the reactor can be switched to the second state first, and then the end of the second tube away from the mass spectrometer can be connected to the atmosphere for replacement. After replacement, the connection between the end of the second tube away from the mass spectrometer and the atmosphere is first blocked, and then the reactor is switched to the second state. This achieves the effect of material replacement with minimal vacuum disruption. Furthermore, since the second tube can move relative to the first shell along the first direction, the length of the portion of the second tube within the first tube can be adjusted during the experiment to adjust the sampling distance, allowing the mass spectrometry device to study the effect of the sampling distance on the analytical results.

[0016] Furthermore, the reactor also includes a sampling hood; the sampling hood is at least partially disposed on the side of the first tube body away from the control unit, and is a hollow structure with a first inner cavity; the sampling hood is sealed to the first tube body, such that the lumen of the first tube body communicates with the first inner cavity; at least two sampling ports communicating with the first inner cavity are formed on the wall of the sampling hood, one of the sampling ports having an axis extending along the first direction, and the other sampling ports having axes extending in directions different from the first direction; on a plane perpendicular to the first direction, the projection of the end of the sampling port whose axis extends along the first direction near the first tube body is located inside the projection of the second tube body. Different sampling ports can be connected to different types of mass spectrometers to jointly detect the reactants of the reaction occurring in the reactor using different types of mass spectrometers, achieving complementary analysis of analytical data from different types of mass spectrometers. Attached Figure Description

[0017] The accompanying drawings are provided to better understand this utility model and do not constitute an undue limitation thereof. Wherein: Figure 1 This is a schematic diagram of the reactor provided according to an embodiment of the present invention, wherein the reactor in the diagram is in a first state; Figure 2 This is a schematic diagram of the reactor provided according to an embodiment of the present invention, wherein the reactor in the diagram is in a second state; Figure 3 This is a schematic diagram of the mass spectrometry device provided according to an embodiment of the present invention; Figure 4 This is a partial structural schematic diagram of a mass spectrometry device according to an embodiment of the present invention; Figure 5 This is a mass spectrum obtained when a standard gas is tested using the first mass spectrometer of the mass spectrometer device provided in an embodiment of this utility model; Figure 6 It is a mass spectrum obtained when a standard gas is tested using a mass spectrometry device with existing technology; Figure 7 This is a mass spectrum obtained in a catalytic pyrolysis experiment of high-density polyethylene using the mass spectrometry device provided in an embodiment of this utility model.

[0018] [The following are explanations of the reference numerals in the attached drawings]: 10-Reactor, 20-Mass spectrometer, 20a-First mass spectrometer, 100-Control unit, 110-First shell, 1101-First through-hole, 1102-Second through-hole, 1103-First sub-cavity, 1104-Second sub-cavity, 111-First channel, 112-Second channel, 120-Switching element, 121-Third through-hole, 200-First tube, 201-First extraction port, 300-Second tube, 400-Sampling hood, 401-First inner cavity, 402-Sampling port, 402a-First sampling port, 410-Medium flow channel, 411-Medium inlet, 412-Medium outlet, 500-Sealing element, 600-Heating wire, 700-Gas inlet. 710-Branch pipe, 720-Manifold, 800-Photoionization section, 810-Second housing, 811-Second inner cavity, 812-Second extraction port, 820-Synchrotron radiation optical interface, 830-Vacuum ultraviolet lamp, 840-Electrode assembly, 841-Cylindrical electrode, 8411-Fourth through hole, 8412-Fifth through hole, 8413-Sixth through hole, 8414-Seventh through hole, 8415-Eighth through hole, 842-Molecular beam focusing cylinder, 8421-Fifth inner cavity, 843-Focusing electrode plate, 900-Mass analysis section, 910-Third housing, 911-Fifth inner cavity, 912-Third extraction port, 920-Ion introduction section, 930-Mass analyzer, 940-Differential sampler. Detailed Implementation

[0019] The following specific examples illustrate the implementation of this utility model. Those skilled in the art can easily understand other advantages and effects of this utility model from the content disclosed in this specification. This utility model can also be implemented or applied through other different specific embodiments, and various details in this specification can be modified or changed based on different viewpoints and applications without departing from the spirit of this utility model. It should be noted that the illustrations provided in this embodiment are only schematic representations of the basic concept of this utility model. Therefore, the drawings only show components related to this utility model and are not drawn according to the actual number, shape, and size of the components in implementation. In actual implementation, the type, quantity, and proportion of each component can be arbitrarily changed, and the component layout may also be more complex.

