CN111298727B - Fluidized bed reaction device and fluidized reaction method for nitrobenzene hydrogenation - Google Patents
Fluidized bed reaction device and fluidized reaction method for nitrobenzene hydrogenation Download PDFInfo
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
- B01J8/26—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with two or more fluidised beds, e.g. reactor and regeneration installations
- B01J8/28—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique with two or more fluidised beds, e.g. reactor and regeneration installations the one above the other
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- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/30—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds
- C07C209/32—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups
- C07C209/36—Preparation of compounds containing amino groups bound to a carbon skeleton by reduction of nitrogen-to-oxygen or nitrogen-to-nitrogen bonds by reduction of nitro groups by reduction of nitro groups bound to carbon atoms of six-membered aromatic rings in presence of hydrogen-containing gases and a catalyst
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Abstract
The invention relates to a fluidized bed reaction device and a fluidized reaction method for nitrobenzene hydrogenation, which mainly solve the problems of low gas-solid contact efficiency, large bubble size, low fluidized quality and the like in a fluidized bed. The invention sets at least one group of composite components in the fluidized bed reactor, so that gas and catalyst particles can break bubbles and particle groups when passing through the components, thereby effectively improving the fluidization quality.
Description
Technical Field
The invention belongs to the technical field of chemical equipment and organic chemical industry, and relates to a fluidized bed reaction device and a fluidized reaction method for nitrobenzene hydrogenation.
Background
Aniline is an important basic organic chemical raw material and a fine chemical intermediate, and downstream products produced by aniline can be more than 300, so that the aniline is widely applied to industries such as dyes, medicines, pesticides, explosives, spices, rubber, synthetic materials and the like. In recent years, with the rapid rise of polyurethane industry in China and worldwide, aniline, which is one of the basic raw materials irreplaceable to MDI (4, 4-diphenylmethane diisocyanate), which is the main raw material, has been remarkably and rapidly developed.
At present, three methods for industrially producing aniline are available, namely a nitrobenzene catalytic hydrogenation method, a phenol ammoniation method and an iron powder reduction method. Wherein, the iron powder reduction method is gradually eliminated due to the poor quality of the generated aniline. The phenol amination process is strongly dependent on the source of the phenol. The prior nitrobenzene catalytic hydrogenation method is adopted by most manufacturers. The nitrobenzene catalytic hydrogenation method is divided into a gas-phase catalytic hydrogenation process and a liquid-phase catalytic hydrogenation process. The nitrobenzene liquid-phase catalytic hydrogenation process is first developed successfully by DuPont company in America, mainly adopts a noble metal catalyst to carry out under the anhydrous condition, and has the advantages of low reaction temperature, high catalyst load, long service life and large equipment production capacity, and has the defects of high required pressure, necessary separation of reactants, the catalyst and a solvent, high equipment operation cost, high catalyst price and more byproducts caused by overhigh catalyst activity. The fluidized bed gas phase catalytic hydrogenation method is that the nitrobenzene as raw material is heated and vaporized and mixed with hydrogen, and then enters a fluidized bed reactor filled with a copper-silica gel catalyst to carry out hydrogenation reduction reaction.
The method for preparing aniline by gas phase hydrogenation of nitrobenzene has been in production history for decades in China, and fluidized bed gas phase catalytic hydrogenation process is adopted by many aniline manufacturers in China.
Document CN1528737A discloses a device and a method for preparing aniline by gas phase hydrogenation of nitrobenzene. The device comprises a fluidized bed reactor, a reaction raw material gas inlet arranged at the bottom of the reactor, a first gas distributor arranged at the upper part of the inlet, a second gas distributor which is arranged at the middle part of the axial height of the reactor and divides the reactor into two catalyst dense-phase areas, and a catalyst overflow device which is arranged outside or inside the reactor and is respectively connected with the upper catalyst dense-phase area and the lower catalyst dense-phase area.
Document CN1634860A discloses a gas distributor in fluidized bed for aniline synthesis and a method for synthesizing aniline. The gas distributor consists of a main pipe for conveying gas, branch pipes, an annular pipeline connected with the main pipe and the branch pipes for distributing gas, and a nozzle for spraying gas downwards and a nozzle for spraying gas upwards, which are arranged on the annular pipeline.
