WO2016055452A1 - Réacteur pour effectuer des réactions en phase gazeuse au moyen d'un catalyseur hétérogène - Google Patents

Réacteur pour effectuer des réactions en phase gazeuse au moyen d'un catalyseur hétérogène Download PDF

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Publication number
WO2016055452A1
WO2016055452A1 PCT/EP2015/073015 EP2015073015W WO2016055452A1 WO 2016055452 A1 WO2016055452 A1 WO 2016055452A1 EP 2015073015 W EP2015073015 W EP 2015073015W WO 2016055452 A1 WO2016055452 A1 WO 2016055452A1
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Prior art keywords
reactor
segment
annular space
outer annular
monolith
Prior art date
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PCT/EP2015/073015
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German (de)
English (en)
Inventor
Gerhard Olbert
Carlos TELLAECHE HERRANZ
Roland Bauer
Original Assignee
Basf Se
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Publication of WO2016055452A1 publication Critical patent/WO2016055452A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J8/0207—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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/248—Reactors comprising multiple separated flow channels
    • B01J19/2485—Monolithic reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/248—Reactors comprising multiple separated flow channels
    • B01J19/249—Plate-type reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J8/0285—Heating or cooling the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • 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
    • B01J8/04—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 passing successively through two or more beds
    • B01J8/0403—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 passing successively through two or more beds the fluid flow within the beds being predominantly horizontal
    • B01J8/0423—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 passing successively through two or more beds the fluid flow within the beds being predominantly horizontal through two or more otherwise shaped beds
    • B01J8/0438—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 passing successively through two or more beds the fluid flow within the beds being predominantly horizontal through two or more otherwise shaped beds the beds being placed next to each other
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • 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
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    • B01J8/0492—Feeding reactive fluids
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    • B01J8/04—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 passing successively through two or more beds
    • B01J8/0496—Heating or cooling the reactor
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
    • C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
    • C07C45/33—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of CHx-moieties
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
    • C07C5/32—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with formation of free hydrogen
    • C07C5/327—Formation of non-aromatic carbon-to-carbon double bonds only
    • C07C5/333—Catalytic processes
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    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
    • C07C51/21—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen
    • C07C51/215—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of saturated hydrocarbyl groups
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    • B01J2208/00194—Tubes
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    • B01J2208/00212—Plates; Jackets; Cylinders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01J2208/00477—Controlling the temperature by thermal insulation means
    • B01J2208/00495—Controlling the temperature by thermal insulation means using insulating materials or refractories
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2208/00522—Controlling the temperature using inert heat absorbing solids outside the bed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2208/00805—Details of the particulate material
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2208/022—Plate-type reactors filled with granular catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Definitions

  • Reactor for carrying out gas phase reactions using a heterogeneous catalyst for carrying out gas phase reactions using a heterogeneous catalyst
  • the invention relates to a reactor for carrying out gas phase reactions using a heterogeneous catalyst, which is preferably formed as a monolith, and a use of the reactor.
  • Ceramic or metallic monoliths as catalyst supports in exhaust gas purification or in chemical production engineering are known, and are present as parallelepiped blocks with a plurality of through channels arranged parallel to one another, with a narrow cross section, in the range of about 0.5 to 4 mm.
  • the channels have a low flow resistance at the same time uniform accessibility of the outer catalyst surface for gaseous reaction media. This is advantageous over random heaps, in which a large pressure loss is created by countless deflections in the flow around the particles and the catalyst surface may not be used evenly. Furthermore, there are dead spaces in beds where the gas lingers longer. As a result, by-products and coking are increasingly generated, which deactivate active catalyst areas by deposition and lead to reduced sales and selectivity.
  • the parallelepiped monoliths are usually installed in such a way that the Monolithkanäle are arranged in the longitudinal direction of the cylindrical or prismatic reactor shell.
  • Such, equipped with monoliths reactor is z.
  • an object of the invention to further improve a reactor with internals containing a heterogeneous catalyst, wherein the internals are in particular monoliths.
