Fluidized bed reactor, heat removal tube and its application in acrylonitrile production

The optimized geometric configuration of vertical heat removal pipes and cyclone separators in fluidized bed reactors addresses bubble growth and heat transfer inefficiencies, enhancing production efficiency and yield in acrylonitrile synthesis.

JP7777526B2Active Publication Date: 2025-11-28CHINA PETROLEUM & CHEMICAL CORP +1
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Patent Information

Application Number
JP2022529712
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2019-11-20
Filing Date
2020-11-18
Publication Date
2025-11-28
Estimated Expiration
2040-11-18

AI Technical Summary

Technical Problem

Existing fluidized bed reactors for acrylonitrile production face challenges in effectively managing bubble growth, backmixing, and heat transfer, leading to inefficient production and increased deep oxidation product generation.

Method used

The design of a fluidized bed reactor with vertically arranged heat removal water pipes and cyclone separators, optimized by specific geometric ratios and configurations, to control bubble growth and enhance mass and heat transfer efficiency.

Benefits of technology

This design promotes rapid flow pattern changes, restricts bubble growth, reduces backmixing, and increases the conversion rate of feed gas, thereby improving the yield of target products and extending the operation time of the device.

✦ Generated by Eureka AI based on patent content.

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Abstract

A fluidized bed reactor and a heat removal pipe for the production of acrylonitrile, as well as their application, are disclosed. The fluidized bed reactor includes at least one reaction cooling section and a vertical internal structure provided within the reaction cooling section. Here, the area of ​​the reaction cooling section in a cross section that intersects the central axis of the fluidized bed reactor and is perpendicular thereto is defined as S1 (unit: m 2 If the outer contour circumference of the cross section of the vertical internal structure is L1 (expressed in meters), then L1 / S1 = 2.0 to 4.3 m -1 The fluidized bed reactor can promote the destruction of bubbles as early as possible and effectively limit the growth of bubbles.
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Description

Detailed Description of the Invention

[0001] [Technical Field] The present invention relates to a fluidized bed reactor and a heat removal pipe particularly suitable for placement in the fluidized bed reactor. Further, the present invention relates to the use of the fluidized bed reactor and the heat removal pipe in the production of acrylonitrile.

[0002] [Background technology] Acrylonitrile is an important chemical raw material in the petrochemical industry. The single-step process for producing acrylonitrile by propylene ammoxidation is widely used worldwide. Propylene is ammoxidized in a fluidized bed ammoxidation catalyst at a certain reaction temperature and pressure to produce acrylonitrile along with by-products such as acetonitrile and hydrocyanic acid, as well as CO and CO2 deep oxidation products. This reaction is highly exothermic and generates a large amount of heat.

[0003] The interior of a typical acrylonitrile fluidized bed reactor includes a propylene-ammonia distributor, an air distribution plate, a heat rejection pipe (also known as a cooling coil), and a cyclone separator. Here, the heat rejection pipe and the dipleg of the cyclone separator are arranged in the catalyst bed as vertical components of the fluidized bed. The heat rejection pipe can timely remove a large amount of heat generated during the reaction from the reaction system and maintain the reaction temperature at a stable state, and the cyclone separator can capture the catalyst carried by the upwardly moving gas and return the catalyst to the catalyst bed through the dipleg to reduce catalyst loss.

[0004] Conventional vertical components of a fluidized bed reactor are shown in Figures 1 and 2. Figure 1 is an axial view of the vertical component, and Figure 2 is a cross-sectional view of the vertical component. The vertical component includes a heat removal water pipe and a dipleg of a cyclone separator. The heat removal water pipe includes a cooling water pipe and a superheated water pipe, and high-pressure steam generated by the superheated water pipe is typically used in the turbines of air compressors and refrigerators. Alternatively, depending on the actual situation of the device, the heat removal water pipe may be provided with only a cooling water pipe. Here, the heat removal water pipe typically has an inlet, a straight pipe section, and an outlet, and two adjacent straight pipe sections are fluidly connected via a U-shaped pipe.

[0005] Chinese patent applications CN104941532A and CN104941529A disclose cooling coil designs for ammoxidation reactors that can be more closely packed by providing the individual lines defining the cooling coil in a horizontal arrangement rather than a linear arrangement.

[0006] Chinese Patent Application CN104624401A discloses an improved cyclone separator configuration. Each of a multi-stage set of cyclone separators includes a first-stage cyclone separator having a first-stage inlet configured to receive an upwardly flowing reaction stream from a fluidized catalyst bed in a reactor and at least partially separate the catalyst from the reaction stream. The ratio of square meters of first-stage inlet area per square meter of available cross-sectional area of ​​the reactor is about 0.03 to about 0.05.

[0007] Summary of the Invention When a fluidized-bed reactor is used for the propylene ammoxidation reaction to produce acrylonitrile, the propylene ammoxidation reaction is a gas-solid heterogeneous catalytic reaction. The gas flow conditions within the reactor are different from those of a free-bubbling bed. The bubbles generated by the gas passing through the distributor plate grow larger as the bed rises. The inventors have found that the presence of a vertical internal structure helps break down the bubbles, with small bubbles favoring mass transfer more than large bubbles, thus improving the production of useful products. Furthermore, the inventors have found that the vertical configuration of the heat removal water pipe and cyclone separator, in addition to their basic functions, also has the function of destroying bubbles, reducing backmixing between the gas and solid phases and contributing to the reduction of the generation of deep oxidation products. The distribution of these vertical components across the cross section of the reactor directly affects whether effective restriction of bubble growth or effective destruction of bubbles can be achieved, which in turn directly affects the reaction results. This finding led to the completion of the present invention.

[0008] Specifically, the present invention relates to the following features: 1. A fluidized-bed reactor comprising at least a reaction cooling section and a vertical internal structure disposed in the reaction cooling section, wherein the total length of the reaction cooling section in a direction along the central axis of the fluidized-bed reactor is defined as L (expressed in units of m), and the cross-sectional area of ​​the reaction cooling section in a cross section perpendicular to the central axis of the fluidized-bed reactor is defined as S1 (expressed in units of m) at any position within the region of the total length L of the reaction cooling section, preferably within the region from 49% L above the center point of the reaction cooling section to 49% L below the center point (more preferably within the region from 45% L above the center point of the reaction cooling section to 38% L below the center point, and even more preferably within the region from 40% L above the center point of the reaction cooling section to 8% L below the center point). 2 The perimeter of the cross section of the vertical internal structure (if there are multiple cross sections, the total perimeter of all cross sections) is defined as L1 (expressed in m), and L1 / S1 = 2.0 to 4.3 m -1, preferably L1 / S1=2.2 to 4.1 m -1 , and more preferably L1 / S1=2.4 to 3.9 m -1 A fluidized bed reactor.

[0009] 2. A fluidized bed reactor having any of the preceding or subsequent embodiments, wherein the vertical internal structure is a heat removal water pipe or a combination of a heat removal water pipe and a gas-solid separator (preferably a cyclone separator).

[0010] 3. A fluidized bed reactor having any of the preceding or subsequent embodiments, wherein the vertical internal structure is a heat removal water pipe, and the cross-sectional area of ​​the reaction cooling section in a cross section perpendicular to the central axis of the fluidized bed reactor is S1 (unit: m 2 The outer periphery of the cross section of the heat removal water pipe (calculated based on the cross section of the straight pipe section) (if there are multiple cross sections, the total outer periphery of all cross sections) is defined as L2 (expressed in m), and L2 / S1 = 1.7 to 3.6 m -1 , preferably L2 / S1=1.9 to 3.5 m -1 , and more preferably L2 / S1=2.1 to 3.3 m -1 The vertical internal structure optionally further includes a gas-solid separator (preferably a cyclone separator), and the cross-sectional area of ​​the reaction cooling section in a cross section perpendicular to the central axis of the fluidized bed reactor is S1 (unit: m 2 The perimeter of the cross section of the gas-solid separator (calculated based on the dipleg) (if there are multiple cross sections, this refers to the sum of the perimeters of all the cross sections) is defined as L3 (expressed in m), and L3 / S1 = 0.25 to 0.85 m -1 , preferably L3 / S1=0.30 to 0.75 m -1 , more preferably L3 / S1=0.35 to 0.65 m -1 A fluidized bed reactor.

[0011] 4. A fluidized bed reactor having any of the preceding or subsequent embodiments, wherein the number of heat removal water pipes (calculated based on the straight pipe sections) is 220 to 5000, preferably 300 to 2400, and / or the number of gas-solid separators (calculated based on diplegs) is 16 to 516, preferably 16 to 210, and / or the ratio of the number of straight pipe sections to the number of diplegs is 8.5 to 24.0, preferably 10.0 to 23.0, more preferably 11.5 to 21.0.