In the fluidized bed reactor for preparing aniline in the prior art, the aniline catalyst particles belong to Geldart B type particles due to large particle size and are not easy to fluidize. The fluidization quality of the bed layer in the reactor is generally adjusted by adding the internals, but the flow guiding principle of different internals is different, and the influence on the fluidization quality is different. The invention provides a composite member in a targeted manner, and effectively solves the problem.
Disclosure of Invention
One of the main technical problems to be solved by the invention is that the gas-solid contact efficiency in the fluidized bed is low, the size of the bubbles is large, the fluidization quality is low and the like in the prior art, and the invention provides an improved fluidized bed reaction device.
The second technical problem to be solved by the present invention is to provide a vulcanization reaction method corresponding to the first technical problem.
In order to solve one of the above technical problems, the technical scheme adopted by the invention is as follows: the fluidized bed reaction device comprises a fluidized bed reactor (3) and is characterized in that a composite component (2) and a heat removal water pipe (4) are arranged in the fluidized bed reactor (3), and the composite component (2) is formed by combining a left baffle (23) and a right baffle (24); the left baffle plate (23) and the right baffle plate (24) are respectively composed of triangular prisms with triangular longitudinal sections.
Further, in the above technical solution, the largest angle α in the triangular longitudinal sections of the left baffle 23 and the right baffle 24 is 90-145 °.
Further, in the above technical solution, the side faces of the prism where the longer side of the triangular longitudinal section of the left baffle 23 and the right baffle 24 of the composite member 2 is located are parallel to each other and are vertically placed.
Further, in the above technical solution, the side surfaces of the left baffle 23 and the right baffle 24 of the composite member 2 are respectively provided with holes and/or slits, and the aperture ratio of the total area of the holes and/or slits to the area of the blade is 5% to 45%.
Further, in the above technical scheme, at least 1 composite member 2 is arranged in the fluidized bed reactor 3, the composite members 2 are uniformly distributed in the reactor in a staggered manner, and acute/right-angle angles of pairwise intersections between adjacent composite members 2 in the vertical direction are 30-90 degrees, and the vertical distance between adjacent composite members 2 in the vertical direction is not less than 80 mm.
Further, in the above technical solution, the composite members 2 are parallel to each other on the same cross section, and the distance between the composite members 2 adjacent to each other in the horizontal direction is not less than 100 mm.
In order to solve the second problem, the invention adopts the following technical scheme: a fluidized bed reaction method for nitrobenzene hydrogenation adopts the fluidized reaction device, and comprises the following steps:
the vaporized nitrobenzene and hydrogen raw materials enter a fluidized bed reactor 3, after the catalyst in the reactor is pushed to fluidize, the catalyst and gas composite member 2 is formed, bubbles are extruded and crushed by the composite member 2, partial gas and particles are sprayed out from a left baffle 23 and a right baffle 24, the rest gas and particles are crushed and escaped from openings and/or seams on the side surfaces of the left baffle 23 and the right baffle 24, catalyst particle clusters and transverse large bubbles are crushed, and nitrobenzene, hydrogen and catalytic particles efficiently contact, mix and react in the space to produce an aniline product.
Further, in the technical scheme, the catalyst is a metal-loaded catalyst, copper is used as a main active component, a carrier is silicon dioxide, and the average particle size of the catalyst is 50-600μm is less than 80μThe content of particles below m is not less than 2%.
Further, in the above technical solution, the linear speed of the gas passing through the space between the left baffle 23 and the right baffle 24 of the composite member 2 is 0.5-6 m/s.
Further, in the above technical scheme, the reaction conditions in the fluidized bed reactor 3 are as follows: the superficial gas velocity is 0.1 to 0.9m/s, and the mass ratio of hydrogen to nitrobenzene is 6 to 21:1, controlling the average reaction temperature in the reaction zone to be 220-285 ℃, and controlling the reaction pressure in the reaction zone to be 0.05-1 MPa.
In the technical scheme of the invention, as the composite component is adopted, the fluidization quality of the bed layer can be improved through the flow guiding effect of the baffle and the crushing effect of the holes/seams distributed in the baffle, the bubbles in the bed are reduced, the retention amount of the emulsified phase is increased, and the expansion ratio is effectively improved; the bed pressure pulsation of the average bubble diameter in the standard fluidized bed is also greatly reduced.