  • an improved reactor for carrying out heterogeneously catalyzed gas phase reactions which is structurally simple manufacturable, has a high compressive strength and easy accessibility of the internals that carry the catalyst, a simple supply and optionally intermediate feed of educts and easy accessibility Measuring sensors and analytics enabled.
  • an efficient preheating of the educts preferably by recovering the heat from the product gas mixture, is to be ensured.
  • the object is achieved by a cylindrical reactor having a vertical longitudinal axis for carrying out heterogeneously catalyzed gas phase reactions by reacting a gaseous reactant stream to a product gas mixture, with a cylindrical reactor jacket and a concentric inner cylinder, which divides the reactor interior into an outer annular space and a central inner space, wherein outer annulus internals are provided, which contain the heterogeneous catalyst, with a feed line for the gaseous reactant stream in an inlet segment of the outer annulus and with a discharge line for the product gas mixture from an exit segment of the outer annulus, wherein the inlet segment and the exit segment are gas-tightly separated from each other, and wherein a heat exchanger is arranged in the central interior, wherein the gaseous reactant stream is preheated prior to feeding it into the inlet segment.
  • the inventive arrangement of a heat exchanger in the central interior of the reactor it is possible to preheat the reactants with high efficiency, in particular with the product gas mixture, whereby a heat recovery is ensured.
  • the reactor of the present invention is a cylindrical, upright apparatus, preferably with a greater degree of slimming, i. a ratio of height of the reactor to the inner diameter in the range of 0.5 to 3.0, in particular in the range of 0.7 to 1.2.
  • the greater degree of slimming has the advantage of greater compressive strength with the same wall thickness.
  • the reactor has a cylindrical reactor jacket, in which a concentric inner cylinder is inserted, which divides the interior of the reactor into an outer annular space and a central inner space.
  • the outer annulus is the same at both ends, ie, top and bottom, closed by covers.
  • the covers are preferably designed such that they can be easily assembled and disassembled.
  • the reactant stream is fed via a thermally compensated supply line via the inlet segment, preferably in the lower region thereof, to the heat exchanger arranged in the central interior and preheated therein by indirect heat exchange, preferably with the product gas mixture.
  • the heat exchanger may advantageously be designed as a plate heat exchanger.
  • the heat exchanger is designed as a tube bundle heat exchanger. This is advantageously designed so that it does not occupy the entire height of the central interior, but that the tubesheets, in which the heat exchanger tubes are welded in the longitudinal direction of the reactor, are spaced from the respective reactor end, so that in each case a free cylindrical space, a kind of hood , remains.
  • the reactant stream is advantageously fed via a thermally compensated supply line to the lower region of the jacket space of the heat exchanger arranged in the central interior, flows through the same around the tubes of the tube bundle heat exchanger, and leaves the heat exchanger from preheated educt current at the upper end thereof via an opening in the inlet segment.
  • the preheating of the reactant stream in the heat exchanger is preferably carried out by the heat of the product gas mixture, the same from the outlet segment via an opening in the upper region, in the upper hood of the central interior, above the heat exchanger, flows and the tubes flows through it.
  • the product gas mixture leaves the heat exchanger in the central interior via the lower hood and a thermally compensated discharge line via the outlet segment.
  • the inlet segment is free of internals and is a subspace (a chamber), which acts as a pre-distributor, that is, which distributes the gaseous reactant stream over the entire reactor height and thus causes a coarse flow distribution of the same over the reactor height.
  • a further homogenization of the gaseous educt current can preferably be achieved by a rectifier, which is advantageously arranged immediately after the entry segment in the annular space over the entire height thereof.
  • the gaseous reactant stream flows through the complete outer annular space, wherein the gas phase reaction takes place on the heterogeneous catalyst, and the product gas mixture exits the outer annular space via the outlet segment, which closes the outer annular space to the inlet segment and is separated from it gas-tight.
  • the exit segment is, like the entry segment, a subspace (a chamber) in the outer annulus and is a collection device for the product gas mixture over the entire height of the outer annulus.
  • the separation between the inlet segment and the outlet segment can be carried out by means of a partition, which can also be advantageously profiled.
  • the separation between the inlet segment and the outlet segment can be carried out by means of a separation segment, that is to say a separation chamber, with the advantage that feed lines can be laid from outside the reactor directly into the central interior of the reactor via the separation segment, and / or the accessibility of the central interior is made possible from outside the reactor.
