CN110871046A - Low-pressure-drop Z-shaped radial centrifugal flow fixed bed reactor - Google Patents
Low-pressure-drop Z-shaped radial centrifugal flow fixed bed reactor 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
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0207—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly horizontal
- B01J8/0214—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly horizontal in a cylindrical annular shaped bed
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0278—Feeding reactive fluids
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00938—Flow distribution elements
Abstract
The invention provides a low-pressure drop Z-shaped radial centrifugal flow fixed bed reactor, which comprises: the catalytic bed comprises a cylindrical pressure container, an inner cylinder, an outer cylinder and a catalytic bed, wherein the inner cylinder, the outer cylinder and the cylindrical pressure container are coaxially arranged, an interlayer space is formed between the outer wall surface of the inner cylinder and the inner wall surface of the outer cylinder, a lower supporting end enclosure, the inner cylinder and the outer cylinder are enclosed to form the catalytic bed, and the lower supporting end enclosure is positioned in the cylindrical pressure container and at the bottom of the cylindrical pressure container; the inner cylinder is communicated with the gas inlet to form a reaction gas flow dividing channel, a reaction gas flow collecting channel is formed between the outer wall surface of the outer cylinder and the inner wall surface of the cylindrical pressure container, and the reaction gas flow collecting channel is communicated with the gas outlet; the flow dividing channel is a reducing flow channel, the inner cylinder is provided with holes, and the outer cylinder is provided with holes; the reaction gas flows through the catalytic bed from the shunting flow passage through the inner cylinder outwards in a radial flow manner, enters the collecting flow passage through the outer cylinder and flows out of the fixed bed reactor, and the direction of the reaction gas in the fixed bed reactor is Z-shaped.
Description
Technical Field
The invention relates to a method for reducing H2/N2A low-pressure drop centrifugal Z-shaped radial centrifugal flow fixed bed reactor for preparing synthetic ammonia by using a ruthenium-based catalyst in comparison with synthetic gas belongs to the technical field of synthetic ammonia chemical technology and energy recycling.
Background
Ammonia synthesis has been an important position in the world's chemical industry, with about 10% of the energy worldwide being used to synthesize ammonia. Therefore, catalysts, reactors and processes for ammonia synthesis are always the focus and the focus of research. Currently, the most common ammonia synthesis catalyst used in industry is an iron-based catalyst. The iron-based catalyst has the advantages of easy preparation and low cost, but the iron-based catalyst has obvious disadvantages, such as higher requirements on the temperature and pressure of the reaction, particularly the temperature, the iron-based catalyst has high activity at higher temperature, and the higher temperature restricts the thermodynamic balance of ammonia synthesis, but increases the energy consumption. In addition, iron-based catalysts are also susceptible to deactivation by poisoning with contaminants such as sulfur dioxide. U.S. Pat. No. 4, 2005053541,8932 and Chinese patents ZL01125634.6, ZL200310116228.9, ZL200810071543.7, ZL201410333516.8 and ZL201410254506.5 provide a ruthenium-based catalyst with large specific surface area and high activity, the catalyst adopts graphitized carbon black or activated carbon as a carrier, and the catalyst has high activity, so that the reaction can be carried out under mild conditions. However, ruthenium-based catalysts are expensive, and although the U.S. Pat. No. 4,000,68532 and chinese patents ZL201610688473.4 and CN201410746394.5 use iron and ruthenium-based catalysts in series, the high activity advantage of ruthenium-based catalysts can be fully exerted, and the catalyst cost can be saved and the catalysts can be industrially applied. However, in the case of the ruthenium catalyst using activated carbon as a carrier, methanation and pulverization by washing are liable to occur, so that the safety of the apparatus is affected.
Most of iron-based catalyst radial ammonia synthesis reactors used in the industry at present are based on US patents US 5429809, US4971771, US 4769220 and the like, because the pressure of a reaction system is up to 12-22 MPa, the radial distribution of fluid is mainly controlled by a central pipe in the reactor, the iron-based catalyst radial ammonia synthesis reactor has the defects of high perforation speed, large pressure drop of the reactor, easy pulverization of ruthenium-based catalyst, incapability of preventing powder from escaping, and unsuitability for ammonia synthesis of the ruthenium-based catalyst, while traditional momentum exchange type radial reactors ZL96114363.0, ZL201410012467.8, ZL 2007101920. X, ZL201120338173.6 and the like use a central guide cone or optimize the radial distribution of fluid of a runner П type, but are not completely used for friction type high-pressure ammonia synthesis reactors.
