EP3710157A1 - Catalyseur scr - Google Patents

Catalyseur scr

Info

Publication number
EP3710157A1
EP3710157A1 EP18796991.0A EP18796991A EP3710157A1 EP 3710157 A1 EP3710157 A1 EP 3710157A1 EP 18796991 A EP18796991 A EP 18796991A EP 3710157 A1 EP3710157 A1 EP 3710157A1
Authority
EP
European Patent Office
Prior art keywords
catalyst
oxide
weight
catalyst according
calculated
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP18796991.0A
Other languages
German (de)
English (en)
Inventor
Elodie Quinet
Stephan Malmberg
Nicola Soeger
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Umicore AG and Co KG
Original Assignee
Umicore AG and Co KG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Umicore AG and Co KG filed Critical Umicore AG and Co KG
Publication of EP3710157A1 publication Critical patent/EP3710157A1/fr
Pending legal-status Critical Current

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
    • F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
    • F01N3/18—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control
    • F01N3/20—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control specially adapted for catalytic conversion ; Methods of operation or control of catalytic converters
    • F01N3/2066—Selective catalytic reduction [SCR]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • B01D53/9404—Removing only nitrogen compounds
    • B01D53/9409—Nitrogen oxides
    • B01D53/9413—Processes characterised by a specific catalyst
    • B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
    • 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
    • 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
    • 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
    • B01J21/066—Zirconium or hafnium; 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/18—Arsenic, antimony or bismuth
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    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/20—Vanadium, niobium or tantalum
    • B01J23/22—Vanadium
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    • B01J23/24—Chromium, molybdenum or tungsten
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    • B01J37/08—Heat treatment
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    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/12—Oxidising
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    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N13/00—Exhaust or silencing apparatus characterised by constructional features ; Exhaust or silencing apparatus, or parts thereof, having pertinent characteristics not provided for in, or of interest apart from, groups F01N1/00 - F01N5/00, F01N9/00, F01N11/00
    • F01N13/009—Exhaust or silencing apparatus characterised by constructional features ; Exhaust or silencing apparatus, or parts thereof, having pertinent characteristics not provided for in, or of interest apart from, groups F01N1/00 - F01N5/00, F01N9/00, F01N11/00 having two or more separate purifying devices arranged in series
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
    • F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
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    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
    • F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
    • F01N3/033—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices
    • F01N3/035—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices with catalytic reactors, e.g. catalysed diesel particulate filters
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    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
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    • F01N3/105—General auxiliary catalysts, e.g. upstream or downstream of the main catalyst
    • F01N3/106—Auxiliary oxidation catalysts
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    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
    • F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
    • F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
    • F01N3/28—Construction of catalytic reactors
    • F01N3/2882—Catalytic reactors combined or associated with other devices, e.g. exhaust silencers or other exhaust purification devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D2258/01—Engine exhaust gases
    • B01D2258/012—Diesel engines and lean burn gasoline engines
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • F01N2370/00—Selection of materials for exhaust purification
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    • F01N2610/00—Adding substances to exhaust gases
    • F01N2610/02—Adding substances to exhaust gases the substance being ammonia or urea
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02T10/00—Road transport of goods or passengers
    • Y02T10/10—Internal combustion engine [ICE] based vehicles
    • Y02T10/12—Improving ICE efficiencies