By adopting the technical scheme of the invention, the fluidized bed reaction device and the reaction method for nitrobenzene hydrogenation are applied to the preparation of aniline by nitrobenzene hydrogenation, so that a better gas-solid contact effect can be obtained, the growth of large bubbles is inhibited, meanwhile, an air cushion generated below a common flow guide inner component is overcome, compared with the prior art, the fluidization quality in the fluidized bed is obviously improved, and a better technical effect is obtained.
Drawings
FIG. 1 is a schematic structural diagram of a fluidized bed reactor for hydrogenation of nitrobenzene in accordance with an embodiment of the present invention.
In FIG. 1, 1 is the vaporized nitrobenzene and hydrogen feed; 2 is a composite member; 3 is a fluidized bed reactor; 4 is a heat removal water pipe.
Fig. 2 is a perspective view of the composite structural member of fig. 1.
In fig. 2, 21 is an upper hole, 22 is a lower hole, 23 is a left baffle, and 24 is a right baffle.
Detailed Description
The present invention will be further illustrated by the following examples, but is not limited to these examples.
[ example 1 ]
The device for preparing aniline by nitrobenzene hydrogenation is shown in figure 1. The average particle diameter of the catalyst is 360μm, and the largest angle alpha in the triangular longitudinal sections of the left baffle and the right baffle is 135 degrees. The side faces of the prism where the longer side of the triangular longitudinal section of the left baffle and the right baffle of the composite member is located are parallel to each other and are vertically arranged. The side surfaces of the left baffle and the right baffle of the composite member are respectively provided with holes and/or slits, and the ratio of the total area of the holes and/or slits to the area of the blade has the aperture ratio of 15%. 4 composite components are arranged in the fluidized bed reactor, are uniformly distributed in the reactor in a staggered manner and are verticalThe acute/right angle at which two-by-two crossing between the composite members adjacent in the direction is 90 °, and the perpendicular distance between the composite members adjacent in the vertical direction is 100 mm. The composite components are parallel to each other on the same section, and the distance between the composite components adjacent to each other in the horizontal direction is 100 mm.
Standard deviation analysis is a common method of analysis of the pressure pulsation characteristics of a fluidized bed. The present embodiment uses the standard deviation to characterize the strength of the pressure pulsation. Will be the transient pressure at any moment
Decomposition to mean value
And the fluctuation value
The sum, i.e.,
standard deviation of pressure at any one measurement point
And N is the number of the sampling data.SdCan be used to characterize the strength of the pressure pulsations. The greater the intensity of the pressure pulsation, the greater the mean bubble in the bed and the poorer the fluidization quality. The expansion coefficient is another technical index for evaluating the fluidization quality, and the higher the expansion coefficient is, the better the fluidization quality is.
The standard deviation of the dense phase zone in the fluidized bed was 825 Pa and the expansion coefficient was 1.40, with the results detailed in Table 1.
[ example 2 ]
The device for preparing aniline by nitrobenzene hydrogenation is shown in figure 1. The average particle diameter of the catalyst is 360μm, and the largest angle alpha in the triangular longitudinal sections of the left baffle and the right baffle is 145 degrees. The side faces of the prism where the longer side of the triangular longitudinal section of the left baffle and the right baffle of the composite member is located are parallel to each other and are vertically arranged. The side surfaces of the left baffle and the right baffle of the composite member are respectively provided with holes and/or seams, and the holes are providedAnd (or) the ratio of the total area of the slots to the area of the blade is 15%. 4 composite components are arranged in the fluidized bed reactor, the composite components are uniformly distributed in the reactor in a staggered mode, the acute/right-angle of pairwise intersection between every two adjacent composite components in the vertical direction is 90 degrees, and the vertical distance between every two adjacent composite components in the vertical direction is 100 mm. The composite components are parallel to each other on the same section, and the distance between the composite components adjacent to each other in the horizontal direction is 100 mm. The dense phase zone within the fluidized bed had a standard deviation of 876 Pa and an expansion coefficient of 1.38, the results are detailed in Table 1.
