WO2011045051A1 - Système de réacteurs pour oxydation en phase gazeuse catalytique - Google Patents

Système de réacteurs pour oxydation en phase gazeuse catalytique Download PDF

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Publication number
WO2011045051A1
WO2011045051A1 PCT/EP2010/006268 EP2010006268W WO2011045051A1 WO 2011045051 A1 WO2011045051 A1 WO 2011045051A1 EP 2010006268 W EP2010006268 W EP 2010006268W WO 2011045051 A1 WO2011045051 A1 WO 2011045051A1
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Prior art keywords
reactor
catalyst
catalytically active
porous support
arrangement according
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PCT/EP2010/006268
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German (de)
English (en)
Inventor
Hans-Jörg WÖLK
Gerhard Mestl
Harald Dialer
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Süd-Chemie AG
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Publication of WO2011045051A1 publication Critical patent/WO2011045051A1/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
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
    • 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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/14—Phosphorus; Compounds thereof
    • B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J27/195—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium or tantalum
    • B01J27/198—Vanadium
    • 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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/20—Carbon compounds
    • B01J27/22—Carbides
    • B01J27/224—Silicon carbide
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61—Surface area
    • B01J35/613—10-100 m2/g
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • B01J37/0203—Impregnation the impregnation liquid containing organic compounds
    • 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • C—CHEMISTRY; METALLURGY
    • 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
    • C07C51/255—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting
    • C07C51/265—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with molecular oxygen of compounds containing six-membered aromatic rings without ring-splitting having alkyl side chains which are oxidised to carboxyl groups
    • C—CHEMISTRY; METALLURGY
    • 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
    • C07C51/31—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation of cyclic compounds with ring-splitting
    • C07C51/313—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation of cyclic compounds with ring-splitting with molecular oxygen

Definitions

  • the present invention relates to a reactor arrangement consisting of a main reactor and a post-reactor, wherein the post-reactor contains at least one catalyst and wherein the catalyst comprises a porous support having a solid SiC sponge, wherein on the porous support
  • the present invention relates to
  • Phthalic anhydride by gas phase oxidation Furthermore, the invention relates to a method for producing the
  • Olefins, or (alkyl) aromatics performed.
  • the production of phthalic anhydride is carried out by
  • a suitable catalyst for each reaction in a reactor preferably a so-called tube bundle reactor, filled and from above or below with a mixture of the hydrocarbon and an oxygen-containing gas, for example air, flows through.
  • hot spots Preventing so-called hot spots ("hot spots") with a heat transfer medium to rinse and the resulting hot spots
  • a heat transfer medium As a heat transfer medium is usually used a molten salt, preferably a eutectic mixture of NaN0 2 and K 0 3rd Likewise one can oppress the molten salt, preferably a eutectic mixture of NaN0 2 and K 0 3rd Likewise one can oppress the molten salt, preferably a eutectic mixture of NaN0 2 and K 0 3rd Likewise one can oppress the
  • coated catalysts As catalysts, so-called coated catalysts have been proven. This is an inert non-porous carrier made of quartz (Si0 2 ), magnesium silicate (steatite), silicon carbide (Sic),
  • Tin oxide, porcelain, etc. which has a shape and expression suitable for the particular reactor used, e.g. Spheres, rings, extrudates, spirals, stars coated with one or more layers of catalytically active mass.
  • Yield of the desired oxidation product here has the task to raise these layers of the active catalysts highly uniformly and homogeneously on all carrier particles.
  • various apparatuses are described for this purpose.
  • organic and often inorganic binders are used in mounting the catalyst layers in such devices.
  • binders are various organic
  • Adhesive e.g. Vinyl acetate / ethylene adhesive.
  • Alkyl aromatics is a variety of different catalysts known. These are often catalyst systems containing as one of the catalytically essential constituents of the oxides of vanadium and titanium. Such
  • Catalysts are described, for example, in EP 0964744 B1. Usually, a variety of promoter elements are used to increase the productivity of these
  • Catalyst systems leads.