Disclosure of Invention
In order to solve the problems of low pressure drop, scour prevention of the catalyst and separation of the broken catalyst in the ammonia synthesis process of the ruthenium-based catalyst, the invention provides a low-pressure-drop Z-shaped radial centrifugal flow fixed bed reactor. The fixed bed reactor is suitable for ammonia synthesis reaction of ruthenium-based catalyst, and is characterized by comprising:
the cylindrical pressure container is provided with an upper end sealing head and a bottom sealing head, the upper end sealing head is provided with a gas inlet, and the bottom sealing head is provided with a gas outlet;
the inner cylinder is arranged in the cylindrical pressure container and is coaxial with the cylindrical pressure container, and the inner cylinder is provided with a plurality of openings and is a porous wall inner cylinder;
the outer cylinder is arranged in the cylindrical pressure container, is coaxial with the inner cylinder and surrounds the inner cylinder, the radius of the inner cylinder is smaller than that of the outer cylinder with the porous wall, and the upper part of the outer cylinder is not provided with a hole and the lower part of the outer cylinder is provided with a hole;
a barrier space is formed between the outer wall surface of the inner barrel and the inner wall surface of the outer barrel, the bottom of the barrier space is connected with a lower supporting end socket used for sealing the bottom of the barrier space, the lower supporting end socket, the inner barrel and the outer barrel enclose to form a catalytic bed, the catalytic bed is filled with catalyst, and the upper part of the catalytic bed is open; the lower supporting seal head is positioned in the cylindrical pressure container and at the bottom of the cylindrical pressure container;
the inner cylinder is communicated with the gas inlet to form a reaction gas flow dividing channel, a reaction gas flow collecting channel is formed between the outer wall surface of the outer cylinder and the inner wall surface of the cylindrical pressure container, and the reaction gas flow collecting channel is communicated with the gas outlet; the flow dividing flow passage is a reducing flow passage;
the reaction gas flows through the catalytic bed from the diversion flow channel through the inner cylinder outwards in a radial flow manner, enters the flow collection flow channel through the outer cylinder, and then flows out of the fixed bed reactor through the gas outlet, and the direction of the reaction gas in the fixed bed reactor is Z-shaped.
In one embodiment, the inner barrel is a perforated cylindrical inner barrel or a perforated waist drum shaped inner barrel.
In one embodiment, the inner cylinder is a porous waist drum inner cylinder, and the shape of the flow distribution channel is also waist drum.
In one embodiment, if the inner cylinder is a porous cylindrical inner cylinder, a dumbbell-shaped diversion cone is arranged in the inner cylinder, and the diversion flow channel is formed by a dumbbell-shaped diversion cone arranged in the inner cylinder.
In one embodiment, the inner cylinder is formed by rolling a double-layer structure consisting of a porous plate and a Johnson net, and the aperture ratio of the porous plate is 1-50%.
In one embodiment, the outer cylinder is a porous wall outer cylinder formed integrally or an outer cylinder formed by a plurality of hollow fan-shaped elements arranged along adjacent circumferences close to the inner wall surface of the cylindrical pressure vessel.
In one embodiment, the outer cylinder comprises a double-layer structure of johnson mesh and a support structure or only a single-layer structure of johnson mesh, and the outer cylinder is formed by rolling johnson mesh alone or by rolling the double-layer structure of johnson mesh and the support structure, and the support structure is provided with openings.
In one embodiment, when the outer cylinder has a double-layer structure of a johnson mesh and a support structure, the johnson mesh is close to the catalyst side, the support structure is close to the inner wall side of the cylindrical pressure vessel, and the support structure is a porous thick plate having an aperture ratio of 20 to 40%.