[ example 3 ]
The device for preparing aniline by nitrobenzene hydrogenation is shown in figure 1. The average particle diameter of the catalyst is 360μm, the largest angle alpha in the triangular longitudinal sections of the left baffle and the right baffle is 90 degrees. The side faces of the prism where the longer side of the triangular longitudinal section of the left baffle and the right baffle of the composite member is located are parallel to each other and are vertically arranged. The side surfaces of the left baffle and the right baffle of the composite member are respectively provided with holes and/or slits, and the ratio of the total area of the holes and/or slits to the area of the blade has the aperture ratio of 15%. 4 composite components are arranged in the fluidized bed reactor, the composite components are uniformly distributed in the reactor in a staggered mode, the acute/right-angle of pairwise intersection between every two adjacent composite components in the vertical direction is 90 degrees, and the vertical distance between every two adjacent composite components in the vertical direction is 100 mm. The composite components are parallel to each other on the same section, and the distance between the composite components adjacent to each other in the horizontal direction is 100 mm. The standard deviation of the dense phase zone in the fluidized bed was 1112 Pa and the expansion coefficient was 1.35, and the results are detailed in Table 1.
[ example 4 ]
The device for preparing aniline by nitrobenzene hydrogenation is shown in figure 1. The average particle diameter of the catalyst is 360μm, and the largest angle alpha in the triangular longitudinal sections of the left baffle and the right baffle is 135 degrees. The side faces of the prism where the longer side of the triangular longitudinal section of the left baffle and the right baffle of the composite member is located are parallel to each other and are vertically arranged. The side surfaces of the left baffle and the right baffle of the composite component are respectively provided with holes and/or slits, and the ratio of the total area of the holes and/or slits to the area of the blade has the aperture ratio of5 percent. 4 composite components are arranged in the fluidized bed reactor, the composite components are uniformly distributed in the reactor in a staggered mode, the acute/right-angle of pairwise intersection between every two adjacent composite components in the vertical direction is 90 degrees, and the vertical distance between every two adjacent composite components in the vertical direction is 100 mm. The composite components are parallel to each other on the same section, and the distance between the composite components adjacent to each other in the horizontal direction is 100 mm. The standard deviation of the dense phase zone in the fluidized bed was 1070 Pa and the expansion coefficient was 1.30, the results are detailed in table 1.
[ example 5 ]
The device for preparing aniline by nitrobenzene hydrogenation is shown in figure 1. The average particle diameter of the catalyst is 360μm, and the largest angle alpha in the triangular longitudinal sections of the left baffle and the right baffle is 135 degrees. The side faces of the prism where the longer side of the triangular longitudinal section of the left baffle and the right baffle of the composite member is located are parallel to each other and are vertically arranged. The side surfaces of the left baffle and the right baffle of the composite member are respectively provided with holes and/or slits, and the ratio of the total area of the holes and/or slits to the area of the blade has the aperture ratio of 45%. 4 composite components are arranged in the fluidized bed reactor, the composite components are uniformly distributed in the reactor in a staggered mode, the acute/right-angle of pairwise intersection between every two adjacent composite components in the vertical direction is 90 degrees, and the vertical distance between every two adjacent composite components in the vertical direction is 100 mm. The composite components are parallel to each other on the same section, and the distance between the composite components adjacent to each other in the horizontal direction is 100 mm. The standard deviation of the dense phase zone in the fluidized bed was 1015Pa and the expansion coefficient was 1.28, the results are detailed in table 1.
[ example 6 ]
The device for preparing aniline by nitrobenzene hydrogenation is shown in figure 1. The average particle diameter of the catalyst is 360μm, and the largest angle alpha in the triangular longitudinal sections of the left baffle and the right baffle is 135 degrees. The side faces of the prism where the longer side of the triangular longitudinal section of the left baffle and the right baffle of the composite member is located are parallel to each other and are vertically arranged. The side surfaces of the left baffle and the right baffle of the composite member are respectively provided with holes and/or slits, and the ratio of the total area of the holes and/or slits to the area of the blade has the aperture ratio of 15%. 2 composite components are arranged in the fluidized bed reactor and are connected with each otherThe stagger is uniformly distributed in the reactor, the acute angle/right angle of pairwise intersection between every two adjacent composite components in the vertical direction is 90 degrees, and the vertical distance between the adjacent composite components in the vertical direction is 100 mm. The composite components are parallel to each other on the same section, and the distance between the composite components adjacent to each other in the horizontal direction is 100 mm. The standard deviation of the dense phase zone in the fluidized bed was 1217 Pa and the expansion coefficient was 1.23, and the results are detailed in Table 2.