  • Such promoters include, among others, the alkali, alkaline earth metals, thallium, antimony, phosphorus, iron, niobium, cobalt, molybdenum, silver, tungsten, tin, zirconium, lead and bismuth (A. Bielanski et al., Ap. Catal. A: Gen. 157, 223 (1997)).
  • JP 2006-000850 describes the use of porous
  • a porosity of the carrier between 16 and 20% is disclosed as particularly advantageous, since at a higher porosity, for example of more than 35%, undesired reactions occur on the surface of the carrier. The same problem occurs when the surface of the carrier is greater than 0.3 m 2 / g.
  • PSA phthalic anhydride
  • Multi-layer catalyst systems used.
  • the aim here is to adapt the activity of the individual catalyst layers to the course of the reaction along the reactor axis. This makes it possible to obtain a high yield of PSA and at the same time the lowest possible yield of undesired intermediates, e.g.
  • downstream post-reactors also called post reactors
  • the catalysts serve To remove suboxidation products from the reaction gas or to further convert to product and to convert secondary oxidation products to C0 2 and thus to increase the product purity.
  • the loading of the main reactor with organic starting material can be further controlled by the design of the
  • the postreactors can be honeycomb catalysts, as described in the
  • EP 1 181 097 A1 are described.
  • the catalysts can also be applied to ceramic rings.
  • the support of the catalytically active material on ceramic rings has the disadvantage that it causes the back pressure in
  • honeycomb bodies have the disadvantage that they are used for so-called "runaway"
  • Reaction gas in the channels a rise in temperature and the channel ignites.
  • various catalyst layers in the reactor with regard to their function optimized (activity, selectivity, layer length).
  • the layer thicknesses of the catalytically active Layers on the non-porous, ceramic support structures are precisely controlled.
  • Product is also the life or service life of the product
  • An object of the present invention is therefore to provide a post-reactor which does not generate a high back pressure in the main reactor. Furthermore, no laminar flows, for example in honeycomb bodies, should be set in the after-reactor in order to suppress the diffusion limitation.
  • Carrier sponge have a homogeneous layer thickness and within the catalyst layer must not express micropores, whereas acropores are desirable. Excessive layer thicknesses and micropores lead to diffusion limitation and
  • the carrier of the post-catalyst should be able to exothermic by a high thermal conductivity
  • Another object of the invention was to provide a
  • this object is achieved by a reactor arrangement consisting of a
  • a main reactor and a post-reactor wherein the post-reactor comprises at least one catalyst, wherein the catalyst comprises a porous support having a solid Sic sponge, wherein on the porous support, a catalytically active composition is applied, which contains Ti0 2 and at least one transition metal oxide, and wherein the TiO 2 used has a bulk density of less than 1.0 g / ml.
  • Post-reactors in contrast to the known post-reactors comprising, for example, catalysts with honeycomb bodies or ceramic support bodies, an uncontrolled "runaway" of the reactors and an increased back pressure in the main reactor can be avoided.
  • Mass is applied, the Ti0 2 and at least one
  • Transition metal oxide wherein the Ti0 2 has a bulk density of less than 1.0 g / ml, the best catalytic
  • the adiabatic temperature increase (hot spot) in the postreactor is lower because the course of the reaction spreads over a larger volume range of the postreactor and thus the reactor can be operated more easily. Due to the thus improved temperature control can be achieved with improved quality of the product with the post-reactors according to the invention, compared to known post-reactors, a higher product yield.
  • no depletion zones are formed in the post-reactor according to the invention, as in the laminar gas streams of the honeycomb body channels.
  • Pore structure is designed as uniform as possible within the catalyst layers. This allows for a better one
  • a uniform pore structure can be
  • Polystyrene sponges are used.
  • the postreactor according to the invention contains at least one
  • a catalyst wherein the catalyst comprises a porous support having a solid SiC sponge, wherein on the porous support, a catalytically active composition is applied, which contains Ti0 2 and at least one transition metal oxide, and wherein the used Ti0 2 has a bulk density of less than 1.0 g / ml.