[0020] Furthermore, while each embodiment described below possesses one or more technical features, this does not imply that users of this utility model must simultaneously implement all technical features in any embodiment, or can only separately implement some or all technical features in different embodiments. In other words, provided it is feasible, those skilled in the art can selectively implement some or all technical features in any embodiment, or selectively implement a combination of some or all technical features in multiple embodiments, based on the disclosure of this utility model and depending on design specifications or implementation requirements, thereby increasing the flexibility in implementing this utility model.

[0021] As used herein, the singular forms “a,” “an,” and “the” include plural objects, and the plural form “a plurality” includes two or more objects, unless otherwise expressly indicated. As used herein, the term “or” is generally used to include the meaning of “and / or,” unless otherwise expressly indicated, and the terms “install,” “connect,” and “link” should be interpreted broadly, for example, as a fixed connection, a detachable connection, or an integral connection. Connections can be mechanical or electrical. Connections can be direct or indirect through an intermediate medium, and can represent internal communication between two elements or an interaction between two elements. Relational terms such as “first,” “second,” etc., are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations, nor do they indicate relative importance or implicitly specify the number of indicated technical features. Those skilled in the art will understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0022] To make the objectives, advantages, and features of this utility model clearer, the following detailed description is provided in conjunction with the accompanying drawings. It should be noted that the drawings are all in a very simplified form and use non-precise proportions, and are only used to conveniently and clearly illustrate the objectives of the embodiments of this utility model. The same or similar reference numerals in the drawings represent the same or similar parts.

[0023] Figure 1 and Figure 2 This is a schematic diagram of the structure of the reactor 10 provided in one embodiment of the present invention. Figure 2 The reactor 10 shown is Figure 1 The reactor 10 shown is in a different state. For example... Figure 1 and Figure 2 As shown, the reactor 10 includes a control unit 100, a first tube 200, and a second tube 300.

[0024] The control unit 100 includes a first housing 110 and a switching element 120. The first housing 110 has a first channel 111 and a second channel 112 arranged along a first direction. The switching element 120 is partially disposed within the first housing 110 and located between the first channel 111 and the second channel 112. The switching element 120 is movably connected to the first housing 110. The reactor 10 is configured to control the opening and closing of the first channel 111 and the second channel 112 by moving the switching element 120 relative to the first housing 110.

[0025] The first tube 200 extends along the first direction. The second tube 200 is disposed on the side of the switching member 120 away from the second channel 112. One axial end of the second tube 200 is sealed to the first housing 110 and communicates with the first channel 111, while the other axial end of the second tube 200 is away from the first housing 110.

[0026] The second tube 300 extends along the first direction and partially passes through the second channel 112. The second tube 300 is sealed to the first housing 110 and is movable relative to the first housing 110 along the first direction.

[0027] When the first channel 111 is connected to the second channel 112, the second tube 300 is allowed to move along the first direction so that the second tube 300 partially passes through the first channel 111 and enters the second channel 112. When the first channel 111 is isolated from the second channel 112, the second tube 300 is entirely located on the side of the switching member 120 away from the first channel 111.

[0028] In other words, the reactor 10 has a first state and a second state. When the reactor 10 is in the first state, the first channel 111 is connected to the second channel 112, and the second tube 300 extends partially into the first tube 200. When the reactor 10 is in the second state, the first channel 111 is isolated from the second channel 112 (i.e., not connected), and the second tube 300 is entirely located on the side of the switching element 120 away from the first channel 111.

[0029] like Figure 3As shown, the reactor 10 and mass spectrometer 20 are used together to form a mass spectrometry device. This device can perform a catalytic pyrolysis reaction and capture and characterize the reaction products generated during the catalytic reaction in real time in situ. The mass spectrometer 20 is sealed to the end of the first tube 200 away from the control unit 100, and the mass spectrometer 20 is in communication with the lumen of the first tube 200. It can be understood that when the reactor 10 is in the first state, the mass spectrometer 20 is in communication with the lumen of the second tube 300; when the reactor 10 is in the second state, the mass spectrometer 20 is isolated from the lumen of the second tube 300. During operation of the mass spectrometry device, a solid substance is carried in the second tube 300. This solid substance includes a catalyst, or the solid substance includes both a catalyst and solid reactants. Thus, the catalytic reaction occurs in the second tube 300.

