Three-phase disturbance unit and reactive distillation column using the same

Abstract

This invention discloses a three-phase disturbance unit and a reactive distillation column using this unit. The three-phase disturbance unit is suitable for gas-liquid-solid reactions in which solid catalysts and / or packing particles are suspended in the liquid phase. It includes: a gas-phase nozzle, fixed to the tray of the reactive distillation column via a gas guide pipe and communicating with the lower gas phase space; the gas-phase nozzle is disposed in the liquid phase and has a first open surface; a cap, fitted over the gas-phase nozzle and having a second open surface; under the pressure of the rising gas, the pores of the second and first open surfaces become interconnected, forming a jet disturbance of gas towards the liquid phase and solid particles; and a magnetic control device, which intermittently controls the pores of the second and first open surfaces to shut off via an electromagnet, forming an adsorption of solid particles by the cap. This invention, through the controllable gas-phase nozzle of the three-phase disturbance unit, can provide sufficient disturbance within the column, effectively improving mass transfer efficiency and reaction rate. In the event of screen blockage leading to flooding, it can also rapidly reduce the liquid level on the corresponding tray.

Description

Technical Field

[0001] This invention relates to the field of oil refining and chemical technology, and in particular to a three-phase disturbance unit and a reactive distillation column using the unit. Background Technology

[0002] Reactive distillation columns play a crucial role in petroleum refining and chemical production. During reactive distillation, multiple feed streams mix, transfer mass, and react. To accelerate mass transfer and increase reaction rates, this is typically achieved by increasing the contact area between the two phases and by adding packing material and catalysts. Currently, the main method for increasing the contact area is to modify the flow or dispersion pattern of the rising or falling liquid streams to minimize the size of the dispersed phase droplets. At a constant flow rate, the smaller the size of the dispersed phase, the higher its dispersion within the continuous phase, and the higher the mass transfer efficiency. The most widely used industrial method for enhancing the dispersion of the dispersed phase is the use of trays such as sieve trays, bubble cap trays, valve trays, and jet trays in reactive distillation. When the dispersed phase flows through these trays, the openings on the trays cut and disperse the dispersed phase, thereby increasing its dispersion within the continuous phase and ultimately improving the efficiency of the two-phase mass transfer reaction.

[0003] In addition, adding packing material and catalyst to the trays of reactive distillation columns is also a common method to enhance the efficiency of mass transfer reactions. When the fluid flows over the surface of the packing material, the continuous phase wets the packing surface, and the dispersed phase flows over the packing surface, thereby enhancing the mass transfer between the two phases. When the fluid flows over the surface of the catalyst, the reaction rate will be significantly accelerated under the action of the catalyst. Therefore, maximizing the contact area between the packing material or catalyst and the fluid is key to increasing mass transfer efficiency and reaction rate. Currently, the main industrial method to increase the contact area between the packing material or catalyst and the fluid is to maximize the surface area of ​​the packing material or catalyst by making the packing material and catalyst into porous, granular, mesh, or ring-shaped structures, and then quantitatively stacking the packing material and catalyst on the trays, thereby increasing the contact area between the fluid and the packing material and catalyst, and thus improving the efficiency of the two-phase mass transfer reaction.

[0004] To achieve higher mass transfer efficiency, different tray types can generally be combined with packing and catalysts. However, regardless of the combination, the structure within the column is relatively stable. When the fluid flow within the column is stable, factors affecting mass transfer efficiency, such as the contact area between the two phases, the position of the packing / catalyst, and the contact area between the fluid and the packing / catalyst, are relatively stable. In particular, once the position of the packing / catalyst is relatively stable, it is prone to stacking and aggregation, making it difficult to maximize the utilization of the packing and catalyst. For example, Chinese patent CN205046018U discloses an apparatus for producing high-purity isobutylene using a novel structured packing, including a catalytic reactive distillation column. The catalytic reactive distillation column has a catalytic rectification section and a stripping section arranged from top to bottom. The catalytic rectification section is filled with several layers of packing with catalyst, and the stripping section is filled with several layers of packing without catalyst. Each packing layer includes two components: a first component and a second component. The first component is a windowed flow-guiding packing sheet, and the second component is a structured packing sheet. The packing material of this catalytic reaction distillation column is a windowed, flow-guided structured packing. Although it can effectively increase the gas-liquid mass transfer area and improve the gas-liquid mass transfer rate, it is still difficult to maximize the utilization of the packing material.

[0005] Therefore, there is an urgent need for a small disturbance unit that can provide sufficient disturbance within the tower and is simple and safe to operate.