In one embodiment, a filtering unit is arranged in the collecting flow channel, and the filtering unit is arranged in a space formed by the lower supporting end socket and the bottom end socket and used for preventing pulverized catalyst dust from flowing out.
In one embodiment, a catalyst seal is inserted into an upper opening of the catalyst bed, the top of the catalyst seal is filled with inert solid particulate materials, a non-perforated part of the upper part of the outer cylinder faces the catalyst seal, and reaction gas flows axially and radially in the catalyst seal.
Compared with the prior art, the reaction method and the reaction device provided by the invention have the following advantages:
1. the diversion flow channel adopts the reducing flow channel, thereby overcoming the influence of friction resistance of the high-pressure reactor on the change of fluid pressure, leading the fluid to be more uniformly distributed along the axial direction of the fixed bed reactor and leading the pressure drop of the reactor to be lower;
2. the inner cylinder with the porous wall adopts higher opening rate, reduces the perforation speed of the catalyst entering the catalytic bed layer, and reduces the washing of the catalyst;
3. reaction gas centrifugally flows outwards from the center in the catalytic bed layer, the flow rate of the gas out of the bed layer is low, and catalyst powder is prevented from being carried out;
4. the outlet of the reactor is provided with a filtering unit to prevent the powdered catalyst powder from escaping.
In conclusion, the fixed bed reactor is adopted to synthesize ammonia of ruthenium-based catalyst with low hydrogen-nitrogen ratio, and has the characteristics of uniform distribution of reaction gas along the axial direction, low perforation speed of the catalytic bed layer, low gas flow velocity of the catalytic bed layer, small washing of fluid on the catalyst, small pressure drop of the flowing fluid through the reactor, high net content of the outlet gas ammonia, safe industrial production and the like.
Drawings
FIG. 1 is a low pressure drop Z-shaped radial centrifugal flow fixed bed reactor provided by the invention.
FIG. 2 is another low-pressure drop Z-shaped radial centrifugal flow fixed bed reactor provided with a dumbbell-shaped diversion cone.
Wherein:
1-gas inlet;
2-a flow dividing channel;
3-an inert solid particulate material;
4, an inner cylinder;
5-catalytic bed;
6, an outer cylinder;
7-reaction gas collecting flow channel;
8-a cylindrical pressure vessel;
9-lower supporting end socket;
10-bottom end enclosure;
11-gas outlet;
12-a filtration unit;
13-dumbbell type diversion cone.
Detailed Description
The invention will be further described with reference to the accompanying drawings, which are only included to assist understanding of the invention and do not limit the scope of the invention:
as can be seen from FIG. 1, the low-pressure drop Z-shaped radial centrifugal flow fixed bed reactor of the present invention is suitable for ammonia synthesis reaction of ruthenium-based catalyst, and can solve the following problems existing in the prior art:
1. the ruthenium-based catalyst takes active carbon or other carbon materials as a carrier, and the carbon carrier is easy to be pulverized and then taken out of a reactor in the ammonia synthesis reaction, so that the safety of the device is greatly influenced.
2. The existing reactor applied to the iron-based catalyst synthesis of ammonia has the defects of high perforation speed, large pressure drop of the reactor and easy pulverization of ruthenium-based catalyst, can not prevent powder from escaping, and is not suitable for ammonia synthesis of ruthenium-based catalyst, and the existing momentum exchange type radial reactor is not completely suitable for a friction resistance type high-pressure ammonia synthesis reactor.