[0030] During the catalytic pyrolysis reaction, the reactor 10 is in the first state, and the end of the second tube 300 away from the first channel 111 is isolated from the atmosphere. Therefore, the mass spectrometer can maintain a high vacuum operating environment. When replacing the solid material, the replacement operation is performed while the reactor 10 is in the second state. The specific replacement process is as follows: Step S1: With the end of the second tube 300 away from the first channel 111 isolated from the atmosphere, move the second tube 300 relative to the first housing 110 along the direction from the first channel 111 to the second channel 112 until the second tube 300 is completely located on the side of the switching member 120 away from the first channel 111.

[0031] Step S2: Control the switching element 120 to move relative to the first housing 110, so that the first channel 111 is isolated from the second channel 112. At this time, the reactor 10 is in the second state.

[0032] Step S3: Connect the end of the second tube 300 away from the first channel 111 to the atmosphere.

[0033] Step S4: Replace the solid material.

[0034] Step S5: Isolate the end of the second tube 300 away from the first channel 111 from the atmosphere.

[0035] Step S6: Control the switching component 120 to move relative to the first housing 110 so that the first channel 111 is connected to the second channel 112.

[0036] Step S7: Move the second tube 300 relative to the first shell 110 along the direction of the second channel 112 pointing to the first channel 111 until the length of the portion of the second tube 300 extending into the first tube 200 is appropriate. At this time, the reactor 10 is in the first state.

[0037] In the above process, the operations of steps S1, S2, and S5 through S7 do not affect the pressure inside the mass spectrometer 20 and the reactor 10. Only the execution of steps S3 and S4 will cause the pressure inside the mass spectrometer 20 and the second tube 200 to increase. However, those skilled in the art will understand that the inner diameter of the second tube 300 is extremely small, generally a few millimeters, for example, about 4 mm. Therefore, the effect of the execution of steps S3 and S4 on the pressure inside the mass spectrometer 20 and the second tube 200 is extremely weak and can be ignored. That is, the application of the reactor 10 provided by this embodiment of the present invention can achieve the effect of replacing the catalyst and / or solid reactants in the mass spectrometer device under conditions that are basically not broken by vacuum.

[0038] Furthermore, since the second tube 300 can move relative to the first shell 110 along the first direction, the movement of the second tube 300 can be controlled during the catalytic pyrolysis reaction to adjust the length of the portion of the second tube 300 located inside the first tube 200, thereby adjusting the length of the transmission path (i.e., sampling distance) of the reaction product from the location of the solid material to the mass spectrometer 20. This allows the mass spectrometer to study the influence of the sampling distance on the analytical results.

[0039] Preferably, both the first tube 200 and the second tube 300 are transparent tubes, allowing the operator to observe the length change of the portion of the second tube 300 within the first tube 200. More preferably, at least one of the first tube 200 and the second tube 300 has a scale arranged along the first direction on its wall. By using the scale, the length of the portion of the second tube 300 within the first tube 200 can be quantitatively adjusted, thereby quantitatively adjusting the sampling distance.

[0040] The structure of the reactor 10 will be further described below.

[0041] The first housing 110 is a hollow structure with a fourth inner cavity (not shown in the figure), and the wall of the housing 110 is provided with two through holes, which communicate with the fourth inner cavity respectively. The two through holes are referred to as the first through hole 1101 and the second through hole 1102, and the first through hole 1101 and the second through hole 1102 are arranged opposite to each other in the first direction. The switching member 120 is partially disposed in the fourth inner cavity and divides the fourth inner cavity into a first sub-cavity 1103 and a second sub-cavity 1104 arranged along the first direction. The first sub-cavity 1103 communicates with the first through hole 1101 and together forms the first channel 111, and the second sub-cavity 1103 communicates with the second through hole 1102 and together forms the second channel 112.

[0042] Optionally, the switching element 120 is rotatably connected to the first housing 110, allowing the switching element 120 to rotate relative to the first housing 110. The axis of rotation of the switching element 120 extends along a second direction, which is perpendicular to the first direction. A through hole, referred to as a third through hole 121, is provided on the portion of the switching element 120 located within the channel 111, and the axis of the third through hole 121 is perpendicular to the second direction. The control unit 100 is configured such that when the switching element 120 rotates to the point where the axis of the third through hole 121 extends along the first direction, the first channel 111 and the second channel 112 communicate through the third through hole 121, allowing the second tube 200 to pass through the third through hole 121, thereby allowing the second tube 200 to move to partially penetrate within the first tube 100 (i.e., allowing the reactor to switch to the first state). The control unit 100 is further configured such that when the switching member 120 is rotated to the point where the axis of the third through hole 121 is perpendicular to the first direction, the first channel 111 and the second channel 112 are isolated by the switching member 120 and no longer connected.