  • monolith modules are preferably used as internals containing the heterogeneous catalyst.
  • the channels are preferably formed with a square cross section, in particular with a side length of the square in the range of 0.6 to 3 mm, particularly preferably from 1, 0 to 1, 5 mm.
  • the monoliths are preferably formed from a ceramic material as a carrier material, whereupon a catalytically active layer, preferably by the so-called wash-coating method, is applied.
  • cordierite a ceramic material consisting of magnesium oxide, silica and alumina in the ratio 2: 5: 2.
  • Monolithic ceramic elements are available with cell densities of 25 - 1600 cpsi (cells per square inch, corresponding to a cell size of 5 - 0.6 mm). By using a higher cell density, the geometric surface area increases, so that the catalyst can be used more efficiently. Disadvantages of higher cell densities are a somewhat more difficult manufacturing process, a more difficult washcoat coating and a higher pressure drop across the reactor. Furthermore, as a rule, the webs are also thinner at high cell densities, which reduces the mechanical stability of the monoliths. In cylindrical reactors, the monoliths in the edge area must be adapted by appropriate cutting. However, the pressure loss remains very low for monoliths with high cell density compared to a packed reactor (usually lower by a factor of 10), which is due to the straight Monolithkanäle.
  • a mixture of talc, clay and alumina-providing components and silica may be prepared, the mixture mixed to form a molding compound, the mixture molded, the greenware dried and heated at a temperature of 1200 to 1500 ° C to obtain a ceramic that contains mainly cordierite and has a low coefficient of thermal expansion.
  • the paste usually consists of a mixture of ceramic powders of suitable size, inorganic and / or organic additives, solvent (water), peptizer (acid) to adjust the pH and a permanent binder (colloidal solution or sol).
  • the additives may be a plasticizer or a surfactant to adjust the viscosity of the paste or a temporary binder which may later be burned off. Sometimes glass or carbon fibers are added to increase the mechanical strength of the monolith. The permanent binder should improve the internal strength of the monolith.
  • Cordierite monoliths can be prepared from a batch consisting of talc, kaolin, calcined kaolin and alumina and together form a chemical compound of 45 to 55% by weight of SiO 2, 32 to 40% by weight of Al 2 O 3 and 12 to 15% by weight. - deliver% MgO.
  • Talc is a material consisting mainly of magnesium silicate hydrate, Mg3Si4O10 (OH) 2.
  • the talc may also be mixed with other minerals such as tremolite (CaMg3 (Si03) 4), serpentine (3Mg0.2Si02, 2H20), anthophyllite (Mg7 (OH) 2 (Si401 1) 2), magnesite (MgC03), mica and chlorite.
  • tremolite CaMg3 (Si03) 4
  • serpentine 3Mg0.2Si02, 2H20
  • anthophyllite Mg7 (OH) 2 (Si401 1) 2
  • MgC03 magnesite
  • mica magnesite
  • monoliths of other materials such as SiC, B4C, Si3N4, BN, AIN, Al2O3, ZrO2, mullite, Al titanate, ZrB2, sialon, perovskite, carbon and ⁇ O2 can also be produced.
  • the nature and properties of the materials used to make the moldable mixture are also the additives added, the pH, the water content and the force used in the extrusion.
  • the additives used in the extrusion are, for example, celluloses, CaCl 2, ethylene glycols, diethylene glycols, alcohols, wax, paraffin, acids and heat-resistant inorganic fibers.
  • other solvents can be used, such as ketones, alcohols and ethers.
  • the addition of additives can lead to improved monolithic properties, such as the formation of microcracks, which improves thermal shock resistance, better porosity and absorbency and increased mechanical strength or low thermal expansion.
  • the bare monolithic structure is coated with a catalyst support layer comprising one or more ceramic oxides, or a catalyst layer which already supports the catalytically active metals and the optional further (promoter) elements on the ceramic oxide support material, the coating following a Washcoat coating method is produced.
  • the macroporous structure of ceramic monoliths facilitates the anchoring of the washcoat layer.