[0012] 5. A fluidized bed reactor having any of the preceding or subsequent embodiments, wherein the outer diameters of the straight pipe sections are the same as or different from each other and are independently 80 to 180 mm, preferably 90 to 170 mm, and / or the inner diameters of the straight pipe sections are the same as or different from each other and are independently 60 to 150 mm, preferably 70 to 140 mm, and / or the lengths of the straight pipe sections are the same as or different from each other and are independently 4.0 to 13 m, preferably 5.5 to 12.0 m, and / or the lengths of the dipleg sections are the same as or different from each other and are independently 4.0 to 13 m, preferably 5.5 to 12.0 m, and / or The outer diameters of the diplegs are the same or different and are independently 150 to 410 mm, preferably 200 to 360 mm, and / or the inner diameters of the diplegs are the same or different and are independently 130 to 400 mm, preferably 180 to 350 mm, and / or the lengths of the diplegs are the same or different and are independently 6 to 14 m, preferably 10 to 13 m, and / or the reaction cooling zone has a diameter of 5 to 29 m, preferably 7 to 20 m, and a length of 19.6 to 660 m. 2 , preferably 38.5 to 314 m 2 and / or a length L of 4 to 12.5 m, preferably 5.5 to 11.5 m.

[0013] 6. A fluidized bed reactor having any of the preceding or subsequent aspects, comprising, in this order from top to bottom, a head, a dilute phase region, said reaction cooling section, a pre-reaction section, and a cone, and further comprising a gas distribution plate and, optionally, a fluid distributor provided in said pre-reaction section.

[0014] 7. A fluidized bed reactor comprising any of the preceding or subsequent embodiments, wherein the reaction cooling section has a substantially circular cross section, and / or the cross section of the vertical internal configuration has a substantially circular inner contour and a substantially circular outer contour, and / or the cross section of the vertical internal configuration has a substantially circular inner contour and a substantially circular outer contour with a protrusion, and / or the vertical internal configuration includes a heat removal water pipe, the heat removal water pipe having a heat removal medium inlet and n straight pipes (preferably straight circular pipes a first straight pipe section having a tip end connected to the heat removing medium inlet, a tail end of the nth straight pipe section connected to the heat removing medium outlet, and a rear end of the ith straight pipe section connected to the head end of the (i+1)th straight pipe section via a U-shaped pipe, n is an integer of 2 to 100 (preferably an integer of 2 to 20), i is an arbitrary integer of 1 to n-1, and a protrusion is provided on the outer wall of part or all (e.g., 1 to 100%, 5 to 80%, or 10 to 40%) of the straight pipe section.

[0015] 8. A heat removal water pipe having a heat removal medium inlet, n straight pipe sections (preferably straight circular pipes), and a heat removal medium outlet, wherein the head end of a first straight pipe section communicates with the heat removal medium inlet, the tail end of the nth straight pipe section communicates with the heat removal medium outlet, and the tail end of the i-th straight pipe section communicates with the head end of the (i+1)-th straight pipe section via a U-shaped pipe, n is an integer of 2 to 100 (preferably an integer of 2 to 20), i is any integer between 1 and n-1, and a protrusion is provided on the outer wall of some or all (1 to 100%, 5 to 80%, or 10 to 40%, for example) of the straight pipe sections.

[0016] 9. A heat water removal pipe having any of the preceding or subsequent embodiments, wherein the straight pipe sections have outer diameters that are the same as or different from each other and are independently 80 to 180 mm, preferably 90 to 170 mm, and / or the straight pipe sections have inner diameters that are the same as or different from each other and are independently 60 to 150 mm, preferably 70 to 140 mm, and / or the straight pipe sections have lengths that are the same as or different from each other and are independently 4.0 to 13 m, preferably 5.5 to 12.0 m, and / or the center lines of any two adjacent straight pipe sections are parallel to each other, and the distance between the center lines of any two adjacent straight pipe sections is the same as or different from each other (preferably the same), and is independently 160 to 540 mm, preferably 180 to 430 mm.

[0017] 10. A heat water removal pipe having any of the preceding or subsequent aspects, wherein the protrusion extends continuously or discontinuously in a direction along the centerline of the straight pipe section, and / or the protrusion extends continuously or discontinuously around the centerline of the straight pipe section, such as in the form of a ring or a spiral.

[0018] 11. A heat removal pipe having any of the preceding or subsequent embodiments, wherein, when the protrusion extends continuously or discontinuously in a direction along the center line of the straight pipe section, the extension length Lt of the protrusion is not longer than the length Lz of the straight pipe section (preferably Lt / Lz is 0.05 to 0.95, more preferably 0.1 to 0.6), and / or when the protrusion extends continuously or discontinuously around the center line of the straight pipe section in the form of a ring, the height Hh of the ring is not longer than the length Lz of the straight pipe section (preferably Hh / Lz is 0 to 0.5, more preferably 0 a heat removal water pipe in which the height Ht of the helix is ​​0.005 to 0.3 times (preferably 0.008 to 0.1 times) the outer diameter of the straight pipe section, and / or the width of the protrusion is 0.005 to 0.3 times (preferably 0.008 to 0.2 times) the outer diameter of the straight pipe section, and / or if the protrusion extends continuously or discontinuously around the center line of the straight pipe section in the form of a spiral, the height Ht of the spiral is not longer than the length Lz of the straight pipe section (preferably Ht / Lz is 0.1 to 0.95, more preferably 0.2 to 0.6), and / or the height of the protrusion is 0.005 to 0.3 times (preferably 0.008 to 0.1 times) the outer diameter of the straight pipe section, and / or the width of the protrusion is 0.005 to 0.3 times (preferably 0.008 to 0.2 times) the outer diameter of the straight pipe section.

[0019] 12. A heat removal water pipe having any of the preceding or subsequent aspects, wherein the protrusion extends continuously or discontinuously around the center line of the straight pipe section, and an angle between the center line of the protrusion and the center line of the straight pipe section is greater than 0° and less than or equal to 90° (preferably greater than or equal to 5° and less than or equal to 75°, more preferably greater than or equal to 10° and less than or equal to 60°).

[0020] 13. A fluidized bed reactor comprising, in this order from top to bottom, a head, a dilute phase region, a dense phase region, and a cone, the dense phase region being provided with at least one heat removal water pipe having any of the preceding or subsequent embodiments.

[0021] 14. Use of a fluidized bed reactor according to any of the preceding or subsequent embodiments in the production of epoxy compounds (such as propylene oxide) or unsaturated nitriles (such as acrylonitrile) by an olefin (such as propylene) oxidation process or an ammoxidation process.

[0022] 15. A method for producing an unsaturated nitrile, comprising subjecting an olefin (such as propylene) to an ammoxidation reaction in a fluidized bed reactor according to any of the preceding or subsequent embodiments to produce an unsaturated nitrile (such as acrylonitrile).

[0023] BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic front view of a prior art fluidized bed reactor.

[0024] FIG. 2 is a schematic cross-sectional view of a prior art fluidized bed reactor cooling section.

[0025] FIG. 3 is a schematic cross-sectional view of the reaction cooling section of the fluidized bed of the present invention.

[0026] FIG. 4 is a schematic front view of a fluidized bed reactor of the present invention.

[0027] FIG. 5 is a schematic diagram of an exemplary embodiment of the heat rejection water pipe of the present invention.

[0028] FIG. 6 shows a graph of the pressure pulsation intensity of Comparative Example 1.

[0029] FIG. 7 shows a graph of the pressure pulsation intensity of Comparative Example 2.

[0030] FIG. 8 shows a graph of pressure pulsation intensity for Example 1.

[0031] FIG. 9 shows a graph of pressure pulsation intensity for Example 2.

[0032] FIG. 10 shows a graph of pressure pulsation intensity for Example 3.

[0033] (Explanation of symbols) 1: Fluidized bed reactor 2: Mixed feed gas supply line 3: Cyclone separator inlet 4: Heat removal water pipe 5: Cyclone separator cylinder 6: Cyclone separator cone 7: Cyclone separator ash bucket 8: Dipleg of the second stage (third stage) of the cyclone separator 9: Dipleg of the first stage of the cyclone separator [Technical effect] By using the fluidized bed reactor of the present invention, it is possible to promote a change in the flow pattern in the fluidized bed as quickly as possible, and to promote the destruction of bubbles.

[0034] By using the fluidized bed reactor of the present invention, the growth of bubbles can be effectively restricted, and as a result, the conversion rate of the feed gas can be improved, and the yield of the target reaction product can be increased.

[0035] By using the fluidized bed reactor of the present invention, backmixing of the gas and solid phases and the production of deep oxidation products can be reduced.

[0036] By using the fluidized bed reactor of the present invention, the heat and mass transfer efficiency can be improved, and the operation time of the device can be extended.

[0037] Detailed Description of the Invention The present application will be described in detail below with reference to embodiments thereof, but it should be noted that the scope of the present application is not limited by those embodiments, but is defined by the appended claims.