[0043] Therefore, the aforementioned step S2 includes controlling the switching member 120 to rotate so that the axis of the third through hole 121 is perpendicular to the first direction. And the aforementioned step S6 includes controlling the switching member 120 to rotate so that the axis of the third through hole 121 extends along the first direction. It can be understood that when the axis of the third through hole 121 extends along the first direction, if the control unit 100 is projected onto a plane perpendicular to the first direction, the projection of the third through hole 121 at least partially coincides with the projections of the first through hole 1101 and the second through hole 1102. Preferably, when the axis of the third through hole 121 extends along the first direction, the axes of the first through hole 1101, the second through hole 1102, and the third through hole 121 coincide.

[0044] Of course, the switching element 120 can also have any other suitable structure, as long as it can achieve the above purpose.

[0045] In practice, a commercially available vacuum straight-through valve can be used as the control unit 100.

[0046] Optionally, the second tube 300 is sealed to the first housing 110 via a vacuum hand-tightening connector (not shown) or any other suitable means.

[0047] Optionally, the first tube 200 is provided with an air extraction port, which is referred to as the first air extraction port 201, so as to be connected to an external vacuum device.

[0048] This invention does not impose any particular limitation on the connection method between the first tube 200 and the mass spectrometer; the two can be directly connected or indirectly connected.

[0049] For example, in an optional example, such as Figure 1 and Figure 2 As shown, the reactor 10 further includes a sampling hood 400. The sampling hood 400 is at least partially disposed on the side of the first tube 200 away from the control unit 100, and is a hollow structure having a first inner cavity 401. The sampling hood 400 is sealed to the first tube 200, such that the lumen of the first tube 200 communicates with the first inner cavity 401. A sampling port 402 communicating with the first inner cavity 401 is formed on the wall of the sampling hood 400. Figure 3 As shown, the mass spectrometer 20 is disposed at the sampling port 402 and is sealed to the sampling cover 400. The mass spectrometer 20 is connected to the lumen of the first tube 200 through the sampling port 402 and the first inner cavity 401. In other words, the mass spectrometer 20 is indirectly connected to the second tube 200 through the sampling cover 400.

[0050] Generally, the sampling cover 400 is connected to the outer side of the first tube 200, and a sealing element 500 is provided between the sampling cover 400 and the outer side of the first tube 200.

[0051] Optionally, such as Figure 1 and Figure 2As shown, the reactor 10 further includes a heating wire 600, which is wound around a portion of the outer circumferential surface of the first tube 200 to heat the first tube 200, and subsequently heat the portion of the second tube 300 that passes through the first tube 200. Preferably, the sampling hood 400 also has a medium flow channel 410, which has a medium inlet 411 and a medium outlet 412. The medium flow channel is located near the sealing element 500 on the sampling hood 400 and extends continuously around the axis of the first tube 200. During the pyrolysis catalytic reaction, the cooling medium enters the medium flow channel 410 through the medium inlet 411, flows along the medium flow channel 410 into the medium outlet 412, and then exits. The cooling medium can cool the sealing element 500 to prevent it from being heated to a high temperature by the heating wire 600 and losing its sealing properties.

[0052] Optionally, at least two sampling ports 402 are formed on the sampling hood 400, and a mass spectrometer 20 (e.g., ...) can be set at each sampling port 402. Figure 3 (As shown). That is, by providing at least two sampling ports 402, the reactor 10 can be simultaneously connected to at least two mass spectrometers 20, and the characteristics of the at least two mass spectrometers 20 may be different, so as to simultaneously detect different substances in the reaction products. For example, a photoionization mass spectrometer can be set at one sampling port 402 to detect organic matter produced by the reaction, and an electron impact ionization mass spectrometer can be set at the other sampling port 402 to detect inorganic matter produced by the reaction.

[0053] Preferably, the axis of at least one of the sampling ports 402 extends in the first direction, while the axis of the remaining sampling ports 402 extends in a direction different from the first direction.

[0054] For ease of description, the sampling port 402 whose axis extends in the first direction is referred to as the first sampling port 402a. The mass spectrometer 20 disposed at the first sampling port 402a is referred to as the first mass spectrometer 20a.

[0055] When the first sampling port 402a and the second tube 300 are projected onto a plane perpendicular to the first direction, the projection of the end of the first sampling port 402a facing the second tube 200 is located inside the projection of the first tube 200. This allows the reaction products to enter the first mass spectrometer 20a located at the first sampling port 402a along the first direction. Optionally, the aperture of the first sampling port 402a gradually decreases in the direction away from the first tube 200; that is, the first sampling port 402a is a conical ultrasonic molecular beam sampling port, and the reaction products form an ultrasonic molecular beam when entering the mass spectrometer 20a through the first sampling port 402a. Preferably, the first mass spectrometer 20a is a photoionization mass spectrometer. The specific construction of other sampling ports 402 is determined as needed.