  • the manner of washcoat coating can be divided into two methods: one can (partially) fill the macroporous support with the high surface area washcoat material or deposit a washcoat as a layer in the pores of the ceramic carrier. Pore filling leads to the strongest interaction between monolith and washcoat, since most of the washcoat layer is actually fixed in the pores of the carrier and is not bound only to the outer surface of the monolith channels.
  • This type of coating is carried out with a solution (or a sol) of the material to be deposited or with a solution containing very small colloidal particles.
  • the disadvantage of coating by means of pore filling is that the amount of depositable coating is limited, since the pores will eventually be completely filled and the washcoat will become inaccessible.
  • Monoliths offer favorable conditions especially for carrying out the autothermal dehydrogenation of hydrocarbons: in particular, are closer Reactor cross sections and higher flow rates compared to random packed fixed beds feasible, so that an effective, stepped metered addition of oxygen into the hydrocarbon-containing main stream is possible. Due to the fact, compared to randomly packed fixed beds, smaller reactor cross-section, both the distributor and the fixed internals of the mixing zones are mechanically less heavily loaded, ie they hang less because of the lower anchoring length. Moreover, the main flow direction through the reactor is not limited to downflow, as in the case of randomly packed fixed beds.
  • the presently recommended catalysts can normally be regenerated in a simple manner, for example by initially air in first regeneration stages, which is (preferably) diluted with nitrogen and / or water vapor, at an inlet temperature of 300 to 600 ° C. (in extreme cases up to 750 ° C), often from 500 to 600 ° C, passes through the fixed catalyst bed.
  • the catalyst loading with regeneration gas may be, for example, 50 to 10,000 h-1 (based on the total amount of regenerated catalyst), and the oxygen content of the regeneration gas may be 0.5 to 20% by volume.
  • monolith modules are provided, which are formed of monoliths with horizontally arranged substantially along concentric circles channels, which are arranged in each case to two, three or more, along each reactor radius adjacent to a row and wherein two, three or more rows of monoliths are stacked on top of each other, each monolithic module being circumferentially encased in one or more fibrous mats, and over the same in a metal sheath, leaving the end faces free of entrance or exit openings of the channels in which each monolith module (MM) completely fills the outer annulus in the radial direction, wherein in each case two or more monolith modules are combined one above the other to form planar packing units arranged radially in the annulus of the reactor, and one, two or more packing units each fill a segment in the outer annulus of the reactor over its entire height and form a catalytically active zone.
  • monolith modules are provided, which are formed of monoliths with horizontally arranged substantially along concentric circles channels, which are arranged in each case to two, three or more
  • Monoliths are more preferably provided as internals containing the heterogeneous catalyst, which are formed of monoliths having horizontally arranged substantially along concentric circles channels, each of which is arranged to four or more, along a respective reactor radius side by side to a row and wherein four or more rows of monoliths are stacked on top of each other, wherein each monolithic module is encased in one or more fibrous mats and over the same in a metal sheath over the periphery thereof, leaving the end faces containing the entrance or exit openings of the channels, each one Monolith module completely fills the outer annulus in the radial direction, wherein in each case two or more monolith modules are summarized one above the other to planar packing units, which are arranged radially in the outer annulus of the reactor, and wherein one, two or more packing units each fill a segment in the annular space of the reactor over its entire height and form a catalytically active zone.
  • monolith modules are provided, which are formed of monoliths with horizontally arranged substantially along concentric circles channels, each of eight or more, are arranged side by side along each reactor radius and eight or more rows of monoliths are stacked on top of each other, wherein each monolith module is enclosed in the circumference of the same, leaving the end faces, the inlet or outlet openings of the channels in one or more fibrous mats and the same in a metal shell, wherein each monolith module the outer annular space in the radial direction completely fills, wherein in each case two or more monolith modules are summarized one above the other to planar packing units, which are arranged radially in the outer annulus of the reactor, and wherein one, two or more flat Packu ngshimen each fill a segment in the annular space of the reactor over the entire height thereof and form a catalytically active zone.
  • Each monolith module fills the outer annulus in the radial direction of the same completely.