  • a "post-reactor" in the context of the present invention is a reactor downstream of the main reactor, which is the in the
  • Downstream thus means that the reaction gas first the main reactor and then in the secondary reactor
  • the postreactor has a reaction space which is charged with catalyst. In contrast, show
  • Main reactor usually containing bulk catalysts charged tube bundles are preferably used in the novel reactor according to catalysts with monolithic carriers comprising SiC sponges. Postreactors are therefore not tube reactors.
  • inventive features are therefore not tube reactors.
  • the reactors are used for the catalytic gas-phase oxidation of organic compounds, in particular of aliphatics, olefins, or (alkyl) aromatics.
  • the postreactor according to the invention can have any desired construction.
  • it may be attached to the main reactor, such as a shell and tube reactor, as a "piggyback reactor.”
  • the catalyst (s) of the postreactor are conventionally incorporated into the reactor so as to optimally contact the reaction gas It is preferred to use a hexagonal post-reactor, in which case it is preferable to use the carrier with a triangular cross-section
  • the postreactor according to the invention comprises at least one, more preferably at least two, even more preferably at least three, different catalyst (s).
  • the catalysts comprise a porous support of a single monolithic support body or of two or more separate support bodies, which are preferably fixedly or movably connected to one another. If the
  • Catalyst consists of two or more separate carrier bodies, it is particularly preferred that between the individual carrier body is at least partially not filled with carrier material space.
  • the term "catalyst” as used herein refers to a porous carrier having thereon
  • Two different catalysts differ in the properties of the porous supports and / or the properties of the catalytically active material. Between the various catalysts may be at least partially not filled with carrier material space, the catalysts are optionally fixed or movable together.
  • the main reactor has at least one first catalyst layer located toward the gas inlet side, a second one located closer to the gas outlet side
  • Catalyst layer is higher than the catalyst activity of the second catalyst layer.
  • Particularly suitable multilayer catalysts for the main reactor are described, for example, in WO 2006/092304.
  • the BET surface area increases from the first to the gas inlet side
  • Preferred BET surface areas are 15 to 25 m 2 / g for the first
  • the Ti0 2 used (anatase modification) has a content of alkali in all catalyst layers,
  • the proportion of Na in particular to Na of less than 0.3 wt .-%, in particular less than 0.2 wt .-%, preferably less than 0.15 wt .-%, more preferably less than 0.02 wt .-% and am most preferably less than 0.015% by weight.
  • the above limits for Na and K. apply.
  • Alkali impurities (total alkali content) of the TiO 2 used determined as the sum of the lithium, sodium, potassium, rubidium and cesium impurities, less than 1000 ppm, in particular less than 500 ppm, more preferably less than 300 ppm.
  • a method for determining the proportion of alkali impurities of the Ti0 2 used is carried out in accordance with DIN ISO 9964-3.
  • the preferred total alkali content allows a more accurate adjustment of the alkali promoter content of the
  • the post-reactor catalysts used according to the invention comprise "porous supports" on which a catalytically active composition is applied
  • the Cells have adjacent to all spatial directions
  • the cells can ideally be described as pentagonal dodecahedra whose edges form the webs of the lattice structure.
  • Pentagon dodecahedron is theoretically 1.6.
  • supports with honeycomb structures, channel structures or cross-channel structures in post-reactors have hitherto been used.
  • the porous support of the catalyst according to the invention therefore preferably has no honeycomb structure or cross-channel structure and preferably has fractal or non-ordered, open pore structures.
  • the porous support is preferably more than 90% by weight, more preferably more than 95% by weight, even more preferably more than 97% by weight, and most preferably at least 99% by weight of silicon carbide .
  • the silicon carbide content can be determined by X-ray diffractometry in the usual way.
  • Suitable Sic sponges are, for example, silicon carbide ceramic composite sponges.
  • the porous support is a pure silicon carbide sponge.
  • the porous carrier of the postreactor preferably has no honeycomb structure or cross channel structure. More preferably, the porous support has fractal or non-ordered structures. Whether a fractal structure is present can be determined by the method described in WO2005 / 003758.
  • the porous support may be cylindrical, cube-shaped, cuboid, prismatic, or any other suitable form or
  • the porous Carrier on a cylindrical shape.