[0056] Optionally, the reactor 10 further includes an air inlet 700, which includes at least two branch pipes 710 and a manifold 720. One end of the manifold 720 can be connected to the end of the second tube 300 away from the first channel 111, and the other end is connected to all the branch pipes 710. The number of branch pipes 710 can be two, three, four, or even more, and this embodiment of the present invention does not limit this. Each branch pipe 710 is used to connect to a gas source used in the experiment to introduce the reaction gas into the second tube 300. The gas source here is, for example, a carrier gas source or a reaction gas source. It can be understood that the carrier gas source is used to provide carrier gas for the reaction, and the reaction gas source is used to provide reaction gas. The specific types of the carrier gas and the reaction gas are determined experimentally.

[0057] It is understood that when the air intake 700 is connected to the second pipe 300, the air intake 700 blocks the connection between the end of the second pipe 300 away from the first channel 111 and the atmosphere; when the air intake 700 is separated from the second pipe 300, the end of the second pipe 300 away from the first channel 111 is connected to the atmosphere.

[0058] The second objective of this utility model embodiment is to provide a mass spectrometry device as described above.

[0059] like Figure 3 and Figure 4As shown, when the first mass spectrometer 20a located at the first sampling port 402a is a photoionization mass spectrometer, the first mass spectrometer 20a includes a photoionization section 800 and a mass analysis section 900. Preferably, the photoionization section 800 includes a second housing 810. The second housing 810 is connected to the sampling cover 400, and the second housing 810 is a hollow structure with a second inner cavity 811. A photoionization region (not shown in the figure) is formed in the second inner cavity 811, and the photoionization region has a sample inlet and a sample outlet. The reaction product enters the photoionization region through the first sampling port 402a and the sample inlet, and is at least partially ionized in the photoionization region. The ionized reaction product flows out of the photoionization region from the sample outlet and then enters the mass analysis section 900 for analysis.

[0060] Preferably, the sample inlet and the sample outlet are arranged opposite to each other in the first direction. A connection hole is provided on the wall of the second housing 810, and the axis of the connection hole passes through the photoionization region. The photoionization unit 800 further includes a synchrotron radiation light interface 820 and a vacuum ultraviolet lamp 830. The synchrotron radiation light interface 820 is located at the connection hole and is used to connect to a synchrotron radiation source, so that the synchrotron radiation light generated by the synchrotron radiation source can be transmitted to the photoionization region via the connection hole. The vacuum ultraviolet lamp 830 is located in the second inner cavity, and the vacuum ultraviolet light beam generated by the vacuum ultraviolet lamp 830 can be transmitted to the photoionization region. That is, the first mass spectrometer 20a, with the vacuum ultraviolet lamp 830, can also be connected to a synchrotron radiation source, so that the first mass spectrometer 20a can perform photoionization using both synchrotron radiation light and vacuum ultraviolet light. Thus, in actual operation, operators can not only select a suitable energy source as needed, but also use the vacuum ultraviolet lamp 830 during synchrotron radiation source maintenance, overcoming the time constraints of synchrotron radiation optical engines. In practice, the axis of the vacuum ultraviolet lamp 830 passes through the photoionization region, and the vacuum ultraviolet beam generated by the vacuum ultraviolet lamp 830 is transmitted along its axis. Preferably, the axis of the vacuum ultraviolet lamp 830, the axis of the connecting hole, and the first direction are perpendicular to each other.

[0061] The photoionization unit 800 further includes an electrode assembly 840. The electrode assembly 840 is disposed in the second inner cavity 811 and includes a cylindrical electrode 841. The cylindrical electrode 841 is a hollow structure with a third inner cavity (not shown in the figure), and the third inner cavity constitutes the photoionization region.

[0062] The cylindrical electrode 841 has a fourth through hole 8411, a fifth through hole 8412, a sixth through hole 8413, a seventh through hole 8414, an eighth through hole 8415 and a ninth through hole (not shown in the figure) that are connected to the photoionization region.