[0038] All publications, patent applications, patents and other references cited in this specification are incorporated by reference in their entirety.Unless otherwise defined, all technical and scientific terms used in this specification have the same meaning as those generally understood by those skilled in the art.In the event of conflict, the contents described in this specification, including definitions, shall prevail.

[0039] When a material, method, component, apparatus, or device described herein is modified by phrases such as "known to those skilled in the art," "generally known in the art," or the like, it is to be understood that said material, method, component, apparatus, or device includes not only those conventionally used in the art at the time of filing this application, but also those that are not currently in general use, but which have become generally known in the art as being suitable for a similar purpose.

[0040] In the context of this application, the term "substantially" means that deviations that would be considered acceptable or reasonable to one of ordinary skill in the art are permitted to exist, such as within ±10%, ±5%, ±1%, ±0.5%, or ±0.1%.

[0041] In the context of this application, unless otherwise specified, all percentages, parts, ratios, etc. are expressed by weight and all pressures given are gauge pressures.

[0042] In the context of the present application, any two or more embodiments of the present application can be arbitrarily combined, and the resulting technical solution forms part of the initial disclosure of the present application and falls within the scope of the present application.

[0043] According to one embodiment of the present invention, the present invention relates to a fluidized bed reactor, particularly a fluidized bed reactor for the production of acrylonitrile, wherein the fluidized bed reactor includes at least a reaction cooling section and a vertical internal structure disposed within the reaction cooling section.

[0044] According to one embodiment of the present invention, when the length of the reaction cooling section in the direction along the central axis of the fluidized-bed reactor is called L (expressed in m), a cross section of the reaction cooling section and a cross section of the vertical internal structure can be obtained at any position within the range of the total length L of the reaction cooling section on a cross-sectional plane that intersects the central axis of the fluidized-bed reactor and is perpendicular to the central axis of the fluidized-bed reactor. Furthermore, when there are multiple vertical internal structures, cross sections of multiple vertical internal structures can be obtained. These cross sections have an outer contour having an area and a circumference (called the outer contour circumference), such as the circles represented by 4, 8, and 9 in Figure 3. Here, the area of ​​the cross section of the reaction cooling section is defined as S1 (expressed in m 2 The outer contour circumference of the cross section of the vertical internal structure (if there are multiple cross sections, this refers to the sum of the outer contour circumferences of all cross sections) is L1 (expressed in meters), and L1 / S1 = 2.0 to 4.3 m -1 Here, L1 / S1 = 2.0 to 4.3 m -1 is preferably within the region from 49%L above the center point of the reaction cooling section to 49%L below the center point, more preferably within the region from 45%L above the center point of the reaction cooling section to 38%L below the center point, and even more preferably within the region from 40%L above the center point of the reaction cooling section to 8%L below the center point. Preferably, L1 / S1=2.2 to 4.1m -1 , preferably L1 / S1=2.4-3.9m -1 L1 / S1 is 2.0m -1 If the L1 / S1 is less than 4.3m, the device may operate unstably. -1 If the vertical internal configuration exceeds 1000 rpm, the space inside the reactor may be excessively occupied. According to one embodiment of the present invention, a specific example of the vertical internal configuration includes a heat rejection water pipe and a gas-solid separator, and in particular, a combination of a heat rejection water pipe and a gas-solid separator.

[0045] According to one embodiment of the present invention, the cross-sectional area S1 of the reaction cooling section is typically 19.6 to 660 m 2 , preferably 38.5 to 314 m 2 is.

[0046] According to an embodiment of the present invention, if the outer contour is substantially circular, then the outer contour circumference = 3.14 x D, where D refers to the diameter of the outer contour (expressed in m) which corresponds to the outer diameter (expressed in m) of the relevant vertical internal feature (for example, the straight section of a heat rejector tube or the dipleg of a cyclone separator).

[0047] According to one embodiment of the present invention, the length L of the reaction cooling section along the central axis of the fluidized bed reactor is typically 4 to 12.5 m, preferably 5.5 to 11.5 m.

[0048] According to one embodiment of the present invention, the heat removal pipe includes a cooling water pipe for removing heat generated by the reaction from the reaction system by utilizing the latent heat of the cooling liquid in the pipe, and a superheated water pipe for removing heat generated by the reaction from the reaction system by utilizing the sensible heat of the cooling liquid in the pipe. Here, the diameters of the cooling water pipe and the superheated water pipe may be the same or different, and are not particularly limited, but may be any conventionally used diameter.

[0049] According to one embodiment of the present invention, the straight pipe section of the heat removal water pipe is disposed substantially in the dense phase region of the fluidized bed reactor and is used to timely remove reaction heat from the system and maintain stable operation of the system. For this reason, in the context of this specification, the term "reaction cooling section" refers to the region of the fluidized bed reactor in which the heat removal water pipe is provided, more particularly the region in the fluidized bed reactor in which the straight pipe section of the heat removal water pipe is disposed, and even more particularly the region in the dense phase region of the fluidized bed reactor in which the straight pipe section of the heat removal water pipe is disposed.

[0050] According to one embodiment of the present invention, the heat removal water pipe has an inlet, a straight pipe section, and an outlet, and two adjacent straight pipe sections are typically connected via a U-shaped pipe to be in fluid communication with each other. The heat removal water pipe may include only one straight pipe section, only one U-shaped pipe, or may be formed by connecting multiple U-shaped pipes in series. The greater the number of U-shaped pipes, the larger the outer contour circumference L1. In addition, the heat removal water pipes are typically evenly distributed within the fluidized bed reactor. As a specific example, if the fluidized bed reactor is divided into quadrants, A, B, C, and D, the outer contour circumferences of the heat removal water pipes in each quadrant are substantially the same.

[0051] According to one embodiment of the present invention, the gas-solid separator may be a cyclone separator. Here, the cyclone separator has a gas inlet, a cone, an ash bucket, diplegs, and a gas outlet. The diplegs are arranged in a vertical configuration in the dense phase region of the catalyst bed, i.e., a fluidized-bed reactor, and another configuration is arranged in the dilute phase region at the top of the fluidized-bed reactor. Here, the cyclone separator may be a single-stage cyclone separator, with one dipleg corresponding to one cyclone separator, or may be a configuration in which two or more cyclone separators are connected in series. Typically, the diplegs of the first-stage cyclone separator extend to a specific position at the bottom of the catalyst bed (corresponding to the bottom of the dense phase region), and the diplegs of the second-stage (or third-stage) cyclone separator extend to a specific position at the bottom, middle, or top of the catalyst bed (corresponding to the bottom, middle, or top of the dense phase region).

[0052] According to an embodiment of the present invention, two or more cyclone separators are typically arranged in a series connection. During the operation of the fluidized bed reactor, part of the fine particle catalyst is carried away from the catalyst bed by the reaction gas, and the catalyst carried by the gas enters the cyclone separator through the inlet of the first stage cyclone separator. After passing through the first stage cyclone separator, most of the catalyst returns to the catalyst bed along the dipleg of the first stage cyclone separator, and the remaining small part of the catalyst enters the second stage cyclone separator together with the gas for further gas-solid separation, and the separated catalyst returns to the catalyst bed along the dipleg of the second stage cyclone separator, and the end of the dipleg of the second stage cyclone separator is provided with a blade valve, and the second stage cyclone separator can be further connected in series with a third stage cyclone separator for further gas-solid separation, and the separated catalyst returns to the catalyst bed along the dipleg, and the gas flows upward through the gas collection chamber and then leaves the reactor. Each cyclone separator has a dipleg for returning the separated catalyst to the catalyst bed. A set of multi-stage cyclone separators has multiple diplegs.

[0053] According to one embodiment of the present invention, the vertical internal structure is a heat removal water pipe, and the cross-sectional area of ​​the reaction cooling section in a cross section perpendicular to the central axis of the fluidized bed reactor is S1 (unit: m 2 When the outer contour circumference of the cross section of the heat removal pipe (calculated based on the straight pipe section) (if there are multiple cross sections, it refers to the total outer contour circumference of all cross sections) is expressed as L2 (expressed in m), L2 / S1 = 1.7~3.6m -1 , preferably L2 / S1=1.9 to 3.5 m -1 , and more preferably L2 / S1=2.1 to 3.3 m -1 The ratio is 1.7m -1 If the ratio is less than 3.6m, there is a risk of impeding the long-term stable operation of the reactor. For example, the molybdenum sheet may adhere to the wall of the heat removal water pipe, reducing the heat transfer coefficient and causing a temperature control failure. -1Exceeding this value means that the number of heat removal water pipes increases, which may be advantageous for breaking down bubbles, but causes inconvenience to technicians when performing maintenance on the device.

[0054] According to one embodiment of the present invention, the number of heat removal water pipes in the fluidized bed reactor (calculated based on the straight pipe section) is typically 220 to 5,000, and preferably 300 to 2,400.