  • the dimensions (height, length,
  • Width of the porous supports are preferably between 0.5 cm and 30 cm, in particular 10 cm and 30 cm, more preferably between 10 cm and 20 cm, and more preferably between 10 cm and 15 cm.
  • the compression strength of the porous supports is more than 0.2 MPa. The determination of the compression strength is described below in the Methods section.
  • the pore volume of the porous support is between 0.01 cm 3 / g and 0.6 cm 3 / g for pores having a
  • the porous support preferably has a density of the open macroporous structure (channel system) of 1-100 ppi (pores per inch), preferably 10-50 ppi.
  • the porous support has open pore structures with an open pore diameter between 500 ⁇ m and 5 mm, more preferably between 800 ⁇ m and 5 mm, more preferably between 0.9 mm and 5 mm, even more preferably between 2 mm and 5 mm and most preferably between 3 mm and 5 mm, on.
  • the SiC sponge is further characterized by cell diameters of 0.1 to 10 ⁇ m,
  • the specific surface area of the porous support according to BET is preferably 1-20 m 2 / g, more preferably 1-10 m / g, even more preferably between 1-5 m 2 / g.
  • the determination of the BET surface area is described in the Methods section.
  • the porous support has an apparent density between 0.05 and 0.5 g / cm 3 , more preferably between 0.14 and 0.36 g / cm 3 and most preferably from 0.1 to 0.4 g / cm 3 up.
  • the determination of the apparent density of the support is described below in the Methods section.
  • the calculation of the apparent density of the porous support is based on the total volume of the porous support minus the open pores
  • porosity refers to the open porosity of the support, i. only the open pores, which are accessible to the reaction gas and are decisive for the catalytic properties, are considered.
  • Subsequent reactor has a porosity of 70 to 98%, more preferably between 70 and 95%, more preferably between 80 and 95%, more preferably between 85 and 95% and even further
  • porous supports Preparation of porous supports is known to the person skilled in the art. The preparation of porous supports having the properties according to the invention is described below. Here, for example, of silicon powder and
  • Phenol resins / polyurethane sponges are assumed.
  • Suitable production methods are, for example, in
  • the SiC sponges according to the invention preferably consist of ⁇ -silicon carbide.
  • Pulverdiffraktometrie be determined in the usual way.
  • the catalytically active composition which is applied to the porous support of the postreactor according to the invention is described below.
  • This catalytically active mass of the catalyst of the post-reactor can also be used for the catalyst of the main reactor.
  • any TiO 2 modification can be used, with TiO 2 in the anatase form being preferred.
  • the TiO 2 used has a BET surface area of at least 15 m 2 / g, preferably between 15 and 60 m 2 / g, in particular between about 15 and 45 m 2 / g and particularly preferably between 15 and 40 m 2 / g on.
  • Pores with a radius of more than 400 nm are preferably less than about 30%
  • the TiO 2 used has the following particle size distribution:
  • the Dio value is preferably 0.5 ⁇ or less; the D 50 value (ie the value at which each half of the
  • Particle has a larger or smaller particle diameter) is preferably at 1.5 ⁇ or less; of the
  • D 90 value is preferably 4 pm or below.
  • the D 90 value of the TiO 2 used is preferably between about 0.5 and 20 ⁇ , in particular between about 1 and 10 ⁇ , more preferably between about 1 and 5 ⁇ .
  • the Ti0 2 used in the invention preferably has an open-pored, sponge-like structure, wherein primary particles or crystallites to more than 30%, in particular more than 50%, to open porous
  • TiO 2 having a primary crystallite size (primary particle size) of more than at least 210 angstroms to at most 900 angstroms, preferably more than at least 250 angstroms to at most 600 angstroms, more preferably more than at least 300
  • Angström to at most 500 angstroms, in particular more than at least 350 angstroms and most preferably more than at least 390 angstroms used.
  • Primary crystallites having this preferred primary crystallite size enable the preparation of particularly advantageous catalysts by allowing the formation of a not too compact but open-pored structure of the titanium dioxide in the catalyst.
  • a method for determining the primary crystallite size is a method for determining the primary crystallite size.
  • TiO 2 is used with a bulk density of less than 0.8 g / ml, more preferably less than 0.6 g / ml.