The fixed bed reactor of the present invention comprises: a cylindrical pressure vessel 8, an inner cylinder 4 and an outer cylinder 6. The cylindrical pressure container 8 is provided with an upper end seal head and a bottom seal head 10, the upper end seal head is provided with a gas outlet 1, and the bottom seal head 10 is provided with a gas outlet 11; an inner cylinder 4 and an outer cylinder 6 which are coaxial with the cylindrical pressure container 8 are arranged in the cylindrical pressure container 8, the outer cylinder 6 is provided with an opening and is a porous wall outer cylinder, the upper side wall of the inner cylinder 4 is not provided with an opening, the lower part of the inner cylinder is provided with an opening, the inner cylinder 4 is coaxial and surrounds the inner cylinder 4, the radius of the inner cylinder 4 is smaller than that of the porous wall outer cylinder, namely the inner cylinder 4 and the outer cylinder 6 are sequentially arranged in the center of the cylindrical pressure container 8 along the radial direction, in one embodiment of the invention, the outer cylinder 6 is an integrally formed porous wall outer cylinder or a porous wall outer cylinder formed by arranging a plurality of hollow fan-shaped elements along the adjacent circumference at the position close. The outer cylinder 6 comprises a double-layer structure of johnson mesh and a support structure or only comprises a single-layer structure of johnson mesh, that is, the outer cylinder 6 is formed by separately rolling johnson mesh, or by rolling the double-layer structure formed by johnson mesh and the support structure, the height of the opening area of the outer cylinder 6 is H, when the outer cylinder 6 is formed by tightly adhering the support structure to the johnson mesh to form a double-layer tight structure, the johnson mesh is close to the catalyst side, the support structure is close to the inner wall side of the cylindrical pressure vessel 8, the support structure is provided with openings, the support structure can be a thick plate with openings, the material of the thick plate can be a metal material, and in an embodiment of the invention, the support structure is a porous thick steel plate.
A barrier space is formed between the outer wall surface of the inner barrel 4 and the inner wall surface of the outer barrel 6, the bottom of the barrier space is connected with a lower supporting end socket 9 for sealing the bottom of the barrier space, the lower supporting end socket 9, the inner barrel 4 and the outer barrel 6 enclose to form a catalytic bed 5, the catalytic bed 5 is filled with catalyst, and the upper part of the catalytic bed 5 is open; the lower supporting end enclosure 9 is positioned in the cylindrical pressure vessel 8 and at the bottom of the cylindrical pressure vessel 8. The reaction gas collecting flow passage 7 is formed by a fan-shaped porous hollow element or between the outer cylinder with the porous wall and the inner wall of the cylindrical container.
The inner cylinder 4 is a porous wall inner cylinder and is formed by rolling a double-layer close-contact structure consisting of a porous plate and a Johnson net, the aperture ratio of the porous plate is 1-50%, and the shape of the inner cylinder 4 can be a cylindrical cylinder or a waist drum-shaped cylinder, such as a porous cylindrical or porous waist drum-shaped inner cylinder. The inner cylinder 4 is communicated with the gas inlet l to form a reaction gas diversion flow channel 2, a reaction gas collecting flow channel 7 is formed between the outer wall surface of the outer cylinder 6 and the inner wall surface of the cylindrical pressure container 8, or a fan-shaped porous hollow element forms the reaction gas collecting flow channel 7, and the reaction gas collecting flow channel 7 is communicated with the gas outlet 11; the flow dividing channel 2 is a reducing channel, all the inner cylinder 4 is provided with holes, and part of the outer cylinder 6 is provided with holes, specifically, the upper part of the outer cylinder 6 is not provided with holes, and the lower part of the outer cylinder is provided with holes.
The reaction gas flows through the catalytic bed 5 from the diversion flow channel 2 through the inner barrel 4 outwards in a radial flow mode, enters the collecting flow channel 7 through the outer barrel 6, and flows out of the fixed bed reactor through the gas outlet 11 in a Z-shaped centrifugal radial flow mode. And a filtering unit 12 is arranged in the collecting flow channel 7, and the filtering unit 12 is arranged in a space formed by the lower supporting end socket 9 and the bottom end socket and used for preventing pulverized catalyst dust from flowing out. The reaction gas collecting flow channel 7 is communicated with a reaction gas outlet 11 arranged on a bottom end enclosure 10 of the cylindrical pressure vessel 8 through the space between the lower supporting end enclosure 9 and the bottom end enclosure 10; the filtering unit 10 is made of a metal wire mesh, so that pulverized catalyst fine particles can be effectively prevented from flowing out, the safety of a rear-stage compressor is guaranteed, and the safety performance of the reaction process is higher.