  • the individual monoliths in the respective monolith modules are to be protected from damage by thermal expansion parallel to the flow direction with fibrous mats.
  • each monolithic module over the circumference of the same, leaving free the end faces, the inlet and outlet openings of the channels included, enclosed in one or more fibrous mat and above in a metal shell.
  • the inlet and outlet openings of the channels included, enclosed in one or more fibrous mat and above in a metal shell.
  • the fiber-containing mats used in the present case are sheets with two opposing large surfaces and two end faces arranged perpendicular thereto.
  • the fibrous mats may preferably be flattening, d. H. Inflatable mats, which expand (swell) at high temperatures.
  • Blähmatten are usually made of silicates, z. For example, aluminum silicate, - or Aluminiumoxidsilikatmaschinen a Blähschiefer, z. As vermiculite, and an organic binder. Blähmatten be marketed for example by the company 3M under the trade name INTERAM®. Furthermore, 3M mats are still made of polycrystalline fibers suitable for high temperature applications.
  • the organic binders have a number of disadvantageous properties under the first temperature control up to the operating temperature, in particular they lead to the odor nuisance by evaporation of volatile components, such as for the poisoning of catalysts. Therefore, it is particularly important that the Blähmatten or fiber mats are brought quickly, preferably in a separate process step in the use state.
  • inflatable mats are increasingly having a lower content of organic binders, from previously about 12 to 14 wt .-%, to now about 2 to 5 wt .-%, in particular 3 to 4 wt .-% organic binder, based on the Total weight of the inflatable mat, required.
  • the Blähmatten be crumbly, but less consistent plastically deformable in the consistency and less manageable and difficult to process during cold processing.
  • the lateral scanning of the mats between the monoliths is added to the rectangular scanning.
  • the metal shell is advantageously formed from a material which is mechanically and chemically stable at the high temperature of the reaction temperature, often in the range of about 400 to 700 ° C, and has no catalytic activity for the heterogeneously catalyzed gas phase reaction, that is no reaction initiated with the reaction gas.
  • the metal shell is preferably formed of a material which has a low coefficient of thermal expansion and is heat-resistant.
  • two or more monolith modules are grouped together to form planar packing units, which are arranged radially in the outer annular space of the reactor and extend over the entire height thereof.
  • a packing unit thus has the shape of a flat cuboid whose length corresponds to the height of the outer annular space whose width corresponds to the radial extent of the outer annular space and whose thickness corresponds to the extent of a single monolith in the direction of the channels thereof.
  • One, two or more packing units each fill a segment in the outer annulus of the reactor and form a catalytically active zone.
  • spacers may be provided between each two successive flat packing units.
  • Two or more flat packing units are advantageously each inserted into preferably U-shaped guide rails, and thus can be exchanged in a simple manner by removing the corresponding upper and / or lower cover of the outer annular space.
  • a supply line for an additional gas and a mixing device is provided.
  • the internals containing the heterogeneous catalyst may be formed as screen baskets filled with particulate heterogeneous catalyst.
  • suitable sites, bays for receiving inert material and / or heat exchange devices can be provided in the outer annulus.
  • reactor jacket can be, in a simple manner, at any required location, facilities for measuring sensors and analysis in the outer annulus introduce and monitor the reaction processes precisely, in a simple manner.
  • measuring elements for determining temperatures and / or concentrations which are introduced into the outer annular space from outside the reactor, can be provided between each two packing units.
  • the reactor can be easily isolated from the inside with respect to the central interior and from the outside by its simple form.
  • the outer annulus, both to the reactor shell and to the central interior provided with a thermal insulation.
  • the thermal insulation can be carried out in one or more layers, preferably the thermal insulation which faces the outer annular space, namely both the thermal insulation applied to the inner wall of the reactor jacket and the inner cylinder, is formed from a microporous material.
  • a further layer can preferably be provided, which isolates to the outside in the reactor jacket, as well as a layer which insulates the inner cylinder toward the central inner space.
  • rock wool can be used.
  • the thermal inertia of the cylinder bounding the outer annular space is lower, so that a faster switching between process sections with different temperature levels, as occur, for example, in autothermal gas phase dehydrogenations, for example in butane dehydrogenation, are advantageous.