  • TiO 2 having a bulk density of not more than 0.55 g / ml. The lower the bulk density of the Ti0 2 used , the better the structure of the catalyst in the
  • the TiO 2 used has a particle size distribution with a Di 0 value of at most 0.5 ⁇ m and / or a D 50 value of
  • the D 90 value of the TiO 2 used is between 0.5 and 20 ⁇ m, in particular between 1 and 10 ⁇ m, particularly preferably between 2 and 5 ⁇ m.
  • the TiO 2 is particularly preferably present in the anatase modification.
  • the catalytically active composition comprises at least one transition metal oxide selected from the group consisting of vanadium oxide, antimony oxide, chromium oxide, niobium oxide, tantalum oxide, molybdenum oxide, tungsten oxide, manganese oxide, iron oxide or their atomic mixtures;
  • the catalytically active composition particularly preferably comprises at least vanadium oxide as the transition metal oxide.
  • the catalytically active composition contains at least one, more preferably at least two, and most preferably at least three of the aforementioned transition metal oxides.
  • the transition metal oxides V 2 0 5 and / or Sb 2 0 3 preferably V 2 0 5 and Sb 2 0 3 are used. Preferably, this is
  • Titanium dioxide of anatase modification from 1 to 30% by weight
  • the catalyst is layered, wherein the actual carrier oxide Ti0 2 is coated with a monoatomic to several atomic layers thick layer of one or more of the aforementioned transition metal oxides.
  • the catalytically active composition contains at least one promoter.
  • the promoter is preferred
  • P selected from the group consisting of P, Sb, Bi, Li, Cs, Sr, Ba, Ni, Co, Fe, b, Mo, W, Sn and noble metals selected from the group consisting of Cu, Ag, Au, Pt, Pd , and Rh.
  • the catalytically active composition comprises at least one, more preferably at least two, and most preferably at least three of the above-mentioned promoters.
  • promoters By using promoters, the activity and selectivity of the catalysts can be influenced, in particular by
  • Selectivity increasing promoters include, for example, the alkali metal oxides and oxidic phosphorus compounds,
  • the components of the catalytically active composition are preferably used in the following amounts (see Table 1).
  • the components not listed in the table are preferably used in proportions of between 1 and 10% by weight, more preferably between 1 and 7% by weight, more preferably between 1 and 2% by weight. Table 1.
  • the remainder of the catalytically active material is TiO 2 . More preferably, the catalytically active composition is at least 70 wt .-%, more preferably at least 80 wt .-%, even more preferably at least 90 wt% of Ti0 second In a preferred
  • the active composition comprises 80-90 wt .-% Ti0 2 , 9.5-19.9 wt .-% V 2 0 5 and 0.1 - 0.5 wt .-% P, more preferably consists of the active composition of the abovementioned constituents.
  • the active composition comprises 80-90 wt .-% Ti0 2 , 9.5-19.9 wt .-% V 2 0 5 and 0.1 - 0.5 wt .-% P, more preferably consists of the active composition of the abovementioned constituents.
  • the active material consists of 85.80 wt .-% of Ti0 2 , 14 wt .-% V 2 0 5 and 0.2 wt -.% P.
  • the amount of active mass in the catalyst is between 5 and 15% by weight, more preferably between 6 and 12% by weight, and most preferably between 7 and 11% by weight.
  • the catalytically active material of the catalyst contains the catalytically active material of the catalyst
  • promoter selected from the group consisting of P, Sb, Bi, Li, Cs, Sr, Ba, Ni, Co and noble metals selected from the group consisting of Cu, Ag, Au, Pt, Pd and Rh.
  • the catalytically active composition of the postreactor according to the invention preferably additionally comprises an organic binder, preferably a vinyl acetate-ethylene copolymer, or a decomposition product of the abovementioned during calcination
  • the catalytically active composition preferably has an inorganic binder in the form of a sol, metal alkoxide (of Si0 2 sol or its precursors, Al 2 0 3 sol or its precursors, Zr0 2 sol or its precursors, Ti0 2 sol, Ce0 2 sol or its precursors, water glass, MgO, etc).