If the inner cylinder 4 is a cylindrical column, a dumbbell-shaped guide cone 13 needs to be arranged in the inner cylinder 4. If the inner cylinder is a porous waist-drum-shaped inner cylinder, the shape of the flow distribution channel 2 is also waist-drum-shaped, and the middle diameter of the waist-drum-shaped inner cylinder is larger than the diameters of the top and the bottom. It should be noted that the flow dividing channel 2 is a variable flow channel, and the variable cross-section technology of the flow dividing channel 2 can ensure that the fluid inside the friction-dominant reactor is uniformly distributed in the radial direction, and since the present invention implements the variable diameter technology of the reaction gas in the flow dividing channel 2, the inner porous wall cylinder 4 serving as the reaction gas distributor can keep a considerable aperture ratio, and the uniform distribution of the reaction gas along the axial direction and the perforation speed of the intersecting inlet catalytic bed 5 layer are ensured while the low pressure drop of the reactor is realized.
A catalyst is filled between the inner cylinder 4 and the outer cylinder 6; the upper opening of the catalytic bed 5 is inserted with a section of catalyst seal with height H', the top of the catalyst seal is filled with a certain thickness of inert solid particle material, the top of the catalyst seal is not provided with a cover plate, the inert solid particle material is inert ceramic ball material 3, for example, the catalyst seal and the inert ceramic ball material 3 are used for ensuring the axial and radial flow of reaction gas and the safety of the catalyst seal.
It is worth mentioning that the inner cylinder 4 is a porous wall inner cylinder with all holes, the porous wall inner cylinder is provided with big holes, the hole opening rate is 5-50%, the hole opening speed on the inner cylinder is reduced, and the washing of the catalyst is reduced. The outer cylinder is a porous wall outer cylinder 6 with no hole on the upper side wall H' and the height of the lower part hole H. The non-hole part on the upper part of the outer cylinder 6 is opposite to the catalyst seal, and the reaction gas flows in the catalyst seal in the axial and radial directions.
The outer cylinder 6 is a porous wall outer cylinder or a porous wall outer cylinder formed by a plurality of fan-shaped hollow elements arranged along the inner near wall of the circular container 8 in an adjacent circumferential mode, the outer cylinder comprises a double-layer structure formed by Johnson nets and a supporting structure or only comprises one layer structure of the Johnson nets, the outer cylinder is formed by independently rolling the Johnson nets or rolling the double-layer structure formed by the Johnson nets and the supporting structure, and the supporting structure is provided with openings. When the outer cylindrical housing has a double-layer structure of a johnson mesh and a support structure, the johnson mesh is close to the catalyst side, the support structure is close to the inner wall side of the cylindrical pressure vessel 8, the support structure is a porous thick plate, and the aperture ratio of the porous thick plate is 20-40%. Wherein the catalyst side is a Johnson mesh and the cylindrical vessel 8 side is a support structure; the height of the opening area of the outer cylinder 6 is H.
The reaction gas enters the reactor from a reaction gas inlet 1, then is shunted with a porous wall inner cylinder 4 through a reaction gas shunt channel 2, sequentially flows through a catalytic bed 5 and a porous wall outer cylinder 6 in a radial flow mode, is removed of powdered catalyst through a filtering unit 12 by a reaction gas collecting channel 7, and then flows out of the reactor from a reaction gas outlet 11, and the reaction gas is in a Z shape in the direction of the fixed bed reactor.
FIG. 1 is a low pressure drop Z-shaped radial centrifugal flow fixed bed reactor provided by the invention. FIG. 2 is another low-pressure drop Z-shaped radial centrifugal flow fixed bed reactor provided with a dumbbell-shaped diversion cone. The structure of fig. 2 is substantially the same as that of fig. 1, except that the inner cylinder 4 in fig. 2 is a porous cylindrical inner cylinder formed by combining a porous plate with a johnson net, and the aperture ratio of the porous plate is 1-50%; the dumbbell-shaped diversion cone 13 is arranged in the inner porous wall cylinder 4 to form a diversion flow channel 2 of the reaction gas, and the variable cross section technology of the diversion flow channel 2 can ensure that the fluid is uniformly distributed in the radial direction in the reactor.