[0063] The fourth through-hole 8411 and the fifth through-hole 8412 are arranged opposite to each other in the first direction, with the fourth through-hole 8411 being closer to the reactor 10 than the fifth through-hole 8412 to form the sample inlet, and the fifth through-hole 8412 forming the sample outlet. Preferably, the diameter of the fourth through-hole 8411 is half the diameter of the third inner cavity, and the diameter of the fifth through-hole 8412 is equal to the diameter of the third inner cavity, so as to achieve directional transport of the reaction products.

[0064] The sixth through-hole 8413 and the seventh through-hole 8414 are arranged opposite to each other on the axis of the connecting hole, with the sixth through-hole 8413 being closer to the connecting hole than the seventh through-hole 8414. The eighth through-hole 8415 and the ninth through-hole are arranged opposite to each other on the axis of the vacuum ultraviolet lamp 830, with the eighth through-hole 8415 being closer to the second connecting hole than the ninth through-hole. The sixth through-hole 8413 allows the synchrotron radiation beam to enter the photoionization region to photoionize the reaction products located there. The seventh through-hole 8414 allows the synchrotron radiation beam to exit from the photoionization region, preventing the synchrotron radiation beam from irradiating the inner wall of the cylindrical electrode 841 and causing problems such as photoelectric effect and photoelectron overflow. The eighth through hole 8415 allows the light beam generated by the vacuum ultraviolet lamp 830 to enter the photoionization region to photoionize the reaction products located in the photoionization region. The ninth through hole allows the light beam generated by the vacuum ultraviolet lamp 830 to exit from the photoionization region, avoiding the light beam of the vacuum ultraviolet lamp 830 from irradiating the inner wall of the cylindrical electrode 841 and causing problems such as photoelectric effect and photoelectron overflow.

[0065] The dimensions of the sixth through-hole 8412, the seventh through-hole 8413, the eighth through-hole 8414, and the ninth through-hole should be appropriate. If the dimensions of the sixth through-hole 8412 and the seventh through-hole 8413 are too small, they will obstruct the synchrotron radiation beam. If the dimensions of the eighth through-hole 8414 and the ninth through-hole are too small, they will obstruct the beam of the vacuum ultraviolet lamp 830. If the dimensions of the sixth through-hole 8412, the seventh through-hole 8413, the eighth through-hole 8414, and the ninth through-hole are too large, they will cause leakage of carrier gas and ionized ions. In practice, it is preferable that the shapes of the sixth through-hole 8412 and the seventh through-hole 8413 are the same as the shape of the synchrotron radiation beam, and it is preferable that the shapes of the eighth through-hole 8414 and the ninth through-hole are the same as the shape of the beam of the vacuum ultraviolet lamp 830.

[0066] Furthermore, the electrode assembly 840 further includes a molecular beam focusing cylinder 842 and a plurality of focusing electrode plates 843. The molecular beam focusing cylinder 842 is disposed between the fourth through hole 8411 and the first sampling port 402a, and has a fifth inner cavity 8421 extending through along the first direction, the fifth inner cavity connecting the first sampling port 402a and the sample inlet 8411. The function of the molecular beam focusing cylinder 842 is to focus the reaction products in the form of ultrasonic molecular beams to increase the molecular density of the reaction products entering the photoionization region. The plurality of focusing electrode plates 843 are arranged at intervals along the first direction on the side of the cylindrical electrode 841 away from the reactor 10, and each focusing electrode plate 843 is provided with a through hole 8431. The through hole 8431 on the focusing electrode plate 843 closer to the cylindrical electrode 841 has a larger aperture, and the through hole 8431 on the focusing electrode plate 843 further away from the cylindrical electrode 841 has a smaller aperture. In one specific embodiment, the number of focusing plates 843 is two.

[0067] Preferably, the first sampling port 402a, the fifth inner cavity 8421, the fourth through hole 8411, the fifth through hole 8412, and the through hole 8431 are coaxially arranged.

[0068] The mass spectrometry mass analysis unit 900 includes a third housing 910, an ion introducer 920, and a mass analyzer 930. The third housing 910 is disposed along the first direction on the side of the photoionization unit 800 away from the reactor 10 and is connected to the second housing 810. The third housing 910 is a hollow structure with a fifth inner cavity 911. The ion introducer 920 and the mass analyzer 930 are both disposed within the fifth inner cavity 911 and are arranged at intervals along the first direction. The ion introducer 920 is closer to the photoionization unit 800 than the mass analyzer 930, and a differential sampler 940 is provided between the ion introducer 910 and the photoionization unit 800. The differential sampler 940 has a differential sampling hole extending along the first direction, and the diameter of the differential sampling hole increases in the direction away from the photoionization unit 800. The ion introducer 910 is connected to the through hole 8431 on the focusing electrode plate 843 through the differential sampling hole. Preferably, the ion introducer 910, the differential sampling hole, and the through hole 8431 are coaxial. In this embodiment of the present invention, the sample introduction method of the mass analyzer 900 is "axial sample introduction," which is beneficial to improving the sensitivity of the mass analyzer 900. The ion introducer 910 can be an electrostatic lens group, or a multi-stage bar, or a multi-stage bar group. The mass analyzer 920 includes, but is not limited to, any one of a quadrupole analyzer, a time-of-flight analyzer, an ion trap analyzer, or an orbital trap analyzer.