  • the present invention relates to a process for producing a post-reactor according to the invention, comprising the following steps: (i) providing a catalytically active composition as defined herein, at least containing TiO 2 , wherein the TiO 2 is a
  • step (v) incorporating the catalyst obtained in step (iv) into a post-reactor.
  • the catalyst obtained in step (iv) into a post-reactor.
  • step v) calcining the catalyst obtained in step v) at a temperature of more than 200 ° C, preferably at a
  • step vi) activating the catalyst obtained in step vi) at a temperature of more than 350 ° C, preferably at a
  • the catalytically active layer is preferably by immersion and extraction, by purging, by
  • the method according to the invention is preferred for producing a reactor arrangement comprising a
  • Manufacturing process can be carried out in the usual manner, for example, a suspension of titanium oxide,
  • vanadium pentoxide preferably in the anatase modification, vanadium pentoxide, diantimony trioxide, with a suitable organic and an inorganic binder, for example vinyl acetate-ethylene copolymer, a Ti0 2 sol and suitable promoters
  • a suitable organic and an inorganic binder for example vinyl acetate-ethylene copolymer, a Ti0 2 sol and suitable promoters
  • the catalytically active composition provided in the form of an aqueous suspension.
  • the suspension contains
  • Suitable binders include organic binders known to the person skilled in the art, preferably copolymers, advantageously in the form of an aqueous dispersion, of vinyl acetate / vinyl laurate, vinyl acetate / acrylate, styrene / acrylate, vinyl acetate / maleate and vinyl acetate / ethylene.
  • organic binders known to the person skilled in the art, preferably copolymers, advantageously in the form of an aqueous dispersion, of vinyl acetate / vinyl laurate, vinyl acetate / acrylate, styrene / acrylate, vinyl acetate / maleate and vinyl acetate / ethylene.
  • Particularly preferred is an organic polymeric or copolymeric adhesive, especially a vinyl acetate copolymer adhesive, most preferably a vinyl acetate-ethylene copolymer as
  • Binder used is added in conventional amounts of the catalytically active composition, preferably with 10 to 25 wt .-%, more preferably with 20 to 25 wt .-%, based on the solids content of the catalytically active material.
  • the binder used is added in conventional amounts of the catalytically active composition, preferably with 10 to 25 wt .-%, more preferably with 20 to 25 wt .-%, based on the solids content of the catalytically active material.
  • step (ii) The preparation of the porous support in step (ii) is carried out as described above. It can too
  • step (iii) the suspension from step (i) can then be applied by single or multiple impregnation, spraying, or by suction, In particular, by applying in.
  • Carrier also possible without organic binders.
  • Useful coating temperatures when using the abovementioned binders are according to DE 21 06 796
  • binders used burn when the catalyst is heated
  • the binders serve primarily to enhance the adhesion of the catalytically active material to the carrier.
  • step (iv) the catalyst is subsequently dried, incorporated in a post reactor and in the usual way
  • the catalyst for at least 24 hours at least 250 ° C, especially between 24 and 72 hours at 350 ° C, in a 0 2 -containing gas, especially in air, is calcined.
  • the temperature should preferably not exceed 500 ° C, especially 470 ° C
  • the conditioning of the post-catalyst takes place by means of the product gas stream from the main reactor at temperatures between 250 and 350 ° C, preferably between 370 and 350 ° C.
  • temperatures between 250 and 350 ° C, preferably between 370 and 350 ° C.
  • high temperatures can not be achieved in situ in the post-reactor, since, for example, the o-xylene content in the feed and the operating temperature are too low. That is, the catalyst for the post-reactor must before installation in a reactor arrangement, for example in a tray oven at the top
  • step (v) the shaped catalyst bodies are so
  • Voids arise and also the catalysts are sealed against the reactor wall, so that the reaction gas is passed through the catalysts.
  • different catalysts can be incorporated into the post-reactor.
  • the catalysts can be interconnected.
  • the present invention relates to the use of a secondary reactor according to the invention and a reactor arrangement according to the invention for the gas phase oxidation of organic
  • Phthalic anhydride by gas phase oxidation of o-xylene and / or naphthalene.