[0055] According to one embodiment of the present invention, the straight pipe portions of the heat removal water pipes may have the same or different outer diameters, each independently ranging from 80 to 180 mm, preferably from 90 to 170 mm.

[0056] According to one embodiment of the present invention, the straight pipe portions of the heat removal water pipes may have the same or different inner diameters, each independently ranging from 60 to 150 mm, preferably from 70 to 140 mm.

[0057] According to one embodiment of the present invention, the lengths of the straight pipe portions of the heat removal water pipes may be the same or different, and are independently 4.0 to 13 m, preferably 5.5 to 12.0 m.

[0058] According to one embodiment of the present invention, the vertical internal structure is a gas-solid separator, in particular a cyclone separator. For this purpose, the area of ​​the reaction cooling cross section in a vertical cross section that intersects the central axis of the fluidized bed reactor is defined as S1 (unit: m 2 If the outer contour circumference of the cross section of the gas separator (if there are multiple cross sections, it means the total outer contour circumference of all cross sections) is L3 (expressed in m), then L3 / S1 = 0.25 to 0.85 m -1 , preferably L3 / S1=0.30 to 0.75 m -1 , more preferably L3 / S1=0.35 to 0.65 m -1 The ratio is 0.25m -1 If the ratio is less than 0.85m, the catalyst separation may be insufficient or the dipleg may be blocked. -1If it is larger, on the one hand, the equipment cost increases, on the other hand, more effective space in the reactor is occupied, and under the same reaction conditions, the linear velocity of the reaction operation increases, which may cause a further increase in catalyst entrainment.

[0059] According to an embodiment of the present invention, the number of gas-solid separators (calculated based on diplegs) in the fluidized bed reactor is 16-516, preferably 16-210.

[0060] According to one embodiment of the present invention, in the fluidized bed reactor, the ratio of the number of straight pipe sections to the number of diplegs is 8.5 to 24.0, preferably 10.0 to 23.0, and more preferably 11.5 to 21.0.

[0061] According to one embodiment of the present invention, the outer diameters of the diplegs of the gas-solid separator may be the same or different, and each independently ranges from 150 to 410 mm, preferably from 200 to 360 mm.

[0062] According to one embodiment of the present invention, the inner diameters of the diplegs of the gas-solid separator may be the same or different, and each independently has a value of 130 to 400 mm, preferably 180 to 350 mm.

[0063] According to one embodiment of the present invention, the lengths of the diplegs of the gas-solid separator may be the same or different and are independently 6 to 14 m, preferably 10 to 13 m.

[0064] According to one embodiment of the present invention, the fluidized bed reactor comprises, from top to bottom, a head, a dilute phase zone, a reaction cooling section, a pre-reaction section, and a cone, and further comprises a gas distribution plate and, optionally, a fluid distributor provided in the pre-reaction section. Here, the fluidized bed reactor is preferably a fluidized bed reactor for producing acrylonitrile. In this case, the other distributor plate is an air distributor plate, and the fluid distributor is a propylene-ammonia distributor. The structure and operation of a fluidized bed reactor, particularly a fluidized bed reactor for producing acrylonitrile, etc., can be directly applied by those skilled in the art, and a detailed description thereof will be omitted herein.

[0065] According to one embodiment of the present invention, the cross section of the reaction cooling section is substantially circular, and the diameter of the reaction cooling section is typically 5 to 29 m, preferably 7 to 20 m, but may not be limited thereto.

[0066] According to one embodiment of the present invention, the inner and outer cross-sectional contours of the vertical inner component are substantially circular, for this purpose the vertical inner component has the shape of a substantially circular tube, in particular a straight circular tube.

[0067] According to one embodiment of the present invention, the vertical internal structure has a substantially circular inner contour and a substantially circular outer contour with protrusions. For this purpose, the appearance of the vertical internal structure is a substantially circular tube with protrusions, and the interior of the vertical internal structure has a substantially circular tubular shape. An example of such a vertical internal structure is the heat water removal pipe of the present invention described below, which is characterized by having protrusions on the outer wall of part or all of the straight pipe section.

[0068] According to one embodiment of the present invention, the vertical internal structure includes the heat removal water pipe of the present invention, as described below. For vertical internal structures having such a specific structure, the cross-sectional outer shape is no longer substantially circular, but has a substantially circular shape with protrusions (i.e., an irregular shape). Therefore, the outer contour circumference must be calculated according to the actual situation of the irregular shape. Regardless of the contour shape, those skilled in the art can use known mathematical and geometric methods to calculate the outer contour circumference of the shape, and a detailed description thereof will be omitted here.

[0069] According to one embodiment of the present invention, the present invention relates to a heat removal water pipe having a heat removal medium inlet, n straight pipe sections, and a heat removal medium outlet. Here, the straight pipe sections are preferably straight circular pipes.

[0070] According to one embodiment of the present invention, in a heat removal water pipe, the tip of the first straight pipe section communicates with the heat removal medium inlet, the rear end of the nth straight pipe section communicates with the heat removal medium outlet, and the rear end of the ith straight pipe section communicates with the tip of the (i+1)th straight pipe section via a U-shaped pipe, and protrusions are provided on part or all of the outer walls of the straight pipe sections. Here, n is an integer of 2 to 100, preferably 2 to 20, and i is any integer of 1 to n-1. Furthermore, the term "part or all" may include, for example, 1 to 100%, 5 to 80%, or 10 to 40% of the total amount, but may not be limited to these.

[0071] According to one embodiment of the present invention, the protrusion is connected to the outer wall of the straight pipe section by any method, including spot welding, continuous welding, integral molding, and the like.

[0072] According to one embodiment of the present invention, the straight pipe portions of the heat removal water pipes have outer diameters that are the same as or different from one another and are independently 80 to 180 mm, preferably 90 to 170 mm.

[0073] According to one embodiment of the present invention, the straight pipe portions of the heat removal water pipes have inner diameters that are the same as or different from one another and are independently 60 to 150 mm, preferably 70 to 140 mm.

[0074] According to one embodiment of the present invention, the lengths of the straight pipe portions of the heat removal water pipes may be the same as or different from each other, and are independently 4.0 to 13.0 m, preferably 5.5 to 12.0 m.

[0075] According to one embodiment of the present invention, in the heat removal water pipe, the center lines of any two adjacent straight pipe sections are parallel to each other, and the distance between the center lines of any two adjacent straight pipe sections is the same or different (preferably the same), and is independently 160 to 540 mm, preferably 180 to 430 mm.

[0076] According to one embodiment of the present invention, in the heat removal water pipe, the protrusions extend continuously or discontinuously along (parallel to) the center line of the straight pipe portion, and the number of protrusions may be 1 to 10, 1 to 4, or 1 or 2.

[0077] According to one embodiment of the present invention, in the heat removal pipe, the protrusions extend continuously or discontinuously around the center line of the straight pipe section in the form of a ring or a spiral, etc. Here, the number of protrusions may be 1 to 20, 1 to 10, 1 to 4, or 1 or 2.

[0078] According to one embodiment of the present invention, in the heat removal pipe in which the protrusions extend continuously or discontinuously in a direction along the center line of the straight pipe section, the extension length Lt of the protrusions is equal to or less than the length Lz of the straight pipe section, and Lt / Lz is preferably 0.05 to 0.95, and more preferably 0.1 to 0.6. When multiple protrusions are present, different protrusions may be parallel to each other or may be angled from each other, preferably parallel to each other, and more preferably uniformly arranged in the radial direction of the straight pipe section.

[0079] According to one embodiment of the present invention, in a heat removal pipe in which a protrusion is in the form of a ring and extends continuously or discontinuously around the center line of a straight pipe section, the height Hh of the ring is equal to or less than the length Lz of the straight pipe section, and preferably Hh / Lz is 0 to 0.9, more preferably 0.01 to 0.6. Here, the height Hh refers to the length of the corresponding portion of the straight pipe section having the protrusion. When multiple protrusions are present, the vertical interval l1 between different protrusions is equal to or less than the length Lz of the straight pipe section, and preferably l1 / Lz is 0.01 to 0.5, more preferably 0.03 to 0.4. Preferably, the angle α1 between the center line of the protrusion and the center line of the straight pipe section is greater than 0° and equal to or less than 90°, preferably 5° to 75°, more preferably 10° to 60°.

[0080] According to one embodiment of the present invention, in a heat removal pipe in which a protrusion is spirally formed and extends continuously or discontinuously around the center line of a straight pipe section, the height Ht of the spiral is equal to or less than the length Lz of the straight pipe section, and preferably Ht / Lz is 0.1 to 0.95, more preferably 0.2 to 0.6. Here, the height Ht refers to the length of the portion of the straight pipe section corresponding to the protrusion. In addition, the thread pitch l1 of the spiral is not greater than the length Lz of the straight pipe section, and preferably l1 / Lz is 0.01 to 0.5, more preferably 0.03 to 0.4. Preferably, the angle α1 between the center line of the protrusion and the center line of the straight pipe section is greater than 0° and less than 90°, preferably 5° to 75°, more preferably 10° to 60°. Furthermore, the angle α2 between the tangent line of the protrusion along the straight pipe section and the center line of the straight pipe section is preferably 0° to 90°, more preferably 5° to 75°, more preferably 10° to 60°.