  • the microporous insulation material may be mounted in cassettes, for example;
  • the individual cassettes are assembled and gas-tight sealed by a thin sheet against the outer annulus, so that the hot reaction gases are not to the two, the outer annulus limiting cylinder, d. H. the reactor jacket and the inner cylinder, can pass.
  • the arranged in the central interior heat exchanger is in a preferred embodiment, a plate heat exchanger.
  • the heat exchanger arranged in the central interior is a tube bundle heat exchanger.
  • the shell-and-tube heat exchanger is arranged in the central interior, preferably in such a way that it does not assume its entire height, but that Above and below the tubesheets, in which the tubes of the tube bundle heat exchanger are welded, each free cylindrical spaces, the type of hoods, remain free.
  • the reactant stream to be heated is introduced into the shell space of the tube bundle heat exchanger and flows through it from bottom to top, in cross-countercurrent to a heat carrier, which is passed through the tubes of the tube bundle heat exchanger from top to bottom.
  • the hot product gas mixture is preferably used as the heat carrier.
  • the cylindrical reactor shell is integrated in a pressure-bearing cylindrical housing, wherein a gap is preferably provided between the cylindrical reactor shell and the pressure-bearing cylindrical housing.
  • the cylindrical pressure-bearing housing can be made with a smaller wall thickness. This is particularly advantageous in a reaction regime in which capacitive influences play a role, for example in autothermal gas phase dehydrogenations, which comprise process steps at different temperature levels.
  • the outer, pressure-bearing cylindrical shell can be designed with lower wall thickness and yet meets the required strength values, their thermal inertia is lower, which leads to corresponding advantages, in particular time saving, in a process management with different temperature levels.
  • the space between the reactor shell and the outer pressure-bearing housing is preferably purged with an inert gas, in particular with nitrogen or water vapor.
  • the invention also relates to the use of the reactor described above for carrying out endothermic, exothermic or adiabatic, heterogeneously catalyzed gas phase reactions.
  • the reactions may be preferably dehydrogenations, in particular autothermal gas phase dehydrogenations, preferably of n-butane, isobutane, n-propane, butene or ethylbenzene, or else oxidations, in particular to acrolein, methacrolein, acrylic acid, methacrylic acid, phthalic anhydride or maleic anhydride or hydrogenations, in particular of maleic anhydride to Tetra hydrofu ran.
  • the inventive arrangement of a heat exchanger in the central interior of the reactor a preheating of the reactants with high efficiency is possible, in particular by indirect heat exchange with the product gas mixture, whereby a heat recovery is ensured.
  • the temperature level generated by the heat of reaction in the outer annulus leads to much higher temperatures in the central interior space than outside the reactor.
  • Figure 2 is a longitudinal section through a further preferred
  • Figure 3A shows a cross section through an advantageous
  • Figure 5 is a cross-section through a further preferred
  • FIG. 5A see above
  • Figures 6A and 6B are longitudinal sectional views through the reactor shown in Figure 5, in the plane B-B (in Figure 6A) and with illustration A-A '(in Figure 6B);
  • Figures 7A and 7B are longitudinal sectional views through a further preferred
  • FIG. 1 shows a section in the plane AA 'by a preferred embodiment of a reactor according to the invention R, with a cylindrical reactor shell RM and a concentric inner cylinder I, the reactor interior in an outer annulus RR and a central interior IR split, wherein in the sectional view in Figure 1 from the outer annulus RR the entry segment ES and the exit segment AS are visible.
  • a gaseous reactant stream is introduced through the inlet segment ES into the jacket space of the heat exchanger W arranged in the central interior IR, flows through it around the tubes, is deflected by baffles, and finally leaves the heat exchanger W at the upper end thereof an opening in the inlet segment ES of the outer annular space RR, to be guided from here to the non-representable in the figure internals containing the heterogeneous catalyst.
  • the product gas mixture leaves the outer annular space RR via the outlet segment AS, via an opening in the upper region thereof, and enters into the hood above the heat exchanger W in the central interior IR, flows into the tubes of the heat exchanger W, heated by indirect heat exchange the educt current and finally leaves the heat exchanger W via the lower hood in the central interior IR and the thermally compensated discharge line 2 through the exit segment AS.