[0006] The information disclosed in this background section is intended only to enhance the understanding of the overall background of the invention and should not be construed as an admission or in any way implying that the information constitutes prior art known to those skilled in the art. Summary of the Invention

[0007] The purpose of this invention is to provide a reactive distillation column suitable for gas-liquid-solid reactions, which can provide sufficient disturbance within the column through a controllable gas-phase nozzle of a three-phase disturbance unit, effectively improving mass transfer efficiency and reaction rate.

[0008] Another objective of this invention is to rapidly reduce the liquid level on the tray when flooding occurs due to screen blockage.

[0009] To achieve the above objectives, according to a first aspect of the present invention, a three-phase disturbance unit is provided, suitable for gas-liquid-solid reactions in which solid catalysts and / or packing particles are suspended in a liquid phase, comprising: a gas phase nozzle, which is fixed to a tray of a reactive distillation column via a gas guide pipe and communicates with a lower gas phase space; the gas phase nozzle is disposed in the liquid phase and has a first opening surface; a cap, which is fitted over the gas phase nozzle and has a second opening surface; under the pressure of the rising gas, the pores of the second opening surface and the first opening surface are connected to form a jet disturbance of the gas phase on the liquid phase and solid particles; and a magnetic control device, which intermittently controls the pores of the second opening surface and the first opening surface to shut off via an electromagnet, thereby forming an adsorption of solid particles by the cap.

[0010] Furthermore, in the above technical solution, the gas phase nozzle can be set as a cone shape, and the cap is adapted to the shape of the gas phase nozzle. Under the pressure of the rising gas, a gap is formed between the second opening surface and the first opening surface to allow the gas phase to pass through.

[0011] Furthermore, in the above technical solution, the gas phase nozzle may be provided with a first base, on which a vertically extending pin is fixedly provided. The pin passes through the second base of the cap and is in clearance fit with the second base. An electromagnet is provided below the second base. When energized and magnetic, the electromagnet attracts the second base of the cap to move downward so that the second opening surface and the first opening surface are tightly attached. At this time, the pores on the two opening surfaces are staggered and the solid particles in the liquid phase are adsorbed on the cap.

[0012] Furthermore, in the above technical solution, the electromagnet can be set as a ring and sleeved on the gas guide pipe; the electromagnet can be connected to the central control unit outside the tower through a wire.

[0013] Furthermore, in the above technical solution, the electromagnet can be fixed on the tray.

[0014] Furthermore, in the above technical solution, the gas phase nozzle can also be configured as an inverted cone shape, and the cap is adapted to the shape of the gas phase nozzle. Under the pressure of the rising gas, a gap is formed between the second opening surface and the first opening surface to allow the gas phase to pass through.

[0015] Furthermore, in the above technical solution, the gas phase nozzle may be provided with a first base, on which a vertically extending pin is fixedly installed. The pin passes through the second base of the cap and is in clearance fit with the second base. An electromagnet is installed above the second base and is fixedly connected to the pin. When energized and magnetic, the electromagnet attracts the second base of the cap to move upward, causing the second opening surface and the first opening surface to fit tightly together. At this time, the pores on the two opening surfaces are staggered and the solid particles in the liquid phase are adsorbed on the cap.

[0016] Furthermore, in the above technical solution, the gas phase nozzle can also be configured to be flat, and the cap is adapted to the shape of the gas phase nozzle. Under the pressure of the rising gas, a gap is formed between the second opening surface and the first opening surface to allow the gas phase to pass through.

[0017] Furthermore, in the above technical solution, the outer wall of the gas phase nozzle can be provided with protrusions at uniform intervals along the circumference, and the inner wall of the cap is provided with vertically extending grooves at corresponding positions; the electromagnet is set below the second base of the cap, and when energized and magnetic, the electromagnet attracts the cap to move downward so that the second opening surface and the first opening surface are tightly attached. At this time, the gas holes on the two opening surfaces are staggered and the solid particles in the liquid phase are adsorbed on the cap.

[0018] To achieve the above objectives, according to a second aspect of the present invention, a reactive distillation column is provided, suitable for gas-liquid-solid reactions in which solid catalysts and / or packing particles are suspended in the liquid phase, including the aforementioned three-phase disturbance unit; multiple three-phase disturbance units may be arranged at uniform intervals on each tray.

[0019] Furthermore, in the above technical solution, the height of the gas guide pipe connected to the gas phase nozzle in the three-phase disturbance unit can be designed to be the same, or it can be set at different heights.

[0020] Furthermore, in the above technical solution, each tray has a vertically extending downcomer along its outer edge, and a screen is provided at the inlet of the downcomer to trap solid particles in that tray.