[0081] According to one embodiment of the present invention, in the heat removal water pipe, the height of the protruding portion is 0.005 to 0.3 times, preferably 0.008 to 0.1 times, the outer diameter of the straight pipe portion.

[0082] According to one embodiment of the present invention, in the heat removal water pipe, the width of the protruding portion is 0.005 to 0.3 times, preferably 0.008 to 0.2 times, the outer diameter of the straight pipe portion.

[0083] According to one embodiment of the present invention, the present invention also relates to a fluidized-bed reactor comprising, from top to bottom, a head, a dilute-phase region, a dense-phase region, and a cone. Here, at least one heat removal pipe according to any of the above-described aspects of the present invention is provided in the dense-phase region. Preferably, the heat removal pipes are uniformly distributed within the fluidized-bed reactor. For a specific example, if the fluidized-bed reactor is divided into four quadrants, A, B, C, and D, the outer contour circumferences of the heat removal pipes in each quadrant are substantially the same. Furthermore, a preferred example of a fluidized-bed reactor is a fluidized-bed reactor for producing acrylonitrile. Regarding the structure and operation of a fluidized-bed reactor, particularly a fluidized-bed reactor for producing acrylonitrile, relevant technical information known to those skilled in the art can be directly applied, and a detailed description thereof will be omitted herein.

[0084] According to one embodiment of the present invention, a fluidized-bed reactor may be provided with a heat removal water pipe having a conventionally known structure in addition to a heat removal water pipe having the characteristic structure of the present invention. Preferably, the number of heat removal water pipes having the characteristic structure of the present invention, calculated based on the straight pipe section, is, for example, 1 to 100%, 5 to 80%, or 10 to 40% of the total number of all heat removal water pipes. Preferably, the heat removal water pipes are uniformly distributed within the fluidized-bed reactor. For example, if the fluidized-bed reactor is divided into quadrants, A, B, C, and D, the outer contour circumference of the heat removal water pipes in each quadrant is substantially the same.

[0085] One embodiment of the present invention also relates to the use of a fluidized bed reactor according to any one of the above aspects of the invention in the production of epoxy compounds or unsaturated nitriles by an olefin oxidation process or an ammoxidation process, wherein the olefin may particularly include propylene, the epoxide may particularly include propylene oxide, and the unsaturated nitrile may particularly include acrylonitrile.

[0086] One embodiment of the present invention particularly relates to a process for producing acrylonitrile, comprising the step of ammoxidizing propylene to produce acrylonitrile in a fluidized bed reactor according to any one of the above aspects of the present invention.

[0087] According to one embodiment of the present invention, the olefin oxidation or ammoxidation process can be carried out by any method and by any method known to those skilled in the art. Such information is known to those skilled in the art, and a detailed description thereof is omitted herein. However, specific examples of conditions for the ammoxidation reaction include a molar ratio of propylene to ammonia to air (calculated based on oxygen molecules) of typically 1:1.1 to 1.3:1.8 to 2.0, a reaction temperature of typically 420 to 440°C, a reaction pressure (gauge pressure) of typically 0.03 to 0.14 MPa, and a weight hourly space velocity of typically 0.04 to 0.10 h -1 Includes:

[0088] [Example] The present invention will be described in more detail below using examples and comparative examples, but the present invention is not limited to the following examples.

[0089] In the following examples and comparative examples, the yield of acrylonitrile and the conversion rate of propylene can be calculated according to the following formulas: Acrylonitrile yield: AN%=C AN / ΣC * 100 Propylene conversion: Cc3% = (1-C C3in / C C3out ) * 100 where: C AN : Molar amount of carbon contained in AN gas at the reactor outlet (mol) ΣC: Total moles of carbon in the gas at the reactor outlet (mol) C C3out : Molar amount of carbon contained in C3 in the gas at the reactor outlet (mol) C C3in : Molar amount of carbon contained in C3 in the gas at the reactor inlet (mol) is.

[0090] In the following examples and comparative examples, the fluidization state of the fluidized bed can also be characterized by graphs or data of pressure pulsation intensity.

[0091] (Comparative Example 1) As shown in Figure 1, 3.8 tons of SANC series acrylonitrile catalyst (available from Shanghai Petrochemical Technology Institute SINOPEC) was loaded into a fluidized-bed reactor with a diameter of 1.5 m and a tangential height of 16 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 13 U-shaped heat removal pipes, each with a straight section outer diameter of 30 mm and a length of 10 m. The reactor also contained two sets of cyclone separators, each with two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 50 mm and 50 mm, respectively. The first stage dipleg length was 15.5 m, and the second stage dipleg length was 14.7 m.

[0092] The reaction cooling section of the fluidized bed reactor had a diameter of 1.5 m and a length L of 8.5 m. At the center of the reaction cooling section, L / S = 1.74 m -1 , L2 / S1=1.39m -1 , L3 / S1=0.36m -1 It was.

[0093] The operating conditions of the device are air flow rate of 3200NM. 3 / h, room temperature, and atmospheric pressure.

[0094] The pressure pulsation intensity data was measured at H0 of 2 m. The pressure pulsation intensity data is shown in Figure 6.

[0095] Comparative Example 2 As shown in Figure 1, 3.8 tons of SANC series acrylonitrile catalyst (available from Shanghai Petrochemical Technology Institute SINOPEC) was loaded into a fluidized-bed reactor with a diameter of 1.5 m and a tangential height of 16 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 39 U-shaped heat removal pipes, each with a straight section outer diameter of 30 mm and a length of 10 m. The reactor also contained two sets of cyclone separators, each with two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 50 mm and 50 mm, respectively. The first stage dipleg length was 15.5 m, and the second stage dipleg length was 14.7 m.

[0096] The reaction cooling section of the fluidized bed reactor had a diameter of 1.5 m and a length L of 8.5 m. At the center of the reaction cooling section, L / S = 4.52 m -1 , L2 / S1=4.16m -1 , L3 / S1=0.36m -1 It was.

[0097] The operating conditions of this device are air flow rate of 3200NM. 3 / h, room temperature, and atmospheric pressure.

[0098] The pressure pulsation intensity data was measured at an H of 2 m. The pressure pulsation intensity data is shown in Figure 7.

[0099] During operation of the device, the concentration of catalyst particles in the gas phase increased at the outlet of the device, indicating relatively severe catalyst attrition.

[0100] Example 1 As shown in Figure 1, 3.8 tons of SANC series acrylonitrile catalyst (available from Shanghai Petrochemical Technology Institute SINOPEC) was loaded into a fluidized-bed reactor with a diameter of 1.5 m and a tangential height of 16 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 30 U-shaped heat removal pipes, each with a straight tube outer diameter of 30 mm and a length of 10 m. The reactor also contained two sets of cyclone separators, each with two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 50 mm and 50 mm, respectively. The first stage dipleg length was 15.5 m, and the second stage dipleg length was 14.7 m.

[0101] The reaction cooling section of the fluidized bed reactor had a diameter of 1.5 m and a length L of 8.5 m. At the center of the reaction cooling section, L / S = 3.56 m -1 , L2 / S1=3.20m -1 , L3 / S1=0.36m -1 It was.

[0102] The operating conditions of this device are air flow rate of 3200NM. 3 / h, room temperature, and atmospheric pressure.

[0103] The pressure pulsation intensity data was measured at an H of 2 m. The pressure pulsation intensity data is shown in Figure 8.

[0104] Example 2 As shown in Figure 1, 3.8 tons of SANC series acrylonitrile catalyst (available from Shanghai Petrochemical Technology Institute SINOPEC) was loaded into a fluidized-bed reactor with a diameter of 1.5 m and a tangential height of 16 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 18 U-shaped heat removal pipes, each with a straight section outer diameter of 30 mm and a length of 10 m. The reactor also contained two sets of cyclone separators, each with two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 50 mm and 50 mm, respectively. The first stage dipleg length was 15.5 m, and the second stage dipleg length was 14.7 m.

[0105] The reaction cooling section of the fluidized bed reactor had a diameter of 1.5 m and a length L of 8.5 m. At the center of the reaction cooling section, L / S = 2.28 m -1 , L2 / S1=1.92m -1 , L3 / S1=0.36m -1 It was.

[0106] The operating conditions of this device are air flow rate of 3200NM. 3 / h, room temperature, and atmospheric pressure.

[0107] The pressure pulsation intensity data was measured at an H of 2 m. The pressure pulsation intensity data is shown in Figure 9.