  • Main reactor for example, a tube bundle reactor with catalyst bed, and then by a
  • the catalysts in the reaction tubes of the main reactor which are thermostated from the outside to the reaction temperature, for example by means of molten salts, filled.
  • the reaction gas at temperatures of generally 250 to
  • the space velocity is generally from 1000 to 50,000 h.sup.- 1 .
  • Inlet temperature of the reaction gas is adjusted by a gas cooler before the postreactor.
  • the reaction gas supplied to the catalyst is in
  • Reaction moderators and / or diluents such as vapor, carbon dioxide and / or nitrogen may contain, produced with the aromatic hydrocarbon to be oxidized, wherein the molecular oxygen-containing gas is generally 1 to 100, preferably 2 to 50 and particularly preferably 10 to 30 mol% of oxygen, 0 to 30, preferably 0 to 10 mol% of water vapor and 0 to 50, preferably 0 to 1 mol% of carbon dioxide, balance nitrogen.
  • the gas containing the molecular oxygen is generally charged with 30 to 150 g per Nm 3 of gas of the aromatic hydrocarbon to be oxidized.
  • Figure 1 is a schematic illustration of cells as they are arranged in a sponge. The numbers in the cells indicate the number of adjacent cells.
  • reaction gas containing the catalysts according to the invention in the form of cylindrical cores, can be used.
  • Main reactor has passed through the inlet 2 in the
  • Reaction space 6 which contains the catalyst, introduced into the secondary reactor 1. Through the outlet 5, the reaction gas is passed out of the secondary reactor 1. Terminals 3 and 4 are used to connect thermocouples to measure the adiabatic T increase in the reactor.
  • Catalysts are used the following methods. If properties of the finished catalyst are to be measured, the catalyst or a part thereof can be pulverized and the determination of the parameters of this powder
  • porous support and catalytically active layer are performed. If properties of the porous support without
  • the catalytically active layer can be removed manually, for example by shaking or scraping.
  • the remaining porous support can then be pulverized and examined again.
  • the manually removed catalytically active layer can be examined.
  • Pore radius distribution / pore diameter / pore volumes The determination of the pore radius distribution of the porous support and the Ti0 2 was carried out by
  • the proportion of active mass (proportion of the catalytically active composition, without binder) in each case refers to the proportion (in% by weight) of the catalytically active composition in the total weight of the catalyst, including support in the respective catalyst layer, measured after conditioning at 400 ° C. for 4 hours in air.
  • Pores are filled with liquid.
  • other liquids which nevertheless have lower vapor pressure (eg toluene) must be selected.
  • the same also changes Buoyancy related to the theoretical density of the material when closed pores are present.
  • the dry mass (mt) the dry mass (mt)
  • Bulk density generally refers to the mass of a dry material by volume, including all pores.
  • the basis for the raw density determination is DIN 1094.
  • volume is not determined according to the Archimedian principle by measuring the buoyancy in a liquid of known density, but determined by the Ausmess vide. This succeeds only on geometrically defined bodies. In this case, sealing in the surface area (wax, zapon varnish) can help, the volume also irregularly shaped porous
  • reaction tube of defined length and inner diameter (for example 25 mm inner diameter, 1 m length), at given reaction conditions (temperature, pressure,
  • Catalyst activity thus on the basis of the level of conversion of o-xylene or naphthalene to the oxidation products.
  • Cause of a higher catalyst activity can either be optimized for the desired nature / quality of the active Centers (see, for example, "turn over frequency") or an increased number of active centers in the same balance area, which is given, for example, if a higher
  • the determination of the compression strength is carried out according to DIN 53291.
  • the compression strength in MPa corresponds to the value at 20% elongation of the test specimen.
  • the pore density is determined by counting the number of open pores that are in an area of one square inch.
  • Comparative Example 1 The comparative example relates to the use of a
  • reaction tube was centrally arranged a 3 mm thermal sleeve with built-in tension element for temperature measurement.
  • Reaction gas samples are taken by means of a separate glass cold trap in an acetone / dry ice mixture directly after the output of the main and secondary reactor and analyzed.
  • the postreactor is downstream of the main reactor and is described below.