[0021] Furthermore, in the above technical solution, the operation of the reactive distillation column includes the following stages: Initial operation stage: The liquid phase of the upper tray flows into the lower tray through the downcomer and accumulates. The three-phase disturbance unit located below the liquid surface opens the gas phase channel under the pressure of the rising gas. The gas phase forms a jet and mixes with the bubbling liquid phase. Under the action of the solid particles suspended in the liquid phase, gas-liquid mass transfer and reaction occur; After a period of operation: When the mass transfer and reaction efficiency decreases, the electromagnet is intermittently controlled to be magnetized, and the solid particles in the liquid phase are controlled to undergo an alternating process of adsorption and stripping on the cap surface, forming a gas-liquid-solid three-phase agitation.

[0022] Furthermore, in the above technical solution, the solid particles can be metal catalysts, metal fillers, and / or solid particles with metal supports.

[0023] Furthermore, in the above technical solution, when flooding occurs due to screen blockage, the gas phase channel entering the upper tray is shut off by continuously magnetizing the electromagnet of the upper three-phase disturbance unit. Simultaneously with shutting off the gas phase channel, the electromagnet of the three-phase disturbance unit near the screen can also be magnetized to remove the blocked solid particles.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] 1) This invention overcomes the shortcomings of insufficient and uncontrollable fluid disturbance in existing reactive distillation columns. The gas phase can enter from the bottom up through the gas guide pipe and be sprayed into the liquid phase through three-phase disturbance units set below the liquid surface on each layer of the column. This disturbs the liquid phase and the solid packing and / or catalyst particles suspended in the liquid phase, enhancing gas-liquid mass transfer and accelerating gas-liquid reaction. By intermittently controlling the opening and closing of the gas phase channel through the three-phase disturbance units, solid packing and / or catalyst particles with metallic components can be alternately adsorbed and stripped, causing the solid particles to move continuously in the liquid phase, disturbing the mixed gas and liquid, forming mutual disturbance of the gas-liquid-solid three phases, which can further improve the gas-liquid mass transfer and reaction efficiency.

[0026] 2) The three-phase disturbance unit of this invention can be controlled uniformly or separately; the opening and closing of the gas phase channel corresponds to the stripping and adsorption of solid particles, and this process can be repeated to disturb the catalyst / packing material and improve its mass transfer reaction efficiency with gas-liquid fluid. For non-metallic catalysts / supports / packing materials, a suitable amount of metal can be added inside the catalyst / support / packing material, or it can be wrapped with a metal mesh bag, etc., so that it can be attracted by a magnetic cap.

[0027] 3) The staggered three-phase disturbance unit design of this invention makes the disturbance superposition effect generated in the liquid phase better, and the gas-liquid mass transfer and reaction effect better.

[0028] 4) The gas phase nozzle of this invention can adopt similar shapes such as conical, inverted conical, and flat, and can obtain upward, downward, and vertically upward jet airflow. Compared with the conical gas phase nozzle, the structure of the inverted conical nozzle allows the electromagnet to be positioned without being affected by the air guide tube, and the contact area with the cap can be larger, maximizing the utilization of the electromagnet's magnetism and further increasing the three-phase disturbance of gas, liquid, and solid. The flat gas phase nozzle not only simplifies the components but also saves axial space and is easier to manufacture.

[0029] 5) This invention effectively solves the flooding problem caused by screen blockage. To prevent liquid phase from flowing back into the upper tray from a certain tray, a continuous electrical signal is input to the electromagnets of all or part of the three-phase disturbance units in the upper tray, closing the gas phase channel. This prevents backflow of liquid from the lower tray and increases the pressure in the lower tray, reducing the flow rate of liquid into that tray. Simultaneously, a continuous electrical signal can be input to the central control unit to magnetize the electromagnets of the three-phase disturbance units near the screen, more strongly attracting the solid particles blocking the screen and causing them to leave the screen, increasing the screen's flow capacity and thus increasing the downstream liquid flow rate.

[0030] The above description is merely an overview of the technical solution of the present invention. In order to better understand the technical means of the present invention and to implement it according to the contents of the specification, and to make the above and other objects, technical features and advantages of the present invention easier to understand, one or more preferred embodiments are listed below and described in detail with reference to the accompanying drawings. Attached Figure Description

[0031] Figure 1 This is a schematic diagram of the overall structure of the reactive distillation column of the present invention.

[0032] Figure 2 This is a schematic diagram of the internal structure of the reactive distillation column of the present invention.

[0033] Figure 3This is a cross-sectional schematic diagram of the first embodiment of the three-phase disturbance unit of the present invention (the gas phase channel is in the off state).

[0034] Figure 4 This is the present invention. Figure 3 A schematic diagram showing the relative positions of the pores on the first and second opening surfaces.

[0035] Figure 5-A This is the present invention. Figure 3 A schematic diagram of the middle gas phase channel in the closed state (solid particles adsorbed on the cap).

[0036] Figure 5-B This is the present invention. Figure 3 A schematic diagram of the middle gas phase channel in the open state (solid particles are blown off by the rising gas phase).