The Z-shaped radial centrifugal flow fixed bed reactor for ammonia synthesis of the ruthenium-based catalyst can be implemented in the ammonia synthesis process of iron-series ruthenium provided by CN 201410746394.5.
In the iron-ruthenium synthesis ammonia process, raw material gas firstly passes through 2-3 reactors filled with iron-based catalysts, after a certain amount of ammonia is contained in products at the outlet of the reactors, the products are limited by chemical thermodynamic equilibrium, and at the moment, the products are introduced into the ruthenium-based catalysts to continue to react, so that more ammonia can be obtained. The inlet temperature of the ruthenium-based catalyst reactor is controlled at 360 ℃, the temperature is lower than that of the iron-based catalyst, the loading amount of the ruthenium-based catalyst is relatively small, the pressure drop of the reactor is low, and the balance right shift is facilitated, so that the ammonia yield can be further increased, and the energy consumption is reduced.
The following examples respectively take an iron-based catalyst and an iron-based catalyst in series with a ruthenium-based catalyst as examples, and compare different reactors to verify the advantages of the iron-based ruthenium process. In all examples, the fresh air intake was kept constant at 5100 kmol/h. Wherein the ammonia yield is increased by taking a KBR (Kallog Brownian-Lutt group in America) three-tower iron-based catalyst reactor as a calculation standard, and the purge hydrogen recovery is performed by taking the hydrogen consumption of the KBR three-tower iron-based catalyst reactor minus the lowest hydrogen consumption of an ammonia synthesis theory as a calculation standard; the ton ammonia compression power consumption takes the KBR three-tower iron-based catalyst reactor compression power consumption as a calculation standard.
Example 1:
taking three existing axial reactor processes filled with iron-based catalyst as an example, fresh room temperature low pressure synthesis gas H2/N2The ratio is 3.00, the air input is 5100kmol/h, the pressure of the synthesis gas entering the first iron-based catalyst reactor is 150atm, the temperature is 350 ℃, the temperature of the synthesis gas entering the second iron-based catalyst reactor and the third iron-based catalyst reactor is 380 ℃, the purge proportion of the circulating gas is 4 percent, and the catalyst filling amount of the first iron-based catalyst reactor is 15m3Second iron-based catalyst reactor catalyst loading 25m3And the catalyst loading of the third iron-based catalyst reactor is 40m3The final outlet ammonia concentration is 20.92%, and the production indexes are shown in Table 1.
TABLE 1 reaction pressure 150atm, H2/N2Iron catalyst production index value of 3.0
Example 2:
taking the process of connecting two existing axial reactors filled with iron-based catalysts in series and one existing axial reactor filled with ruthenium-based catalysts as an example, the air input is 5100kmol/H, and the fresh synthesis gas H with normal temperature and low pressure2/N2The ratio is 3.00, the pressure of the synthesis gas entering the iron-based catalyst reactor is 150atm, and the synthesis gas enters the first reactorThe temperature of the iron-based catalyst reactor is 350 ℃, the temperature of the synthesis gas entering the second iron-based catalyst reactor is 380 ℃, and the reaction temperature entering the third ruthenium-based catalyst reactor is 360 ℃. The purge ratio of the circulating gas is 4 percent, and the catalyst loading of the first iron-based catalyst reactor is 15m3And a second iron-based catalyst reactor having a loading of 40m3Catalyst loading of the third ruthenium-based catalyst reactor 9m3And the final outlet ammonia concentration is 22.78%, and the production indexes are shown in Table 2.
TABLE 2 reaction pressure 150atm, H2/N2Iron-ruthenium catalyst production index at 3.0
Example 3:
two existing axial reactors filled with iron-based catalyst are connected in series with a Z-shaped radial centrifugal flow fixed bed reactor filled with ruthenium-based catalyst, for example, the device shown in the attached figures 1 and 2 is used, the air input is 5100kmol/H, and the fresh synthesis gas H at normal temperature and low pressure is2/N2The ratio is 3.00, the pressure of the synthesis gas entering the iron-based catalyst reactor is 150atm, the temperature of the synthesis gas entering the first iron-based catalyst reactor is 350 ℃, the temperature of the synthesis gas entering the second iron-based catalyst reactor is 380 ℃, and the reaction temperature of the synthesis gas entering the third ruthenium-based catalyst reactor is 360 ℃. The purge ratio of the circulating gas is 4 percent, and the catalyst loading of the first iron-based catalyst reactor is 15m3And a second iron-based catalyst reactor having a loading of 40m3Catalyst loading of the third ruthenium-based catalyst reactor 9m3The final outlet ammonia concentration is 22.98%, and the production indexes are shown in Table 3.