[0108] Example 3 As shown in Figure 1, 3.8 tons of SANC series acrylonitrile catalyst available from Shanghai Petrochemical Technology Institute (SINOPEC) was loaded into a fluidized-bed reactor with a diameter of 1.5 m and a tangential height of 16 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 36 U-shaped heat removal pipes, each with a straight section outer diameter of 30 mm and a length of 10 m. The reactor also contained two sets of cyclone separators, each with two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 50 mm and 50 mm, respectively. The first stage dipleg length was 15.5 m, and the second stage dipleg length was 14.7 m.

[0109] The reaction cooling section of the fluidized bed reactor had a diameter of 1.5 m and a length L of 8.5 m. At the center of the reaction cooling section, L / S = 4.20 m. -1 , L2 / S1=3.84m -1 , L3 / S1=0.36m -1 It was.

[0110] The operating conditions of this device are air flow rate of 3200NM. 3 / h, room temperature, and atmospheric pressure.

[0111] The pressure pulsation intensity data was measured at an H of 2 m. The pressure pulsation intensity data is shown in Figure 10.

[0112] During operation of the device, the concentration of particulate catalyst in the gas phase at the outlet of the device was within an acceptable range.

[0113] Comparative Example 3 As shown in Figure 1, 160 tons of SANC series acrylonitrile catalyst, available from Shanghai Petrochemical Technology Institute (SINOPEC), was loaded into a fluidized-bed reactor with a diameter of 8 m and a tangential height of 18 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 100 U-shaped heat removal pipes, each with a straight tube outer diameter of 114 mm and a length of 8 m. The 100 U-shaped heat removal pipes were divided into 18 groups, each consisting of two U-shaped, five U-shaped, and six U-shaped pipes connected in series. The reactor also contained 18 cyclone separators, divided into nine sets, each consisting of two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 326 mm and 219 mm, respectively. The first stage dipleg length was 12.0 m, and the second stage dipleg length was 10.1 m.

[0114] The ratio of the number of cooling water pipes to the number of cyclone diplegs in the fluidized bed reactor was 11.11.

[0115] The reaction cooling section of the fluidized bed reactor had a diameter of 8 m and a length of L6.9 m. At the center of the reaction cooling section, L1 / S1 = 1.73 m -1 , L2 / S1=1.43m -1 , L3 / S1=0.31m -1 It was.

[0116] The pressure pulsation intensity data was measured at H0 of 2 m, and the graph of the pressure pulsation intensity data was similar to that of Comparative Example 1.

[0117] The operating conditions of the equipment were: propylene feed rate 5900NM 3 / h, reaction temperature 430°C, reaction pressure 0.055 MPa, and propylene:ammonia:air ratio 1:1.2:9.6.

[0118] Results from operation of the unit were an AN yield of 78.3% and a propylene conversion of 95.4%.

[0119] Example 4 As shown in Figure 4, 160 tons of SANC series acrylonitrile catalyst, available from Shanghai Petrochemical Technology Institute (SINOPEC), was loaded into a fluidized-bed reactor with a diameter of 8 m and a tangential height of 18 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 225 U-shaped heat removal pipes, each with a straight section outer diameter of 114 mm, a straight section length of 10 m, and a straight section spacing of 220 mm. The 225 U-shaped heat removal pipes were divided into 40 groups, each consisting of two U-shaped, five U-shaped, and six U-shaped pipes connected in series. The reactor also contained 20 cyclone separators, divided into 11 sets, each consisting of two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 326 mm and 219 mm, respectively, the length of the first stage dipleg was 12.0 m, and the length of the second stage dipleg was 10.1 m.

[0120] The ratio of the number of cooling water pipes to the number of cyclone diplegs in the fluidized bed reactor was 20.45.

[0121] The reaction cooling section of the fluidized bed reactor had a diameter of 8 m and a length of L7.4 m. At the center of the reaction cooling section, L1 / S1 = 3.58 m -1 , L2 / S1=3.21m -1 , L3 / S1=0.37m -1 It was.

[0122] The pressure pulsation intensity data was measured at an H of 2 m. The graph of the pressure pulsation intensity data was similar to that of Example 1.

[0123] The operating conditions of the equipment were: propylene feed rate 5900NM 3 / h, reaction temperature 430°C, reaction pressure 0.04 MPa, and propylene:ammonia:air ratio 1:1.2:9.6.

[0124] Results from operation of the unit were an AN yield of 80.5% and a propylene conversion of 98.5%.

[0125] Example 5 As shown in Figure 4, 160 tons of SANC series acrylonitrile catalyst, available from Shanghai Petrochemical Technology Institute (SINOPEC), was loaded into a fluidized-bed reactor with a diameter of 8 m and a tangential height of 18 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 110 U-shaped heat removal pipes, each with a straight section outer diameter of 114 mm, a straight section length of 10 m, and a straight section spacing of 220 mm. The 110 U-shaped heat removal pipes were divided into 20 groups, each consisting of two U-shaped, five U-shaped, and six U-shaped pipes connected in series. The reactor also contained 28 cyclone separators, divided into 14 sets, each consisting of two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 326 mm and 219 mm, respectively. The length of the first stage dipleg was 12.0 m, and the length of the second stage dipleg was 10.1 m.

[0126] The ratio of the number of cooling water pipes to the number of cyclone diplegs in the fluidized bed reactor was 7.85.

[0127] The reaction cooling section of the fluidized bed reactor had a diameter of 8 m and a length of L7.4 m. At the center of the reaction cooling section, L1 / S1 = 2.04 m -1 , L2 / S1=1.57m -1 , L3 / S1=0.48m -1 It was.

[0128] The pressure pulsation intensity data was measured at an H of 2 m. The graph of the pressure pulsation intensity data was similar to that of Example 2.

[0129] The operating conditions of the equipment were: propylene feed rate 5900NM 3 / h, reaction temperature 430°C, reaction pressure 0.04 MPa, and propylene:ammonia:air ratio 1:1.2:9.6.

[0130] Results from operation of the unit were an AN yield of 79.3% and a propylene conversion of 96.8%.

[0131] Example 6 As shown in Figure 4, 160 tons of SANC series acrylonitrile catalyst, available from Shanghai Petrochemical Technology Research Institute (SINOPEC), was loaded into a fluidized-bed reactor with a diameter of 8 m and a tangential height of 18 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 266 U-shaped heat removal pipes, each with a straight section outer diameter of 114 mm, a straight section length of 10 m, and a straight section spacing of 215 mm. The 266 U-shaped heat removal pipes were divided into 48 groups, each consisting of two U-shaped, five U-shaped, and six U-shaped pipes connected in series. The reactor contained 18 cyclone separators, divided into nine sets, each consisting of two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 326 mm and 219 mm, respectively. The length of the first stage dipleg was 12.0 m, and the length of the second stage dipleg was 10.1 m.

[0132] The ratio of the number of cooling water pipes to the number of cyclone diplegs in the fluidized bed reactor was 29.55.

[0133] The reaction cooling section of the fluidized bed reactor had a diameter of 8 m and a length of L7.4 m. At the center of the reaction cooling section, L1 / S1 = 4.10 m -1 , L2 / S1=3.79m -1 , L3 / S1=0.31m -1 It was.

[0134] The pressure pulsation intensity data was measured at an H0 of 2 m, and the graph of the pressure pulsation intensity data was similar to that of Example 3.

[0135] The operating conditions of the equipment were: propylene feed rate 5900NM 3 / h, reaction temperature 430°C, reaction pressure 0.04 MPa, and propylene:ammonia:air ratio 1:1.2:9.6.

[0136] Results from operation of the unit were an AN yield of 80.5% and a propylene conversion of 98.6%.

[0137] Example 7 One hundred and sixty tons of SANC series acrylonitrile catalyst, available from Shanghai Petrochemical Technology Institute (SINOPEC), was loaded into the fluidized-bed reactor shown in Figure 4, with a diameter of 8 m and a tangential height of 18 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 225 U-shaped heat removal pipes, each with a straight section outer diameter of 114 mm, a straight section length of 10 m, and a straight section spacing of 220 mm. The 225 U-shaped heat removal pipes were divided into 40 groups, each consisting of two U-shaped, five U-shaped, and six U-shaped pipes connected in series. The reactor also contained 12 cyclone separators, divided into four sets, each consisting of three stages of cyclone separators connected in series. The outer diameters of the first, second, and third stages were 326 mm, 219 mm, and 219 mm, respectively. The first stage dipleg length was 12.0 m, and the second and third stage dipleg lengths were 10.1 m.

[0138] The reaction cooling section of the fluidized bed reactor had a diameter of 8 m and a length of L7.4 m. The central part of the reaction cooling section was L1 / S1 = 3.40 m. -1 , L2 / S1=3.21m -1 , L3 / S1=0.19m -1 is.

[0139] The pressure pulsation intensity data was measured at an H0 of 2 m, and the graph of the pressure pulsation intensity data was similar to that of Example 1.