[0037] Figure 6 This is a cross-sectional schematic diagram of the second embodiment of the three-phase disturbance unit of the present invention (the gas phase channel is in the off state).

[0038] Figure 7 This is a cross-sectional schematic diagram of the third embodiment of the three-phase disturbance unit of the present invention (the gas phase channel is in the off state).

[0039] Figure 8 This is the present invention. Figure 7 A schematic diagram showing the relative positional relationship of the air holes on the first and second opening surfaces (also showing the groove structure opened on the inner wall of the cap).

[0040] Explanation of key figure labels:

[0041] 1-Reactive distillation column, 10-Train plate, 11-Downcomer, 110-Screen, 2-Central control unit, 20-Wire, 3-Three-phase disturbance unit, 31-Gas nozzle, 310-Gas pipe, 311-First opening surface, 3110-First gas hole, 312-First base, 32-Cap, 320-Slide groove, 321-Second opening surface, 3210-Second gas hole, 322-Second base, 33-Electromagnet, 330-Tray, 34-Pin. Detailed Implementation

[0042] The specific embodiments of the present invention will now be described in detail with reference to the accompanying drawings, but it should be understood that the scope of protection of the present invention is not limited to the specific embodiments.

[0043] Unless otherwise expressly stated, throughout the specification and claims, the term "comprising" or its variations such as "including" or "comprises" shall be understood to include the stated elements or components without excluding other elements or other components.

[0044] In this document, for ease of description, spatial relative terms such as “below,” “under,” “down,” “above,” “above,” “upper,” etc., are used to describe the relationship of one element or feature to another element or feature in the accompanying drawings. It should be understood that spatial relative terms are intended to encompass different orientations of an object in use or operation, in addition to those depicted in the figures. For example, if an object in the figure is flipped, an element described as “below” or “under” another element or feature would be oriented “above” that element or feature. Thus, the exemplary term “below” can encompass both the downward and upward orientations. An object may also have other orientations (rotated 90 degrees or other orientations), and the spatial relative terms used herein should be interpreted accordingly.

[0045] In this document, the terms "first," "second," etc., are used to distinguish two different elements or parts, and are not used to define specific positions or relative relationships. In other words, in some embodiments, the terms "first," "second," etc., can also be used interchangeably.

[0046] like Figure 1 As shown, this invention provides a reactive distillation column 1 suitable for gas-liquid-solid mass transfer reactions. The liquid phase can flow from top to bottom through downcomers to each tray, while the gas phase can enter from bottom to top through gas guide pipes and be sprayed into the liquid phase through three-phase disturbance units set below the liquid surface on each tray. This disturbs the liquid phase and the solid packing and / or catalyst particles suspended in the liquid phase, enhancing gas-liquid mass transfer and accelerating the gas-liquid reaction. By intermittently controlling the opening and closing of the gas phase channel through the three-phase disturbance units, solid packing and / or catalyst particles with metallic components can be alternately adsorbed and stripped, causing the solid particles to move continuously in the liquid phase, disturbing the mixed gas and liquid, forming mutual disturbance of the gas-liquid-solid three phases, which can further improve the gas-liquid mass transfer and reaction efficiency. In order to control the opening and closing of the gas phase channel in the reactive distillation column 1 and the adsorption and stripping of solid particles, the magnetic control device of the three-phase disturbance unit of each tray is connected to the central control unit 2 through the wire 20. This is used to transmit electrical signals to control the three-phase disturbance unit of each tray in a unified or separate manner.

[0047] Further as Figure 2 As shown, the three-phase disturbance unit 3 is arranged at uniform intervals on each tray. The gas guide pipe 310 (reference) in the three-phase disturbance unit 3 is connected to the gas phase nozzle 31. Figure 3The heights can be uniform or staggered. The inventors discovered that by changing the height of the gas guide pipe, the longitudinal distribution of the gas phase nozzles can be altered; by changing the horizontal position of the gas guide pipe and its distribution on the tray, the lateral distribution of the gas phase nozzles can be changed. The height of the gas guide pipe on the tray needs precise calculation. A uniform longitudinal distribution of the gas guide pipe maximizes the agitation effect on solid particles. However, the longer the gas guide pipe, the shorter the flow distance of the rising gas in the liquid phase, which affects the gas-liquid contact mass transfer reaction effect. Experimental studies have shown that the staggered three-phase agitation unit design results in a better superposition effect of the agitation generated in the liquid phase, leading to better gas-liquid mass transfer and reaction effects.

[0048] Further as Figure 2 As shown, each tray of the reactive distillation column 1 is provided with a vertically extending downcomer 11 along its outer edge. A screen 110 is provided at the inlet of the downcomer 11 to trap solid particles from that tray. The solid particles in this invention are packing and / or catalyst particles, specifically metal catalysts, metal packing, and / or solid particles with a metal support.