[0069] It can also be understood that the second housing 810 has a second air extraction port 812 communicating with the second inner cavity 811 on its wall, and the third housing 910 has a third air extraction port 912 communicating with the fifth inner cavity 911 on its wall. Both the second air extraction port 812 and the third air extraction port 912 are used to connect to an external vacuum device.

[0070] When performing a catalytic reaction and analyzing the reactants using the mass spectrometer, the vacuum level inside the reactor 10 can be 10 Pa to 1 × 10⁻⁶ Pa. 5 Pa, the vacuum degree of the photoionization section 800 of the first mass spectrometer 20a is 1×10 Pa. -2 Pa to 2 Pa, the vacuum degree of the mass spectrometer mass analysis unit 900 is 1×10⁻⁶ Pa. -3 Pa ~ 1×10 -5 Pa.

[0071] The mass spectrometer requires commissioning before use. One possible commissioning process is as follows: The reactor 10 is placed in the first state, and photoionization is performed using the vacuum ultraviolet lamp 830. At a photon energy of 10.6 eV, the standard mixed gas flows into the mass spectrometer, and the first mass spectrometer 20a is used to accumulate and acquire mass spectra for 10 seconds. The voltage parameters are then adjusted to their optimal values. In this example, the standard mixed gas includes 10 sccm ethylene and 200 sccm argon, with ethylene and argon entering the reactor 10 through two branch pipes 610, respectively. After voltage parameter commissioning, the voltage applied to the cylindrical electrode 841 is determined to be 10V, the voltage applied to the first focusing electrode 843a to be 4V, the voltage applied to the second focusing electrode 843b to be 0V, the voltage applied to the differential sampler 911 to be -20V, and the voltage on the molecular focusing cylinder 842 is the same as or zero compared to the voltage on the cylindrical electrode 841. At the optimal voltage, the mass spectrum acquired by the first mass spectrometer 20a is as follows: Figure 5 As shown.

[0072] Figure 6 The mass spectrum is collected when the mass spectrometry analysis device disclosed in CN114994166A is debugged using the standard mixed gas.

[0073] Compare Figure 5 and Figure 6 As can be seen, the sensitivity of the mass spectrometry device provided in this application embodiment is significantly higher than that of the mass spectrometry device disclosed in CN114994166A.

[0074] The mass spectrometer provided in this embodiment of the present invention can be used to perform catalytic pyrolysis reactions after debugging, such as the catalytic pyrolysis reaction of high-density polyethylene (HDPE) at 400°C, with Pt / ZSM-5 as the catalyst. The specific reaction operation can be referred to the prior art. Figure 7 It is a mass spectrum collected by the first mass spectrometer 20a during the reaction process. Figure 7 The mass spectrometry results show mass spectrometry signals of low-carbon olefins such as ethylene (m / z=28), propylene (m / z=42), and butene (m / z=56), as well as mass spectrometry signals of monocyclic aromatic hydrocarbons such as benzene (m / z=78) and toluene (m / z=92). These low-carbon olefins and monocyclic aromatic hydrocarbons are the core products of the catalytic pyrolysis of 1% Pt / ZSM-5+HDPE, indicating that the catalytic reaction proceeds smoothly and can be detected on the mass spectrometry device provided by this invention.

[0075] While the present invention has been disclosed above, it is not limited thereto. Those skilled in the art can make various modifications and variations to the present invention without departing from its spirit and scope. Therefore, if such modifications and variations fall within the scope of the claims of the present invention and their equivalents, the present invention also intends to include such modifications and variations.