[ example 7 ]
The device for preparing aniline by nitrobenzene hydrogenation is shown in figure 1. The average particle diameter of the catalyst is 360μm, and the largest angle alpha in the triangular longitudinal sections of the left baffle and the right baffle is 135 degrees. The side faces of the prism where the longer side of the triangular longitudinal section of the left baffle and the right baffle of the composite member is located are parallel to each other and are vertically arranged. The side surfaces of the left baffle and the right baffle of the composite member are respectively provided with holes and/or slits, and the ratio of the total area of the holes and/or slits to the area of the blade has the aperture ratio of 15%. 4 composite components are arranged in the fluidized bed reactor, the composite components are uniformly distributed in the reactor in a staggered mode, the acute/right-angle of pairwise intersection between every two adjacent composite components in the vertical direction is 90 degrees, and the vertical distance between every two adjacent composite components in the vertical direction is 80 mm. The composite components are parallel to each other on the same section, and the distance between the composite components adjacent to each other in the horizontal direction is 100 mm. The standard deviation of the dense phase zone in the fluidized bed was 1053 Pa and the expansion coefficient was 1.34, and the results are detailed in Table 2.
[ example 8 ]
The device for preparing aniline by nitrobenzene hydrogenation is shown in figure 1. The average particle diameter of the catalyst is 360μm, and the largest angle alpha in the triangular longitudinal sections of the left baffle and the right baffle is 135 degrees. The side faces of the prism where the longer side of the triangular longitudinal section of the left baffle and the right baffle of the composite member is located are parallel to each other and are vertically arranged. The side surfaces of the left baffle and the right baffle of the composite member are respectively provided with holes and/or slits, and the ratio of the total area of the holes and/or slits to the area of the blade has the aperture ratio of 15%. 4 composite components are arranged in the fluidized bed reactor, are uniformly distributed in the reactor in a staggered manner and are adjacent to each other in the vertical directionThe acute/right angle of the pairwise intersection between the components is 45 °, and the vertical distance between vertically adjacent composite components is 100 mm. The composite components are parallel to each other on the same section, and the distance between the composite components adjacent to each other in the horizontal direction is 100 mm. The standard deviation of the dense phase zone in the fluidized bed was 1089 Pa and the expansion coefficient was 1.35, and the results are detailed in Table 2.
[ example 9 ]
The device for preparing aniline by nitrobenzene hydrogenation is shown in figure 1. The average particle diameter of the catalyst is 360μm, and the largest angle alpha in the triangular longitudinal sections of the left baffle and the right baffle is 135 degrees. The side faces of the prism where the longer side of the triangular longitudinal section of the left baffle and the right baffle of the composite member is located are parallel to each other and are vertically arranged. The side surfaces of the left baffle and the right baffle of the composite member are respectively provided with holes and/or slits, and the ratio of the total area of the holes and/or slits to the area of the blade has the aperture ratio of 15%. 4 composite components are arranged in the fluidized bed reactor, the composite components are uniformly distributed in the reactor in a staggered mode, the acute/right-angle of pairwise intersection between every two adjacent composite components in the vertical direction is 90 degrees, and the vertical distance between every two adjacent composite components in the vertical direction is 100 mm. The composite components are parallel to each other on the same section, and the distance between the composite components adjacent to each other in the horizontal direction is 160 mm. The standard deviation of the dense phase zone in the fluidized bed was 1100 Pa and the expansion coefficient was 1.29, the results are detailed in Table 2.
[ COMPARATIVE EXAMPLE 1 ]
The grid type baffle plate used in the prior art is arranged in a fluidized bed reactor device, and the average particle size of the catalyst is 360 DEGμm, otherwise identical process conditions, a standard deviation of 1680 Pa for the dense phase zone in the fluidized bed and an expansion coefficient of 1.17, the results are detailed in table 3.
[ COMPARATIVE EXAMPLE 2 ]
The large-hole baffle plate used in the prior art is arranged in a fluidized bed reactor device, and the average particle size of the catalyst is 360 DEGμm, otherwise identical process conditions, a dense phase zone within the fluidized bed having a standard deviation of 1660 Pa and an expansion coefficient of 1.18, the results are detailed in Table 3.