[0049] Further as Figures 3 to 8 As shown, the three-phase disturbance unit of the present invention is suitable for gas-liquid-solid reactions in which solid catalysts and / or packing particles are suspended in the liquid phase. The three-phase disturbance unit includes a gas phase nozzle 31, a cap 32, and a magnetic control device. The gas phase nozzle 31 is fixed to the tray 10 of the reactive distillation column via a gas guide pipe 310 and communicates with the lower gas phase space. The gas phase nozzle 31 is disposed in the liquid phase and has a first opening surface 311. First gas holes 3110 are uniformly arranged on the first opening surface 311 (see reference). Figure 4 The cap 32 is fitted over the outside of the gas phase nozzle 31 and has a second opening surface 321. Second gas holes 3210 are evenly distributed on the second opening surface 321 (see reference). Figure 4Under the pressure of the rising gas from the lower tray's gas phase space, the vents of the second opening surface 321 and the first opening surface 311 become open, creating a jet disturbance of gas relative to the liquid phase and solid particles. This results in gas-liquid bubbling mixing and agitation of the solid particles. The magnetic control device, via electromagnet 33, can intermittently control the vents of the second opening surface 321 and the first opening surface 311 to close, causing the cap 32 to adsorb solid particles. Specifically, by controlling the electromagnet 33 with a pulsed electrical signal to intermittently energize and magnetize, alternating between gas phase disconnection and particle adsorption with gas flow and particle stripping. When the electromagnet 33 is energized and magnetized, the cap, through contact with the electromagnet, also becomes magnetic, attracting solid particles such as metal catalysts, metal packing, or metal carriers flowing around the cap, causing these metal solid particles to adsorb and stack on the cap surface. When the electromagnet is de-energized, the cap loses its magnetism and shifts, causing the solid metal particles to detach from its surface. Simultaneously, high-pressure rising gas is ejected from the cap's openings, carrying the metal particles outwards. This process repeats, disturbing the catalyst / packing material and improving its mass transfer efficiency in the gas-liquid-fluid reaction. For non-metallic catalysts / supports / packing materials, adding an appropriate amount of metal inside or wrapping them with a metal mesh bag can also make them attractive to the magnetic cap.

[0050] Specifically, the gas guide pipe 310 can be a cylindrical conduit, with its upper end connected to the gas phase nozzle 31 and its lower end connected to the tray 10. The rising gas flow from the lower tray can flow into the gas phase nozzle 31 through the gas guide pipe 310 and then be injected into the liquid phase accumulated on this tray. The shape of the gas phase nozzle 31 is not fixed and can be various shapes such as conical, frustum, cubic, or spherical, depending on actual needs. The cap 32 covers the gas phase nozzle 31, and the shape of the cap is similar to that of the nozzle. The second opening surface 321 on the cap 32 can be tightly fitted with the first opening surface of the gas phase nozzle 31 under the action of the electromagnet 33. When the cap and the nozzle are tightly fitted, the opening of the cap can just intersect with the opening of the nozzle. At this time, there is no connecting space between the cap 32 and the gas phase nozzle 31, thereby achieving the purpose of closing the gas phase channel. When the electromagnet 33 is not energized and is magnetic, the cap and the gas nozzle are not in close contact, forming a space for gas flow. The rising gas flow enters this space through the opening on the gas nozzle 31, and then exits through the opening on the cap, mixing with the liquid phase in a bubbling manner. During the outflow of the rising gas from the lower tray, it is successively affected by the openings of the gas nozzle 31 and the cap 32, dispersing the continuous gas flow into multiple gas streams or bubble streams. This increases the dispersion of the gas in the liquid phase above the tray, thereby increasing the gas-liquid contact area and mass transfer efficiency. To ensure that the cap 32 maintains stable axial movement under the attraction of the electromagnet, this invention uses a pin or groove structure to restrict the direction of movement. Of course, other similar methods can also be used to maintain the stable direction of movement of the cap 32. The shape of the electromagnet can be adjusted according to the shape and arrangement of the gas nozzle and the cap.

[0051] The three-phase disturbance unit of the present invention will be described in detail below through three specific embodiments.