Claims

1. A reactor, characterized in that, include: The control unit includes a first housing and a switching component; the first housing is provided with a first channel and a second channel arranged along a first direction; The switching element is partially disposed within the first housing and located between the first channel and the second channel; the switching element is movably connected to the first housing. A first tube extends along the first direction and is disposed on the side of the switching member away from the second channel; one end of the first tube is connected to the first channel and is sealed to the first housing. as well as, The second tube extends along the first direction and partially passes through the second channel; The second tube is sealed to the first housing and is movable relative to the first housing along the first direction; The reactor is configured to control the opening and closing of the first channel and the second channel by the movement of the switching element relative to the first housing; When the first channel is connected to the second channel, the second tube is allowed to partially extend into the second tube. When the first channel is isolated from the second channel, the second tube is located on the side of the switching element away from the first channel.

2. The reactor according to claim 1, characterized in that, The switching element is configured to rotate relative to the first housing, and the axis of rotation of the switching element extends along a second direction, which is perpendicular to the first direction; the portion of the switching element located inside the first housing is provided with a through hole, the axis of which is perpendicular to the second direction; The control unit is configured such that when the switching member is rotated relative to the first housing to an axis extending along the first direction from the through hole, the first channel communicates with the second channel, and when the switching member is rotated relative to the first housing to an axis perpendicular to the first direction from the through hole, the first channel is isolated from the second channel.

3. The reactor according to claim 1, characterized in that, The walls of both the first and second tubes are transparent.

4. The reactor according to claim 3, characterized in that, The first tube and / or the second tube are provided with scales arranged along the first direction.

5. The reactor according to claim 1, characterized in that, The reactor further includes a sampling hood; the sampling hood is at least partially disposed on the side of the first tube body away from the control unit, and is a hollow structure with a first inner cavity; the sampling hood is sealed to the first tube body, and the lumen of the first tube body communicates with the first inner cavity; at least two sampling ports communicating with the first inner cavity are formed on the wall of the sampling hood, one of the sampling ports having an axis extending along the first direction, and the other sampling ports having an axis extending in a direction different from the first direction. On a plane perpendicular to the first direction, the projection of the sampling port, whose axis extends along the first direction, near the end of the first tube is located inside the projection of the second tube.

6. The reactor according to claim 5, characterized in that, The reactor also includes a heating wire wound around a portion of the outer circumferential surface of the first tube. The sampling hood is connected to the outer side of the first tube, and a sealing element is provided between the sampling hood and the outer side of the first tube; a medium flow channel is provided on the sampling hood near the sealing element, and the medium flow channel has a medium inlet and a medium outlet.

7. The reactor according to claim 1, characterized in that, The reactor further includes an air inlet, which comprises at least two branch pipes and a manifold; one end of the manifold is connected to the end of the second pipe body away from the first pipe body, and the other end is connected to all the branch pipes; and / or The first tube body is also provided with an air extraction port.

8. A mass spectrometry device, characterized in that, The device includes a first mass spectrometer and a reactor as described in any one of claims 1-7, wherein the first mass spectrometer is sealed and connected to the end of the first tube away from the control unit.

9. The mass spectrometry apparatus according to claim 8, characterized in that, The first mass spectrometer includes a photoionization section, which includes a second housing, a synchrotron radiation optical interface, and a vacuum ultraviolet lamp. The second housing is a hollow structure with a second inner cavity, in which a photoionization region is formed. A connection hole is provided on the wall of the second housing, and the axis of the connection hole passes through the photoionization region. The synchrotron radiation optical interface is located at the connection hole. The vacuum ultraviolet lamp is located in the second inner cavity, and the vacuum ultraviolet beam generated by the vacuum ultraviolet lamp can be transmitted to the photoionization region.

10. The mass spectrometry apparatus according to claim 9, characterized in that, The photoionization section further includes an electrode assembly disposed in the second inner cavity and including a cylindrical electrode. The cylindrical electrode is a hollow structure with a third inner cavity, which constitutes the photoionization region. The cylindrical electrode has a fourth, fifth, sixth, seventh, eighth, and ninth through-hole on its wall. The fourth and fifth through-holes are arranged opposite each other along the first direction, with the fourth through-hole being closer to the reactor than the fifth through-hole. The fourth through-hole constitutes a sample inlet, and the fifth through-hole constitutes a sample outlet. The sixth and seventh through-holes are arranged opposite each other on the axis of the connecting hole to allow the synchrotron radiation beam to pass through. The eighth and ninth through-holes are arranged opposite each other on the transmission path of the vacuum ultraviolet beam generated by the vacuum ultraviolet lamp to allow the vacuum ultraviolet beam generated by the vacuum ultraviolet lamp to pass through; and / or, The first mass spectrometer further includes a mass analysis unit, which includes an ion implanter and a mass analyzer. The ion implanter and the mass analyzer are arranged along the first direction, and the ion implanter is closer to the photoionization unit than the mass analyzer.

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