  • the postreactor was constructed as shown in Figure 2 and contained 3 "cores" in the form of honeycomb catalysts
  • Post reactor was 292 ° C, the gas outlet temperature after the post reactor was 307 ° C.
  • Post-reactor catalyst temperature was determined to be 309 ° C in the middle of the middle core. 236 g Ti0 2 (BET about 30m 2 / g) with a middle
  • Particle diameter of about 1 ⁇ , 236 g Ti0 2 (BET about 20m 2 / g) with an average particle diameter of about 1 ⁇ ⁇ , 120 g V 2 0 5 and 8.24 g of (NH 4 ) 2 HPO 4 were suspended in 1400 ml of deionized water and stirred for 18 hours to achieve a homogeneous distribution.
  • the solids content of the resulting suspension was 29.6 wt .-%. Thereafter, 60 g were added
  • organic binder a copolymer of ethylene / vinyl acetate, added in the form of a 50 wt .-% aqueous dispersion.
  • this coating suspension was a monolithic ceramic carrier honeycomb of cordierite with a cell density of 200 cpsi and the dimensions described below
  • honeycomb bodies calcined in air in a rack oven at 450 ° C for 24 h.
  • the honeycomb bodies had a diameter of 55 mm and a length of 150 mm, with the 3 catalysts
  • the drill cores are located in the reaction space through which the reaction gas flows.
  • the crude yield is determined as follows. Max. Raw PSA yield [% by weight]
  • the table below compares the reaction gas samples before and after the post reactor, which were obtained at an o-xylene loading of 80g / Nm 3 .
  • the yield of phthalic anhydride in the reaction gas sample after the main reactor was 114.7 wt .-%.
  • This inventive example relates to the use of a main reactor, as described in Comparative Example 1, in combination with a post-reactor according to the invention.
  • the postreactor according to the invention is the main reactor
  • the secondary reactor was constructed as shown in Figure 2 and contained 3 "cores" in the form of catalysts according to the invention
  • the gas inlet temperature into the post reactor was 292 ° C, the
  • the post-reactor catalyst temperature was determined to be 305 ° C in the middle of the middle core.
  • the catalysts comprised a porous support (Sic sponge with 110 ppi) with a diameter of 55 mm and a length of 150 mm, wherein the 3 catalysts in succession in the
  • the catalytically active composition applied to the porous carrier contained: 79.8% by weight of TiO 2 / 20.0% by weight of V 2 O 5 , 0.2% by weight of P. In addition, 2.3% by weight of % of an organic binder
  • the catalyst thus prepared had a BET surface area of about 32 m 2 / g.
  • the table below compares the reaction gas samples before and after the post reactor, which were obtained at an o-xylene loading of 80g / Nm 3 .
  • the yield of phthalic anhydride in the reaction gas sample after the main reactor was 114.4 wt .-%.
  • the yield Phthalic anhydride in the reaction gas sample after the post-reactor according to the invention was 116, l-wt%.

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Abstract

La présente invention concerne un système de réacteurs constitué d'un réacteur principal et d'un réacteur secondaire, le réacteur secondaire contenant au moins un catalyseur et le catalyseur comprenant un support poreux, qui comprend une éponge de SiC solide, une masse catalytiquement active contenant du TiO2 et au moins un oxyde de métal de transition étant appliquée sur le support poreux, et le TiO2 utilisé possédant une densité apparente inférieure à 1,0 g/ml. La présente invention concerne en outre l'utilisation du réacteur secondaire dans la production d'anhydride d'acide phtalique au moyen d'une oxydation en phase gazeuse, ainsi qu'un procédé de fabrication dudit réacteur secondaire.
PCT/EP2010/006268 2009-10-13 2010-10-13 Système de réacteurs pour oxydation en phase gazeuse catalytique WO2011045051A1 (fr)

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CN114126757A (zh) * 2019-05-21 2022-03-01 马克斯·普朗克科学促进会 用于放热反应的催化剂

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Publication number Priority date Publication date Assignee Title
CN114126757A (zh) * 2019-05-21 2022-03-01 马克斯·普朗克科学促进会 用于放热反应的催化剂

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