[0052] Example 1

[0053] like Figure 3 , Figure 4 As shown, in this embodiment of the three-phase disturbance unit, the gas phase nozzle 31 is conical, and the cap 32 is adapted to the shape of the gas phase nozzle 31. Under the pressure of the rising gas, a gap for gas phase passage is formed between the second opening surface 321 on the cap 32 and the first opening surface 311 on the gas phase nozzle 31 (see reference). Figure 5-B This can create an upward-sloping airflow. Further, for example... Figure 3As shown, the gas phase nozzle 31 also has a first base 312, on which a vertically extending pin 34 is fixedly mounted. The pin 34 passes through the second base 322 of the cap and is in clearance fit with the second base (ensuring that the movement of the cap is restricted to the axial direction, i.e., moving up and down along the axial direction). An electromagnet 33 is located below the second base 322. When energized and magnetic, the electromagnet 33 attracts the second base 322 of the cap to move downward, causing the second opening surface 321 of the cap and the first opening surface 311 of the gas phase nozzle to fit tightly together. At this time, the pores on the two opening surfaces are staggered, and solid particles in the liquid phase can be attracted to the cap due to its magnetic properties (see reference). Figure 5-A When electromagnet 33 is de-energized, the cap is demagnetized and moves upward under gas pressure, thus opening the gas phase channel. At this time, solid particles are blown off by the gas phase, achieving disturbance of the gas-liquid mixture by the solid phase. Further, as... Figure 3 As shown, the electromagnet 33 is configured as a ring and sleeved on the gas guide pipe 310. The electromagnet 33 is connected to the central control unit 2 outside the tower through the wire 20 (reference). Figure 1 The electromagnet 33 can be fixed using a tray, that is, the tray 330 is fixed on the air duct 310, and the electromagnet 33 is installed on the tray.

[0054] In this embodiment, the reactive distillation process involves the reaction of monomethyl maleate (MMM) and methanol to produce dimethyl maleate (DMM). The catalyst used is a metal oxide and is non-magnetic. Without catalyst treatment, only gas dispersion can be achieved, not three-phase disturbance with a solid phase. Considering that directly adding metal to the active component of the catalyst may affect its activity, this invention incorporates metal particles during catalyst support preparation to enable the catalyst support to be magnetically adsorbed. Liquid monomethyl maleate enters from the upper feed inlet of the reactive distillation column, while gaseous methanol enters from the bottom feed inlet, with the two reactants in countercurrent contact. As the liquid phase passes through a certain tray, it flows in along the upper downcomer 11, while the gas phase flows from the lower tray through tray 10 and gas guide pipe 310 into the gas phase nozzle 31. The gas phase then pushes up the cap 32 through the vent 3110 on the first opening surface 311 of the gas phase nozzle, and flows out through the vent 3210 on the second opening surface 321 of the cap through the gap between the cap and the nozzle. The continuous gas phase passes through the tray openings, nozzle openings, and cap openings successively, being dispersed into fine gas streams or bubble streams, increasing the mass transfer efficiency between the gas and liquid phases. Under the control of the central control unit 2, the cap moves down and closes with the nozzle after the electromagnet 33 is energized and magnetized. The catalyst carrier containing metal particles, carrying the active catalyst components, is attracted by the magnetized cap and adsorbs and stacks on the cap surface. After the electromagnet 33 is de-energized and demagnetized, the gas phase channel between the cap and the nozzle opens, and the gas flows out, carrying the catalyst to disperse in all directions, thereby increasing the disturbance of the gas-liquid-solid three-phase system, thus improving the catalyst utilization efficiency and increasing the gas-liquid mass transfer reaction efficiency.

[0055] Example 2

[0056] like Figure 6 As shown, the gas phase nozzle in this embodiment is inverted conical in shape, and the shape of the cap 32 is adapted to the gas phase nozzle 31. Under the pressure of the rising gas, a gap is formed between the second opening surface 321 of the cap 32 and the first opening surface 311 of the gas phase nozzle 31 to allow the gas phase to pass through, thereby forming a downwardly inclined airflow. Further as... Figure 6 As shown, the gas-phase nozzle 31 also has a first base 312, on which a vertically extending pin 34 is fixedly mounted. The pin 34 passes through the second base 322 of the cap and is in clearance fit with the second base. Unlike Embodiment 1, the electromagnet 33 is positioned above the second base 322 and is fixedly connected to the pin 34. In the energized and magnetic state, the electromagnet 33 attracts the second base 322 of the cap, causing it to move upwards and tightly contact the second opening surface 321 of the cap and the first opening surface 311 of the nozzle. At this time, the pores on the two opening surfaces are staggered, and the solid particles in the liquid phase are adsorbed onto the cap. In this embodiment, the position of the electromagnet 33 is not affected by the gas guide tube 310, and the contact area with the cap 32 can be larger, resulting in stronger magnetism in the cap. This maximizes the utilization of the electromagnet's magnetism and further increases the three-phase disturbance of gas, liquid, and solid compared to Embodiment 1. The opening and closing of the gas phase channel and the adsorption and stripping process of the solid phase in this embodiment are the same as in Embodiment 1, and will not be described again here.