Definitions

  • the present invention relates to a SCR catalyst based on vanadium oxide containing niobium and cerium oxide.
  • the exhaust gas of motor vehicles which are operated with lean-burn combustion engines, for example with diesel engines, contains not only carbon monoxide (CO) and nitrogen oxides (NOx) but also components resulting from the incomplete combustion of the fuel in the combustion chamber of the cylinder.
  • CO carbon monoxide
  • NOx nitrogen oxides
  • HC residual hydrocarbons
  • these also include particulate emissions.
  • These are complex agglomerates of predominantly carbon-containing solid particles and an adhering liquid phase, which mostly consists of relatively long-chain hydrocarbon condensates.
  • Liquid phase is also referred to as “Soluble Organic Fraction SOF” or “Volatile Organic Fraction VOR”.
  • One known method of removing nitrogen oxides from exhaust gases in the presence of oxygen is the selective catalytic reduction by means of ammonia on a suitable catalyst (SCR process).
  • SCR process the nitrogen oxides to be removed from the exhaust gas are reacted with ammonia as a reducing agent to nitrogen and water.
  • the exhaust gas from lean-burn internal combustion engines usually comprises NO.sub.2 in amounts of only about 10% of the total nitrogen oxide fraction, it is normally the intention to increase its proportion in order to benefit from the rapid SCR reaction. This happens, for example, by means of an upstream oxidation catalyst. Depending on the exhaust system used in the specific case, however, an SCR catalytic converter may nevertheless have very different NO 2 / NO x ratios
  • ammonia used as a reducing agent can be prepared by metering in an ammonia precursor compound, such as, for example, urea,
  • Ammonium carbamate or ammonium formate are made available in the exhaust line and subsequent hydrolysis.
  • mixed oxide catalysts are based on oxides of vanadium and usually also oxides of titanium and other metals, such as tungsten, contain (see Isabella Nova and Enrico Tronconi (ed.), Urea SCR Technology for deOx After Treatment of Diesel Exhausts, Chapter 3, Springer Verlag, 2014).
  • SCR catalysts based on vanadium oxide are characterized by good activity and stability. However, they show significant activity losses in the case of excess N02. Although the addition of ceria to the vanadium oxide-based SCR catalysts improves N02 excess activity, it also decreases the low temperature activity (T ⁇ 250 ° C) with NO excess.
  • niobium oxide on metal oxide-based SCR catalysts.
  • US Pat. No. 9,555,371 discloses an SCR catalyst which contains at least 91% by weight of cerium oxide and 0.1 to 9% by weight of niobium oxide or tantalum oxide.
  • WO 2012/004263 A1 also describes a catalyst which comprises cerium oxide and 2 to 20% by weight of niobium oxide.
  • zirconium oxide and other metal oxides may also be present.
  • WO 2011/032020 A2 discloses an SCR catalyst comprising a carrier layer and a catalytic layer. While the backing layer, for example, TiO2, Al2O3, SiO2, TiO2 -AI2O3, TiO 2 - SiO 2, CeO 2, AI2O3-SiO 2 or TiO 2 -Al20 3 -SiO 2, the catalytic layer may also contain niobium.
  • the present invention accordingly relates to a catalyst which
  • At least one oxide of cerium in an amount of from 2 to 4% by weight
  • At least one oxide of titanium in an amount calculated to result in a total of 100% by weight
  • the at least one oxide of titanium acts as a carrier material, the at least one oxide of vanadium as the active catalyst component, and the respective at least one oxide of tungsten, cerium and niobium as promoters.
  • Promoters are substances
  • the catalyst according to the invention additionally contains at least one oxide of silicon.
  • Catalyst further comprises at least one oxide of tungsten in an amount of 0.001 to 2 wt .-%.
  • At least one oxide of tungsten in an amount of 0.001 to 2% by weight
  • At least one oxide of cerium in an amount of from 2 to 4% by weight
  • At least one oxide of titanium in an amount which is such that a total of 100% by weight
  • the catalyst according to the invention additionally contains at least one oxide of molybdenum, antimony, zirconium, tantalum and / or hafnium. In preferred embodiments of the catalyst according to the invention it contains at least one oxide of cerium in amounts of 2 to 4 wt .-%, based on the weight of the catalyst and calculated as CeO 2 . In further preferred embodiments of the invention
  • Catalyst it contains at least one oxide of niobium in amounts of 1 to 7 wt .-%, based on the weight of the catalyst and calculated as Nb 2 O 5 .
  • Embodiments of the catalyst according to the invention are furthermore preferred which contain at least one oxide of cerium in amounts of from 2 to 4% by weight, calculated as CeO 2 , and at least one oxide of niobium in amounts of from 1 to 7% by weight, in each case based on the weight of the catalyst and calculated as Nb 2 O 5 .