  • the upper and the lower cover of the central inner space IR are advantageously detachable, so that accessibility to the heat exchanger W, for example for maintenance purposes, is ensured.
  • Figure 2 shows a section in the plane A-A 'by another embodiment of the reactor R shown in longitudinal section in Figure 1, wherein the reactor on all sides has a thermal insulation IS to reduce heat loss.
  • FIG. 3 shows a cross section through the preferred embodiment of a reactor R according to the invention shown in FIG. 2, with a cylindrical reactor jacket RM and a concentric inner cylinder I which divide the reactor interior into an outer annular space RR and a central inner space IR, wherein outer annular space RR internals are provided, which are formed in the preferred embodiment shown in the figure as monoliths M, wherein in the radial direction by way of example six monoliths are arranged.
  • section BB As can be seen from the longitudinal section in FIG. 4 (section BB), several rows of monoliths M are stacked one above the other in each case for a monolith module MM and by way of example, 7 monolith modules MM are stacked on top of each other, forming a flat packing unit P in each case.
  • a gaseous reactant stream is first introduced into the shell space of the heat exchanger W in the central interior IR and then flows into the inlet segment ES of the outer annulus RR is equalized via the flow rectifier G and flows through the arranged in the outer annulus RR internals, the contain heterogeneous catalyst, and which are formed in the preferred embodiment shown in Figure as monoliths M, which are summarized to monolith modules MM.
  • the monolith modules MM are inserted into guide rails F, which are arranged on the walls of the reactor jacket RM and of the inner cylinder I facing the outer annular space RR.
  • the reaction gas mixture flows through the complete outer annular space RR, which in the preferred embodiment shown in FIG. 3 comprises three catalytically active zones Z, flows through an opening in the upper region as exit segment AS into the upper hood space, flows through the tubes from top to bottom into the lower hood space Dome space and leaves the same via the discharge line 2 through the exit segment AS, which, in the preferred embodiment shown in the figure by a partition T is separated from the inlet segment.
  • Additional feed gas is fed via three feed lines 3, whereby after each feed line 3 a mixing device EV is arranged in each case.
  • FIG. 3A shows a cross section through a further improved embodiment of the reactor R shown in FIG. 3, wherein additionally a fuel gas feed line BG is provided in the entry segment ES.
  • FIG. 4 shows a longitudinal section B-B through the preferred embodiment of a reactor R according to the invention shown in cross-section in FIG. 3.
  • the section B-B is laid through monolith modules MM and illustrates their expansion in the longitudinal direction of the reactor, forming a flat packing unit P.
  • FIG. 5 shows a longitudinal section through a further improved embodiment of the reactor shown in cross-section in FIG. 3, wherein the reactor jacket RM having an insulation IS is in a pressure-bearing cylindrical jacket Housing D is wrapped, which also has an insulation IS, with a gap between the reactor jacket RM and the pressure-carrying cylindrical housing D, which is flushed by an inert gas.
  • FIG. 5A shows a cross section through a further improved embodiment of the reactor R shown in FIG. 5, wherein additionally a fuel gas feed line BG is provided in the inlet segment ES.
  • FIGS. 7A and 7B show sectional views in the plane AA 'for the reactor R shown in cross-section in FIG. 5A, each with different embodiments for the fuel gas supply BG, this being designed as a tube with a multiplicity of openings in FIG FIG. 7B as a dip tube, followed by static mixers.