[0140] The operating conditions of the equipment were: propylene feed rate 5900NM 3 / h, reaction temperature 430°C, reaction pressure 0.04 MPa, and propylene:ammonia:air ratio 1:1.2:9.6.

[0141] Results from operation of the unit were as follows: 79.5% AN yield, and 97.6% propylene conversion.

[0142] Example 8 As shown in Figure 4, 160 tons of SANC series acrylonitrile catalyst, available from Shanghai Petrochemical Technology Research Institute (SINOPEC), was loaded into a fluidized-bed reactor with a diameter of 8 m and a tangential height of 18 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 225 U-shaped heat removal pipes, each with a straight section outer diameter of 114 mm, a straight section length of 10 m, and a straight section spacing of 220 mm. The 225 U-shaped heat removal pipes were divided into 40 groups, each consisting of two U-shaped, five U-shaped, and six U-shaped pipes connected in series. The reactor contained 24 cyclone separators, divided into eight sets, each consisting of three stages of cyclone separators connected in series. The outer diameters of the first, second, and third stages were 326 mm, 219 mm, and 219 mm, respectively. The first stage dipleg length was 12.0 m, and the second and third stage dipleg lengths were 10.1 m.

[0143] The reaction cooling section of the fluidized bed reactor had a diameter of 8 m and a length of L7.4 m. The central part of the reaction cooling section was L1 / S1 = 3.23 m. -1 , L2 / S1=2.85m -1 , L3 / S1=0.38m -1 is.

[0144] The pressure pulsation intensity data was measured at an H0 of 2 m, and the graph of the pressure pulsation intensity data was similar to that of Example 1.

[0145] The operating conditions of the equipment were: propylene feed rate 5900NM 3 / h, reaction temperature 430°C, reaction pressure 0.04 MPa, and propylene:ammonia:air ratio 1:1.2:9.6.

[0146] Results from operation of the unit were an AN yield of 80.2% and a propylene conversion of 98.1%.

[0147] Example 9 As shown in Figure 4, 160 tons of SANC series acrylonitrile catalyst available from Shanghai Petrochemical Technology Institute (SINOPEC) was loaded into a fluidized-bed reactor with a diameter of 8 m and a tangential height of 18 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 140 U-shaped heat removal pipes, each with a straight section outer diameter of 114 mm and a straight section length of 8 m. The 140 U-shaped heat removal pipes were divided into 26 groups, each consisting of two U-shaped, five U-shaped, and six U-shaped pipes connected in series. The reactor contained 18 cyclone separators, divided into nine sets, each consisting of two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 326 mm and 219 mm, respectively. The first stage dipleg length was 12.0 metres, and the second stage dipleg length was 10.1 metres.

[0148] The reaction cooling section of the fluidized bed reactor had a diameter of 8 m and a length of L7.2 m. The central part of the reaction cooling section was L1 / S1 = 2.28 m. -1 , L2 / S1=2.00m -1 , L3 / S1=0.29m -1 is.

[0149] The pressure pulsation intensity data was measured at an H0 of 2 m, and the graph of the pressure pulsation intensity data was similar to that of Example 2.

[0150] The operating conditions of the equipment were: propylene feed rate 5900NM 3 / h, reaction temperature 430°C, reaction pressure 0.04 MPa, and propylene:ammonia:air ratio 1:1.2:9.6.

[0151] Results from operation of the unit were an AN yield of 79.6% and a propylene conversion of 97.3%.

[0152] Example 10 As shown in Figure 4, 160 tons of SANC series acrylonitrile catalyst available from Shanghai Petrochemical Technology Institute (SINOPEC) was loaded into a fluidized-bed reactor with a diameter of 8 m and a tangential height of 18 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 190 U-shaped heat removal pipes, each with a straight section outer diameter of 114 mm and a straight section length (Lz) of 8 m. The 190 U-shaped heat removal pipes were divided into 34 groups, each consisting of two U-shaped pipes, five U-shaped pipes, and six U-shaped pipes connected in series. Additionally, 95 of the U-shaped pipes had fins on the outer wall of the straight pipe section, as shown in Figure 5f. Four fins were uniformly distributed on the outer wall of the straight pipe section. The fin length (Lt) was 3000 mm, height 10 mm, and width 20 mm. The reactor contained 22 cyclone separators, divided into 11 sets, each set containing two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 326 mm and 219 mm, respectively. The length of the first stage dipleg was 12.0 m, and the length of the second stage dipleg was 10.1 m.

[0153] The reaction cooling section of the fluidized bed reactor had a diameter of 8 m and a length of L7.4 m. The central part of the reaction cooling section was L1 / S1 = 3.12 m. -1 , L2 / S1=2.75m -1 , L3 / S1=0.37m -1 is.

[0154] The pressure pulsation intensity data was measured at an H0 of 2 m, and the graph of the pressure pulsation intensity data was similar to that of Example 1.

[0155] The operating conditions of the equipment were: propylene feed rate 5900NM 3 / h, reaction temperature 430°C, reaction pressure 0.04 MPa, and propylene:ammonia:air ratio 1:1.2:9.6.

[0156] Results from operation of the unit were an AN yield of 80.7% and a propylene conversion of 98.8%.

[0157] Example 11 As shown in Figure 4, 160 tons of SANC series acrylonitrile catalyst, available from Shanghai Petrochemical Technology Institute (SINOPEC), was loaded into a fluidized-bed reactor with a diameter of 8 m and a tangential height of 18 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 190 U-shaped heat removal pipes, each with a straight section outer diameter of 114 mm and a straight section length (Lz) of 8 m. The 190 U-shaped heat removal pipes were divided into 34 groups, each consisting of two U-shaped, five U-shaped, and six U-shaped pipes connected in series. Additionally, 95 of the U-shaped pipes had fins on the outside of their straight sections, as shown in Figure 5a. Eight fins were arranged on the outside of the straight section, with a vertical spacing of 500 mm between the fins and an angle α1 of 50°. The fins had a length (Lt) of 3,500 mm, a height of 10 mm, and a width of 20 mm. The fluidized-bed reactor was equipped with 20 cyclone separators, divided into 10 sets, each set containing two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 326 mm and 219 mm, respectively. The length of the first stage dipleg was 12.0 m, and the length of the second stage dipleg was 10.1 m.

[0158] The reaction cooling section of the fluidized bed reactor had a diameter of 8 m and a length of L7.4 m. The central part of the reaction cooling section was L1 / S1 = 3.15 m. -1 , L2 / S1=2.78m -1 , L3 / S1=0.37m -1 is.

[0159] The pressure pulsation intensity data was measured at an H0 of 2 m, and the graph of the pressure pulsation intensity data was similar to that of Example 1.

[0160] The operating conditions of the equipment were: propylene feed rate 5900NM 3 / h, reaction temperature 430°C, reaction pressure 0.04 MPa, and propylene:ammonia:air ratio 1:1.2:9.6.

[0161] Results from operation of the unit were an AN yield of 80.6% and a propylene conversion of 98.7%.

[0162] Example 12 As shown in Figure 4, 160 tons of SANC series acrylonitrile catalyst, available from Shanghai Petrochemical Technology Institute (SINOPEC), was loaded into a fluidized-bed reactor with a diameter of 8 m and a tangential height of 18 m (i.e., the total height of the dense and dilute phase regions shown in the figure). The reactor contained 225 U-shaped heat removal pipes, each with a straight section outer diameter of 114 mm and a length of 8 m. The 225 U-shaped heat removal pipes were divided into 40 groups, each consisting of two U-shaped, five U-shaped, and six U-shaped pipes connected in series. The reactor contained 42 cyclone separators, divided into 21 sets, each consisting of two stages of cyclone separators connected in series. The outer diameters of the first and second stage diplegs were 400 mm and 325 mm, respectively. The first stage dipleg length was 12.0 metres, and the second stage dipleg length was 10.1 metres.

[0163] The reaction cooling section of the fluidized bed reactor had a diameter of 8 m and a length of L7.2 m. The central part of the reaction cooling section was L1 / S1 = 4.16 m. -1 , L2 / S1=3.21m -1 , L3 / S1=0.95m -1 is.

[0164] The pressure pulsation intensity data was measured at an H0 of 2 m, and the graph of the pressure pulsation intensity data was similar to that of Example 1.

[0165] The operating conditions of the equipment were: propylene feed rate 5900NM 3 / h, reaction temperature 430°C, reaction pressure 0.04 MPa, and propylene:ammonia:air ratio 1:1.2:9.6.