[0057] Example 3

[0058] like Figure 7 , 8 As shown, the gas phase nozzle 31 in this embodiment is flat. This design not only simplifies the components but also saves axial space and facilitates processing. The cap 32 is adapted to the shape of the gas phase nozzle 31. Under the pressure of the rising gas, a gap is formed between the second opening surface 321 on the cap and the first opening surface 311 on the nozzle to allow the gas phase to pass through, forming a vertically upward sheet-like airflow. Unlike embodiments 1 and 2, the outer wall of the gas phase nozzle 31 has protrusions evenly spaced circumferentially, and the inner wall of the cap 32 has vertically extending grooves 320 at corresponding positions (see reference). Figure 8 The axial movement of the cap 32 is achieved through the cooperation of the protrusion and the groove. This structural design makes the movement of the cap more stable. Alternatively, a groove can be provided on the nozzle, and a corresponding protrusion on the cap, achieving the same technical effect. Similar to Embodiment 1, the electromagnet 33 is located below the second base 322 of the cap 32. When energized and magnetic, the electromagnet 33 attracts the cap downwards, causing the second opening surface 321 on the cap and the first opening surface 311 of the nozzle to fit tightly together. At this time, the air holes on the two opening surfaces are staggered (see reference). Figure 8 Furthermore, the solid particles in the liquid phase are adsorbed onto the cap 32. The opening and closing of the gas phase channel and the adsorption and stripping process of the solid phase in this embodiment are the same as in Example 1, and will not be described again here.

[0059] It should be noted that during the operation of a reactive distillation column, flooding may occur due to the accumulation of liquid phase on each tray. The three-phase disturbance unit of this invention can effectively solve this problem.

[0060] Specifically, refer to Figure 2 As shown, the operation of the reactive distillation column of the present invention may include the following stages:

[0061] During normal operation:

[0062] 1) During the initial operation phase, the liquid phase of the upper tray 10 flows into the lower tray through the downcomer 11 and accumulates. The three-phase disturbance unit 3 located below the liquid surface opens the injection channel under the pressure of the rising gas. The gas phase forms an injection and mixes with the liquid phase bubble. Under the action of the solid particles suspended in the liquid phase, gas-liquid mass transfer and reaction are carried out.

[0063] 2) After running for a period of time, when the mass transfer and reaction efficiency decreases, the electromagnet is intermittently magnetized to control the alternating process of adsorption and stripping of solid particles in the liquid phase on the cap surface, forming a three-phase agitation of gas, liquid and solid.

[0064] When screen blockage leads to flooding:

[0065] By continuously magnetizing the electromagnets of the upper three-phase disturbance unit, the gas phase channel entering the upper tray can be shut off. Simultaneously, the electromagnets of the three-phase disturbance unit near the screen can be magnetized to remove clogged solid particles. Specifically, refer to... Figure 2 At a certain tray, the downcomer 11 inlet screen 110 is blocked by catalyst or packing particles, causing a decrease in downcomer flow and resulting in flooding on that tray. To prevent backflow of liquid from this tray into the upper tray, the central control unit 2 inputs a continuous electrical signal to all or part of the electromagnets of the three-phase disturbance unit on the upper tray, closing the gas phase channel. This prevents backflow of liquid from the lower tray and increases the pressure on the lower tray, reducing the flow rate of liquid into this tray. Simultaneously, preferably but not limitingly, to resolve the screen blockage problem more quickly, the central control unit can also input a continuous electrical signal to magnetize the electromagnets of the three-phase disturbance unit 3 near the screen, more strongly attracting the solid particles blocking the screen and causing them to leave the screen, increasing the screen's flow capacity and thus increasing the downstream liquid flow. When the liquid level on this tray drops to a safe value, the gas phase channel on the upper tray is opened, restoring normal operation.

[0066] The foregoing description of specific exemplary embodiments of the present invention is for illustrative and explanatory purposes. These descriptions are not intended to limit the invention to the precise forms disclosed, and it will be apparent that many changes and variations can be made in accordance with the foregoing teachings. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application, thereby enabling those skilled in the art to implement and utilize various different exemplary embodiments of the invention, as well as various different choices and variations. Any simple modifications, equivalent changes, and alterations made to the foregoing exemplary embodiments should fall within the scope of protection of the present invention.

Claims

1. A three-phase disturbance unit, characterized in that, Suitable for gas-liquid-solid reactions in which solid catalysts and / or packing particles are suspended in the liquid phase, including: A gas phase nozzle is fixed to the tray of a reactive distillation column via a gas guide pipe and communicates with the lower gas phase space; the gas phase nozzle is disposed in the liquid phase and has a first opening surface; A cap is fitted over the outside of the gas phase nozzle and has a second opening surface; under the pressure of the rising gas, the gas holes of the second opening surface and the first opening surface are connected to form a jet disturbance of gas phase and liquid phase and solid particles. The magnetic control device uses an electromagnet to intermittently control the air holes of the second and first opening surfaces to achieve shut-off, thereby forming the cap's adsorption of solid particles. When the electromagnet is energized and magnetized, the electromagnet attracts the second base of the cap to move upward or downward, causing the second opening surface and the first opening surface to fit tightly together. At this time, the pores on the two opening surfaces are staggered and the solid particles in the liquid phase are adsorbed on the cap. When the electromagnet is energized and magnetized, the cap also becomes magnetic through contact with the electromagnet, thereby attracting the solid particles flowing around the cap, causing the solid particles to be adsorbed and stacked on the surface of the cap.