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Abstract

L'invention concerne un réacteur cylindrique (R) à axe longitudinal vertical utilisé pour effectuer des réactions en phase gazeuse à catalyse hétérogène par réaction d'un flux de substance de départ sous forme gazeuse en un mélange de produits gazeux, ledit réacteur présentant une enveloppe de réacteur (RM) cylindrique et un cylindre intérieur (I) concentrique qui divise l'espace intérieur du réacteur en un espace annulaire extérieur (RR) et en un espace intérieur central (IR), des éléments intégrés étant prévus dans l'espace annulaire extérieure (RR), qui contiennent le catalyseur hétérogène. Ledit réacteur comporte également une conduite d'alimentation (1) pour le flux de substance de départ sous forme gazeuse dans le segment d'entrée (ES) de l'espace annulaire extérieur (RR) ainsi qu'une conduite d'évacuation (2) pour le mélange de produits gazeux provenant d'un segment de sortie (AS) de l'espace annulaire extérieur (RR), le segment d'entrée (ES) et le segment de sortie (AS) étant séparés l'un de l'autre de manière étanche aux gaz et un échangeur de chaleur étant disposé dans l'espace intérieur central (I), échangeur de chaleur dans lequel le flux de substance de départ sous forme gazeuse est préchauffé avant d'être acheminé dans le segment d'entrée (ES).
PCT/EP2015/073015 2014-10-07 2015-10-06 Réacteur pour effectuer des réactions en phase gazeuse au moyen d'un catalyseur hétérogène WO2016055452A1 (fr)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10576449B2 (en) 2015-12-16 2020-03-03 Basf Se Reactor for carrying out heterogeneously catalysed gas phase reactions, and use of the reactor
US10618873B2 (en) 2016-02-01 2020-04-14 Basf Se Method for producing C4-C15 lactams
CN111821921A (zh) * 2020-06-27 2020-10-27 淮阴工学院 一种氯甲烷反应塔的进气装置
US10974964B2 (en) 2015-11-27 2021-04-13 Basf Se Modular catalyst monoliths

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US3954417A (en) * 1974-08-20 1976-05-04 General Motors Corporation Monolithic catalytic converter with central flow tube
US4372920A (en) * 1979-07-13 1983-02-08 Ammonia Casale S.A. Axial-radial reactor for heterogeneous synthesis
DE10031347A1 (de) * 1999-06-28 2001-01-04 Basf Ag Reaktor mit Wärmetauscherplatten
US20100288704A1 (en) * 2009-05-12 2010-11-18 Jeffrey Michael Amsden Flow-Through Substrate Assemblies and Methods for Making and Using Said Assemblies
WO2011067235A1 (fr) * 2009-12-01 2011-06-09 Basf Se Réacteur pour la mise en œuvre de déshydrogénations autothermiques en phase gazeuse
JP2011207704A (ja) * 2010-03-30 2011-10-20 Jx Nippon Oil & Energy Corp 水素製造装置及び燃料電池システム
WO2014090841A2 (fr) * 2012-12-12 2014-06-19 Basf Se Réacteur pour la réalisation d'une déshydrogénation autothermique en phase gazeuse

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Publication number Priority date Publication date Assignee Title
US3954417A (en) * 1974-08-20 1976-05-04 General Motors Corporation Monolithic catalytic converter with central flow tube
US4372920A (en) * 1979-07-13 1983-02-08 Ammonia Casale S.A. Axial-radial reactor for heterogeneous synthesis
DE10031347A1 (de) * 1999-06-28 2001-01-04 Basf Ag Reaktor mit Wärmetauscherplatten
US20100288704A1 (en) * 2009-05-12 2010-11-18 Jeffrey Michael Amsden Flow-Through Substrate Assemblies and Methods for Making and Using Said Assemblies
WO2011067235A1 (fr) * 2009-12-01 2011-06-09 Basf Se Réacteur pour la mise en œuvre de déshydrogénations autothermiques en phase gazeuse
JP2011207704A (ja) * 2010-03-30 2011-10-20 Jx Nippon Oil & Energy Corp 水素製造装置及び燃料電池システム
WO2014090841A2 (fr) * 2012-12-12 2014-06-19 Basf Se Réacteur pour la réalisation d'une déshydrogénation autothermique en phase gazeuse

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10974964B2 (en) 2015-11-27 2021-04-13 Basf Se Modular catalyst monoliths
US10576449B2 (en) 2015-12-16 2020-03-03 Basf Se Reactor for carrying out heterogeneously catalysed gas phase reactions, and use of the reactor
US10618873B2 (en) 2016-02-01 2020-04-14 Basf Se Method for producing C4-C15 lactams
CN111821921A (zh) * 2020-06-27 2020-10-27 淮阴工学院 一种氯甲烷反应塔的进气装置

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