[ COMPARATIVE EXAMPLE 3 ]
Without any baffles in the fluidized-bed reactor unit, i.e. free fluidized bed, the catalyst has an average particle size of 360%μm, the other process conditions were the same, the standard deviation of the dense phase zone in the fluidized bed was 1810 Pa, the expansion coefficient was 1.05 and the results are detailed in Table 3.
Obviously, has great technical advantages and can be used in the industrial production of preparing aniline. The method can also be used in other fluidized bed reactors, and is particularly suitable for coarse particle fluidized bed reactors.
TABLE 1
| Item | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Maximum angle alpha, DEG in the longitudinal section of the triangle | 135 | 145 | 90 | 135 | 135 |
| Open ratio of total area of openings and/or slits to area of blade | 15 | 15 | 15 | 5 | 45 |
| Number of |
4 | 4 | 4 | 4 | 4 |
| Horizontal direction interval in each layer of composite member, mm | 100 | 100 | 100 | 100 | 100 |
| Acute/right angle of two-by-two intersection between adjacent |
90 | 90 | 90 | 90 | 90 |
| Vertical distance, mm, between vertically adjacent composite members | 100 | 100 | 100 | 100 | 100 |
| Standard deviation of bed pressure, Pa | 825 | 876 | 1112 | 1070 | 1015 |
| Coefficient of bed expansion | 1.40 | 1.38 | 1.35 | 1.30 | 1.28 |
TABLE 2
| Item | Example 6 | Example 7 | Example 8 | Example 9 |
| Maximum angle alpha, DEG in the longitudinal section of the triangle | 135 | 135 | 135 | 135 |
| Open ratio of total area of openings and/or slots to area of blade | 15 | 15 | 15 | 15 |
| Number of |
2 | 4 | 4 | 4 |
| Horizontal direction interval in each layer of composite member, mm | 100 | 80 | 100 | 100 |
| Acute/right angle of two-by-two intersection between adjacent |
90 | 90 | 45 | 90 |
| Vertical distance, mm, between vertically adjacent composite members | 100 | 100 | 100 | 160 |
| Standard deviation of bed pressure, Pa | 1217 | 1053 | 1089 | 1100 |
| Coefficient of bed expansion | 1.23 | 1.34 | 1.35 | 1.29 |
TABLE 3
| Item | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Baffle type | Grille type baffle in prior art | Large hole baffle plate in prior art | Without baffle |
| Standard deviation of bed pressure, Pa | 1680 | 1660 | 1810 |
| Coefficient of bed expansion | 1.17 | 1.18 | 1.05 |
Claims (6)
1. A fluidized bed reaction device comprises a fluidized bed reactor (3), and is characterized in that a composite component (2) and a heat removal water pipe (4) are arranged in the fluidized bed reactor (3), and the composite component (2) is formed by combining a left baffle (23) and a right baffle (24); the left baffle (23) and the right baffle (24) are respectively composed of triangular prisms with triangular longitudinal sections, the largest angle alpha in the triangular longitudinal sections of the left baffle (23) and the right baffle (24) is 90-145 degrees, the prism side surfaces where the longer sides in the triangular longitudinal sections of the left baffle (23) and the right baffle (24) are located are parallel to each other and are vertically arranged, two rows of holes and/or slits are respectively formed in the side surfaces of the left baffle (23) and the right baffle (24), and gas and particles can be crushed from the holes and/or slits and escape; the holes and/or slits in the upper row are upper holes (21), the holes and/or slits in the lower row are lower holes (22), and the aperture ratio of the total area of the holes and/or slits to the area of the blade is 5% -45%;
at least 1 composite component (2) is arranged in the fluidized bed reactor (3), the composite components (2) are uniformly distributed in the reactor in a staggered mode, the acute/right angle of pairwise intersection between every two adjacent composite components (2) in the vertical direction is 30-90 degrees, and the vertical distance between every two adjacent composite components (2) in the vertical direction is not smaller than 80 mm.
2. The fluidized bed reactor according to claim 1, characterized in that the composite members (2) are parallel two by two on the same cross section, and the distance between the horizontally adjacent composite members (2) is not less than 100 mm.