[0166] Results from operation of the unit were an AN yield of 80.1% and a propylene conversion of 98.7%. [Brief explanation of the drawings]

[0167] [Figure 1] FIG. 1 is a schematic front view of a prior art fluidized bed reactor. [Figure 2] 1 is a schematic cross-sectional view of a prior art fluidized bed reactor cooling section. FIG. [Figure 3] 1 is a schematic cross-sectional view of a reaction cooling section of a fluidized bed according to the present invention. [Figure 4] 1 is a schematic front view of a fluidized bed reactor of the present invention. [Figure 5] 1 is a schematic diagram of an exemplary embodiment of a heat rejection water pipe of the present invention. FIG. [Figure 6] 10 shows a graph of pressure pulsation intensity in Comparative Example 1. [Figure 7] 10 shows a graph of pressure pulsation intensity in Comparative Example 2. [Figure 8] 1 shows a graph of pressure pulsation intensity in Example 1. [Figure 9] 10 shows a graph of pressure pulsation intensity in Example 2. [Figure 10] 10 shows a graph of pressure pulsation intensity in Example 3.

Claims

1. A fluidized bed reactor comprising at least a reaction cooling section and a vertical internal structure disposed in the reaction cooling section, wherein the total length of the reaction cooling section in a direction along the central axis of the fluidized bed reactor is defined as L (expressed in units of m), and the cross-sectional area of ​​the reaction cooling section in a cross section perpendicular to the central axis of the fluidized bed reactor is defined as S1 (expressed in units of m) at any position within a region from 45% L above the center point of the reaction cooling section to 38% L below the center point. 2 The perimeter of the cross section of the vertical internal structure (if there are multiple cross sections, the total perimeter of all cross sections) is defined as L1 (expressed in meters), and L1 / S1 = 2.0 to 4.3 m -1 and The vertical internal structure is a combination of a heat removal water pipe and a gas-solid separator, The outer periphery of the cross section of the heat removal pipe (calculated based on the cross section of the straight pipe portion of the pipe) (if there are multiple cross sections, the total of the outer peripheries of all cross sections) is defined as L2 (expressed in m), and L2 / S1 = 1.7 to 3.6 m -1 ; The fluidized bed reactor, wherein the perimeter of the cross section of the gas-solid separator (calculated based on the dipleg) (if there are multiple cross sections, this refers to the sum of the perimeters of all the cross sections) is defined as L3 (expressed in m), and L3 / S1 = 0.25 to 0.85 m -1 .

2. L1 / S1=2.2~4.1m -1 and L2 / S1 = 1.9 to 3.5 m -1 and the gas-solid separator is a cyclone separator, and / or L3 / S1=0.30 to 0.75 m. -1 2. The fluidized bed reactor of claim 1, wherein

3. 2. The fluidized bed reactor according to claim 1, wherein the number of heat removal water pipes (calculated based on the straight pipe sections of the pipes) is 220 to 5000, and / or the number of gas-solid separators (calculated based on diplegs) is 16 to 516, and / or the ratio of the number of straight pipe sections to the number of diplegs is 8.5 to 24.

0.

4. 4. The fluidized bed reactor according to claim 3, wherein the number of the heat removal water pipes (calculated based on the straight pipe sections of the pipes) is 300 to 2400, the number of the gas-solid separators (calculated based on the diplegs) is 16 to 210, and / or the ratio of the number of the straight pipe sections to the number of diplegs is 11.5 to 21.

0.

5. and / or the straight pipe sections have the same or different outer diameters, independently of one another, of 80 to 180 mm; and / or the straight pipe sections have the same or different inner diameters, independently of one another, of 60 to 150 mm; and / or the straight pipe sections have the same or different lengths, independently of one another, of 4.0 to 13 m; and / or the diplegs have the same or different outer diameters, independently of one another, of 150 to 410 mm; and / or the diplegs have the same or different inner diameters, independently of one another, of 130 to 400 mm; and / or the diplegs have the same or different lengths, independently of one another, of 6 to 14 m; and / or the reaction cooling section has a diameter of 5 to 29 m, a length of 19.6 to 660 m. 2 and / or a length L of 4 to 12.5 m.

6. The straight pipe sections have an outer diameter of 90 to 170 mm, and / or the straight pipe sections have an inner diameter of 70 to 140 mm, and / or the straight pipe sections have a length of 5.5 to 12.0 m, and / or the diplegs have an outer diameter of 200 to 360 mm, and / or the diplegs have an inner diameter of 180 to 350 mm, and / or the diplegs have a length of 10 to 13 m, and / or the reaction cooling section has a diameter of 7 to 20 m, a length of 38.5 to 314 m. 2 and / or a length L of 5.5 to 11.5 m.

7. 2. The fluidized bed reactor of claim 1, comprising, in this order from top to bottom, a head, a dilute phase zone, the reaction cooling section, a pre-reaction section, and a cone, and further comprising a gas distribution plate and, optionally, a fluid distributor provided in the pre-reaction section.

8. 2. The fluidized bed reactor according to claim 1, wherein the reaction cooling section has a substantially circular cross section, and / or the cross section of the vertical internal configuration has a substantially circular inner contour and a substantially circular outer contour, and / or the cross section of the vertical internal configuration has a substantially circular inner contour and a substantially circular outer contour with a protrusion, and / or the vertical internal configuration includes a heat removal water pipe, the heat removal water pipe having a heat removal medium inlet, n straight pipe sections, and a heat removal medium outlet, a tip of a first straight pipe section communicates with the heat removal medium inlet, a tail end of the nth straight pipe section communicates with the heat removal medium outlet, and a rear end of the i-th straight pipe section communicates with a head end of the (i+1)th straight pipe section via a U-shaped pipe, n is an integer from 2 to 100, i is an integer from 1 to n-1, and protrusions are provided on outer walls of some or all of the straight pipe sections.

9. 9. The fluidized bed reactor according to claim 8, wherein the straight pipe section is a straight circular pipe, n is an integer of 2 to 20, and / or the protrusion is present on 10 to 40% of the outer wall of the straight pipe section.

10. 9. The fluidized bed reactor according to claim 8, wherein the center lines of any two adjacent straight pipe sections are parallel to each other, and the distances between the center lines of any two adjacent straight pipe sections are the same as each other or different from each other and are independently 160 to 540 mm.

11. 11. The fluidized bed reactor according to claim 10, wherein the distances between the center lines of any two adjacent straight pipe sections are the same and independently range from 180 to 430 mm.

12. 9. The fluidized bed reactor according to claim 8, wherein the protrusions extend continuously or discontinuously in a direction along a center line of the straight pipe section and / or the protrusions extend continuously or discontinuously around a center line of the straight pipe section.

13. 13. The fluidized bed reactor of claim 12, wherein the protrusion extends continuously or discontinuously around the centerline of the straight pipe section in the form of a ring or a spiral.

14. 13. The fluidized bed reactor according to claim 12, wherein, when the protrusion extends continuously or discontinuously in a direction along the center line of the straight pipe section, the extension length Lt of the protrusion is not longer than the length Lz of the straight pipe section; and / or, when the protrusion extends continuously or discontinuously around the center line of the straight pipe section in the form of a ring, the height Hh of the ring is not longer than the length Lz of the straight pipe section; or, when the protrusion extends continuously or discontinuously around the center line of the straight pipe section in the form of a spiral, the height Ht of the spiral is not longer than the length Lz of the straight pipe section; and / or, the height of the protrusion is 0.005 to 0.3 times the outer diameter of the straight pipe section; and / or the width of the protrusion is 0.005 to 0.3 times the outer diameter of the straight pipe section.

15. 15. The fluidized bed reactor according to claim 14, wherein Lt / Lz is 0.1 to 0.6, Hh / Lz is 0.01 to 0.3, Ht / Lz is 0.2 to 0.6, and / or the height of the protrusion is 0.008 to 0.1 times the outer diameter of the straight pipe portion, and / or the width of the protrusion is 0.008 to 0.2 times the outer diameter of the straight pipe portion.

16. 9. The fluidized bed reactor according to claim 8, wherein the protrusion extends continuously or discontinuously around the center line of the straight pipe section, and an angle between the center line of the protrusion and the center line of the straight pipe section is greater than 0° and less than or equal to 90°.

17. 17. The fluidized bed reactor according to claim 16, wherein an angle between a center line of the protrusion and a center line of the straight pipe section is 10° or more and 60° or less.

18. 10. Use of the fluidized bed reactor according to claim 1 in the production of epoxy compounds or unsaturated nitriles by an olefin oxidation process or an ammoxidation process.

19. 19. The use according to claim 18, wherein the epoxy compound is propylene oxide, and / or the unsaturated nitrile is acrylonitrile, and / or the olefin is propylene.

20. 10. A method for producing an unsaturated nitrile, comprising the step of subjecting an olefin to an ammoxidation reaction in the fluidized bed reactor of claim 1 to produce the unsaturated nitrile.

21. 21. The process of claim 20, wherein the olefin is propylene and / or the unsaturated nitrile is acrylonitrile.

22. L1 / S1=2.4~3.9m -1 and L2 / S1 = 2.1 to 3.3 m -1 and / or L3 / S1=0.35 to 0.65 m -1 2. The fluidized bed reactor of claim 1, wherein

Citation Information

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