TABLE 3 reaction pressure 150atm, H2/N2Iron-ruthenium catalyst production index at 3.0
Example 4:
two existing axial reactors filled with iron-based catalyst are connected in series with two Z-shaped radial centrifugal flow fixed bed reactors filled with ruthenium-based catalyst, the Z-shaped radial centrifugal flow fixed bed reactors are shown in the attached figures 1 and 2, the air input is 5100kmol/H, and the fresh normal-temperature low-pressure synthesis gas H is2/N2The ratio is 3.00, the pressure of the synthesis gas entering the iron-based catalyst reactor is 150atm, the temperature of the synthesis gas entering the first iron-based catalyst reactor is 350 ℃, the temperature of the synthesis gas entering the second iron-based catalyst reactor is 380 ℃, and the reaction temperature of the synthesis gas entering the third and the fourth ruthenium-based catalyst reactors is 360 ℃. The purge ratio of the circulating gas is 4 percent, and the catalyst loading of the first iron-based catalyst reactor is 15m3And a second iron-based catalyst reactor having a loading of 40m3Catalyst loading of the third ruthenium-based catalyst reactor 7m3Catalyst loading of the fourth ruthenium-based catalyst reactor 9m3The final outlet ammonia concentration is 23.09%, and the production indexes are shown in Table 4.
TABLE 4 reaction pressure 150atm, H2/N22.90 hours iron-on-ruthenium catalyst production index
It can be seen from the above examples that, in the process of synthesizing ammonia by using iron-ruthenium catalyst, the low-pressure drop Z-shaped radial centrifugal flow fixed bed reactor of the present invention has the advantages of low energy consumption, low pressure drop, etc., which also results in that the yield of ammonia gas using the reactor is higher than that of the traditional axial reactor, more hydrogen can be recovered, not only the reaction raw materials are saved, but also the energy consumption is reduced.
The Z-shaped radial centrifugal flow fixed bed reactor provided by the invention aims at the characteristic that ruthenium-based catalyst is easy to pulverize under the condition of high flow rate, the perforation rate of the ruthenium-based catalyst in a catalytic bed layer is increased and reduced, and the flow rate of reaction gas out of the catalytic bed layer is reduced by centrifugal flow, so that the catalyst is prevented from being washed away. And secondly, aiming at the dominant frictional resistance characteristic of the high-pressure ammonia synthesis reactor, a flow channel is changed or a flow guide cone is additionally arranged, so that the distribution condition of the fluid in the reactor is optimized. In order to improve the safety of the reactor, a filtering unit is arranged in front of the reaction gas outlet 11 to filter the pulverized catalyst, so that safety accidents are prevented.
Claims (10)
1. A low pressure drop Z-shaped radial centrifugal flow fixed bed reactor is suitable for ammonia synthesis reaction of ruthenium-based catalyst, and is characterized in that the fixed bed reactor comprises:
the cylindrical pressure container is provided with an upper end sealing head and a bottom sealing head, the upper end sealing head is provided with a gas inlet, and the bottom sealing head is provided with a gas outlet;
the inner cylinder is arranged in the cylindrical pressure container and is coaxial with the cylindrical pressure container, and the inner cylinder is provided with a plurality of openings and is a porous wall inner cylinder;
the outer cylinder is arranged in the cylindrical pressure container, is coaxial with the inner cylinder and surrounds the inner cylinder, the radius of the inner cylinder is smaller than that of the outer cylinder with the porous wall, and the upper part of the outer cylinder is not provided with a hole and the lower part of the outer cylinder is provided with a hole;
a barrier space is formed between the outer wall surface of the inner barrel and the inner wall surface of the outer barrel, the bottom of the barrier space is connected with a lower supporting end socket used for sealing the bottom of the barrier space, the lower supporting end socket, the inner barrel and the outer barrel enclose to form a catalytic bed, the catalytic bed is filled with catalyst, and the upper part of the catalytic bed is open; the lower supporting seal head is positioned in the cylindrical pressure container and at the bottom of the cylindrical pressure container;
the inner cylinder is communicated with the gas inlet to form a reaction gas flow dividing channel, a reaction gas flow collecting channel is formed between the outer wall surface of the outer cylinder and the inner wall surface of the cylindrical pressure container, and the reaction gas flow collecting channel is communicated with the gas outlet; the flow dividing flow passage is a reducing flow passage;
the reaction gas flows through the catalytic bed from the diversion flow channel through the inner cylinder outwards in a radial flow manner, enters the flow collection flow channel through the outer cylinder, and then flows out of the fixed bed reactor through the gas outlet, and the direction of the reaction gas in the fixed bed reactor is Z-shaped.