2. The three-phase disturbance unit according to claim 1, characterized in that, The gas phase nozzle is conical, and the cap is adapted to the shape of the gas phase nozzle. Under the pressure of the rising gas, a gap is formed between the second opening surface and the first opening surface for the gas phase to pass through.

3. The three-phase disturbance unit according to claim 2, characterized in that, The gas phase nozzle is provided with a first base, on which a vertically extending pin is fixedly installed. The pin passes through the second base of the cap and is in clearance fit with the second base. The electromagnet is located below the second base. When energized and magnetic, the electromagnet attracts the second base of the cap to move downward, so that the second opening surface and the first opening surface are tightly attached.

4. The three-phase disturbance unit according to claim 3, characterized in that, The electromagnet is ring-shaped and sleeved on the gas guide pipe; the electromagnet is connected to the central control unit outside the tower through a wire.

5. The three-phase disturbance unit according to claim 4, characterized in that, The electromagnet is fixed on the tray.

6. The three-phase disturbance unit according to claim 1, characterized in that, The gas phase nozzle is inverted conical in shape, and the cap is adapted to the shape of the gas phase nozzle. Under the pressure of the rising gas, a gap is formed between the second opening surface and the first opening surface for the gas phase to pass through.

7. The three-phase disturbance unit according to claim 6, characterized in that, The gas phase nozzle is provided with a first base, on which a vertically extending pin is fixedly installed. The pin passes through the second base of the cap and is in clearance fit with the second base. The electromagnet is disposed above the second base and is fixedly connected to the pin. When energized and magnetic, the electromagnet attracts the second base of the cap to move upward, so that the second opening surface and the first opening surface are tightly fitted together.

8. The three-phase disturbance unit according to claim 1, characterized in that, The gas phase nozzle is flat, and the cap is adapted to the shape of the gas phase nozzle. Under the pressure of the rising gas, a gap is formed between the second opening surface and the first opening surface for the gas phase to pass through.

9. The three-phase disturbance unit according to claim 8, characterized in that, The outer wall of the gas phase nozzle is provided with protrusions evenly spaced along the circumference, and the inner wall of the cap is provided with vertically extending grooves at corresponding positions; the electromagnet is located below the second base of the cap, and when energized and magnetic, the electromagnet attracts the cap to move downward so that the second opening surface and the first opening surface are tightly fitted together.

10. A reactive distillation column, characterized in that, Suitable for gas-liquid-solid reactions in which solid catalysts and / or packing particles are suspended in the liquid phase, including the three-phase disturbance unit as described in any one of claims 1 to 9; multiple three-phase disturbance units are arranged at uniform intervals on each tray.

11. The reactive distillation column according to claim 10, characterized in that, The gas guide pipes connected to the gas phase nozzle in the three-phase disturbance unit are at the same height or staggered in height.

12. The reactive distillation column according to claim 11, characterized in that, Each tray has a vertically extending downcomer along its outer edge, and a screen is installed at the inlet of the downcomer to trap solid particles in that tray.

13. The reactive distillation column according to claim 12, characterized in that, The operation of the reactive distillation column includes the following stages: Initial operation phase: The liquid phase of the upper tray flows into the lower tray through the downcomer and accumulates. The three-phase disturbance unit located below the liquid surface opens the gas phase channel under the pressure of the rising gas. The gas phase forms a jet and mixes with the bubbling liquid phase. Under the action of solid particles suspended in the liquid phase, gas-liquid mass transfer and reaction occur. After running for a period of time: when the mass transfer and reaction efficiency decreases, the electromagnet is intermittently magnetized to control the alternating process of adsorption and stripping of solid particles in the liquid phase on the cap surface, forming a three-phase agitation of gas, liquid and solid.

14. The reactive distillation column according to claim 13, characterized in that, The solid particles are metal catalysts, metal fillers, and / or solid particles with metal supports.

15. The reactive distillation column according to claim 13, characterized in that, When the screen becomes clogged and flooding occurs, the gas phase channel entering the upper tray is shut off by continuously magnetizing the electromagnet of the upper three-phase disturbance unit.

16. The reactive distillation column according to claim 15, characterized in that, While shutting off the gas phase channel entering the upper tray, the electromagnet of the three-phase disturbance unit near the screen is magnetized to draw out the blocked solid particles.

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