3. A fluidized reaction method for hydrogenation of nitrobenzene using the fluidized bed reactor of claim 1 or 2, characterized by comprising the steps of: the vaporized nitrobenzene and hydrogen raw materials enter a fluidized bed reactor (3), the catalyst in the reactor is pushed to fluidize, bubbles with different sizes and flowing catalyst are formed, after large bubbles are extruded and crushed by a composite member (2), part of gas and particles are sprayed out from a left baffle (23) and a right baffle (24), the rest gas and particles are crushed and escaped from openings and/or slits on the side surfaces of the left baffle (23) and the right baffle (24), catalyst particle clusters and transverse large bubbles are crushed, and nitrobenzene, hydrogen and catalytic particles efficiently contact, mix and react in the fluidized bed reactor to produce aniline products.
4. The fluidized bed reaction method according to claim 3, wherein the catalyst is a metal supported catalyst comprising copper as a main active component and silica as a carrier, and has an average particle diameter of 50 to 600μm is less than 80μThe content of particles below m is not less than 2%.
5. The fluidized bed reaction method according to claim 3, wherein the linear velocity of the gas passing between the left baffle (23) and the right baffle (24) of the composite member (2) is 0.5 to 6 m/s.
6. The fluidized bed reaction method according to claim 3, characterized in that the reaction conditions in the fluidized bed reactor (3) are: the superficial gas velocity is 0.1-0.9 m/s, the mass ratio of hydrogen to nitrobenzene is 6-21: 1, the average reaction temperature in the reaction zone is controlled at 220-285 ℃, and the reaction pressure in the reaction zone is 0.05-1 MPa.
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| CN113908779A (en) * | 2020-07-10 | 2022-01-11 | 国家能源投资集团有限责任公司 | Stationary fluidized bed, fluidizing system and fluidizing method |
| CN114425282B (en) * | 2020-10-14 | 2023-05-02 | 中国石油化工股份有限公司 | Aromatic hydrocarbon ammoxidation fluidized bed reaction device and reaction method |
| CN114426489A (en) * | 2020-10-15 | 2022-05-03 | 中国石油化工股份有限公司 | Device and method for preparing aniline by nitrobenzene hydrogenation |
| CN113522743B (en) * | 2021-07-30 | 2022-05-17 | 中国矿业大学 | Method and system for weakening bubbles in gas-solid separation fluidized bed |
| CN114649496B (en) * | 2022-03-28 | 2023-06-27 | 中国石油大学(北京) | Preparation device and method of silicon composite material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2680665Y (en) * | 2004-02-17 | 2005-02-23 | 山东海化魁星化工有限公司 | Melamine fluidized bed reactor |
| CN101912753A (en) * | 2010-08-13 | 2010-12-15 | 中国石油大学(北京) | Composite inner component for gas-solid fluidized bed |
| CN103638877A (en) * | 2013-11-15 | 2014-03-19 | 浙江大学 | Fluidized bed reactor |
| CN107281981A (en) * | 2017-06-26 | 2017-10-24 | 清华大学 | A kind of inner member, fluidized-bed reactor and application process |
| CN212119948U (en) * | 2020-03-26 | 2020-12-11 | 中国石油化工股份有限公司 | Fluidized bed reactor |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6063434A (en) * | 1984-08-17 | 1985-04-11 | Babcock Hitachi Kk | Measurer for temperature in fluidized bed |
-
2020
- 2020-03-26 CN CN202010222841.2A patent/CN111298727B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2680665Y (en) * | 2004-02-17 | 2005-02-23 | 山东海化魁星化工有限公司 | Melamine fluidized bed reactor |
| CN101912753A (en) * | 2010-08-13 | 2010-12-15 | 中国石油大学(北京) | Composite inner component for gas-solid fluidized bed |
| CN103638877A (en) * | 2013-11-15 | 2014-03-19 | 浙江大学 | Fluidized bed reactor |
| CN107281981A (en) * | 2017-06-26 | 2017-10-24 | 清华大学 | A kind of inner member, fluidized-bed reactor and application process |
| CN212119948U (en) * | 2020-03-26 | 2020-12-11 | 中国石油化工股份有限公司 | Fluidized bed reactor |
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