2. The low-pressure-drop Z-type radial centrifugal flow fixed bed reactor of claim 1, wherein the inner cylinder is a porous cylindrical inner cylinder or a porous waist drum shaped inner cylinder.
3. The low pressure drop Z-type radial centrifugal flow fixed bed reactor of claim 2, wherein the inner cylinder is a porous waist-drum inner cylinder, and the shape of the flow-dividing channel is also waist-drum.
4. The low pressure drop Z-type radial centrifugal flow fixed bed reactor of claim 2, wherein if the inner cylinder is a porous cylindrical inner cylinder, a dumbbell-shaped diversion cone is disposed in the inner cylinder, and the diversion flow channel is formed by the dumbbell-shaped diversion cone disposed in the inner cylinder.
5. The low-pressure-drop Z-shaped radial centrifugal flow fixed bed reactor as claimed in claim 2, wherein the inner tube is formed by rolling a double-layer structure consisting of a porous plate and a Johnson net, and the porous plate has an aperture ratio of 1-50%.
6. The low-pressure-drop Z-type radial centrifugal flow fixed-bed reactor of claim 1, wherein said outer barrel is an integrally formed perforated wall outer barrel or an outer barrel formed by a plurality of hollow sector-shaped elements arranged in adjacent circumferential rows along an inner wall surface adjacent to said cylindrical pressure vessel.
7. The low-pressure-drop Z-type radial centrifugal flow fixed-bed reactor as claimed in claim 6, wherein said outer cylindrical shell comprises a double-layer structure of Johnson mesh and a support structure or only a single-layer structure of Johnson mesh, said outer cylindrical shell being formed by rolling Johnson mesh alone or by rolling a double-layer structure of Johnson mesh and a support structure, said support structure being provided with openings.
8. The low-pressure-drop Z-type radial centrifugal flow fixed-bed reactor of claim 7, wherein when said outer cylindrical shell is a double-layered structure of a johnson mesh and a support structure, said johnson mesh is adjacent to said catalyst side, said support structure is adjacent to an inner wall side of said cylindrical pressure vessel, said support structure is a porous thick plate, and an aperture ratio of said porous thick plate is 20-40%.
9. The low pressure drop Z-type radial centrifugal flow fixed bed reactor of claim 1, wherein a filtering unit is disposed in the collecting flow channel, and the filtering unit is disposed in a space formed by the lower supporting head and the bottom head to prevent pulverized catalyst dust from flowing out.
10. The low pressure drop Z-type radial centrifugal flow fixed bed reactor as claimed in claim 1, wherein a catalyst seal is inserted into an upper opening of said catalyst bed, a top portion of said catalyst seal is filled with inert solid particulate material, a non-perforated portion of an upper portion of said outer shell faces said catalyst seal, and the reaction gas flows axially and radially in said catalyst seal.
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| CN113509894A (en) * | 2021-07-22 | 2021-10-19 | 中冶赛迪工程技术股份有限公司 | Moving bed gas-solid radial reactor |
| CN114425278A (en) * | 2020-10-15 | 2022-05-03 | 中国石油化工股份有限公司 | Device and method for producing low-carbon olefin and application |
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