  • At least one oxide of cerium in an amount of 2 to 4% by weight
  • At least one oxide of titanium in an amount calculated to result in a total of 100% by weight
  • the catalyst according to the invention contains at least one oxide of silicon, it is preferably present in amounts of from 2 to 7% by weight, based on the weight of the catalyst and calculated as SiO 2 . If the catalyst according to the invention at least one oxide of silicon
  • Hafniums comprises, the total amount of these oxides is preferably 0.5 to 20 wt .-%, based on the weight of the catalyst and calculated as MoO3, Sb 2 0 5 , Zr0 2 , Ta 2 0 5 or Hf02.
  • the catalyst according to the invention is preferably free of magnesium or compounds of magnesium.
  • the catalyst according to the invention is also free of zirconium or compounds of zirconium.
  • oxide of vanadium in the context of the present invention comprises all oxides which are formed under the conditions of preparation, storage and use of the catalyst according to the invention or
  • V2O5 may be present. It thus includes, for example, V2O5, but also all other oxides of vanadium.
  • oxide of tungsten includes, for example, WO3, but also all other oxides of tungsten, the term oxide of cerium for example Ce0 2 , but also all other oxides of cerium, the term oxide of niobium, for example Nb 2 O 5 , but All other oxides of niobium, the term oxide of titanium, for example TiO 2 , but also all other oxides of titanium, as well as oxide of silicon, for example SiO 2 , but also all other oxides of silicon.
  • oxide of molybdenum, antimony, zirconium, tantalum or hafnium oxide of molybdenum, antimony, zirconium, tantalum or hafnium.
  • the catalyst according to the invention can be prepared in a simple manner.
  • oxides of vanadium, tungsten, cerium, niobium and titanium and, if appropriate, the other metal oxides in powder form can be intimately mixed in the desired amounts and then calcined.
  • only some of the metal oxides are introduced as such, while the other metals are added in the form of water-soluble metal salts.
  • oxides of vanadium, tungsten, cerium, niobium and titanium and, if appropriate, the other metal oxides in powder form can be intimately mixed in the desired amounts and then calcined.
  • only some of the metal oxides are introduced as such, while the other metals are added in the form of water-soluble metal salts.
  • Suitable water-soluble vanadium compounds are, in particular, vanadyl oxalate, which can be obtained by dissolving vanadium pentoxide in oxalic acid (see, for example, EP 0 345 695 A2) or reaction products of
  • Vanadium pentoxide with amines or ethanolamines see for example WO89 / 03366 Al and W02011 / 013006), especially ammonium metavanadate.
  • DE 11 2007 000 814 T5 also describes the use of vanadium oxytrichloride.
  • oxides of vanadium, cerium, niobium and titanium can also be initially charged and then with the aqueous solution of a water-soluble
  • Tungsten compound impregnated and subsequently dried and calcined A suitable water-soluble tungsten compound is
  • two or more metal oxides may also be used in the form of the corresponding mixed oxides or in the form of metal oxides doped with one or more other metal oxides.
  • titanium dioxide doped with silica and tungsten trioxide may be impregnated with water-soluble compounds of vanadium and niobium and then dried and calcined.
  • the catalyst according to the invention can be present as a mixture of metal oxides, as mixed oxide, but especially in the form of intermediates between a mixture of metal oxides and mixed oxide.
  • two or three metals may be in the form of a mixed oxide impregnated with the remaining metals.
  • the catalyst according to the invention is present as a coating on a carrier body, which may be present as a flow-through honeycomb body or wall-flow filter.
  • the support body is catalytically inert and is made of ceramic or metallic material, for example of silicon carbide, aluminum titanate or cordierite. In these embodiments, all components of the catalyst according to the invention are present in a coating.
  • Coated carrier bodies can be produced by methods familiar to the person skilled in the art, for example by the customary dip coating methods or by pumping and suction coating methods
  • Inventive catalyst itself component of the support body, which is formed in this case from the catalyst of the invention, and a matrix component.
  • inert matrix component 10 to 95 wt .-% inert matrix component and 5 to 90 wt .-% of catalytically active material extruded by methods known per se.
  • matrix components it is also possible to use all inert materials which are otherwise used to prepare catalyst substrates. These are, for example, silicates, oxides, nitrides or carbides, with particular preference being given to magnesium-aluminum silicates.
  • the catalyst according to the invention is outstandingly suitable for the reduction of nitrogen oxides in exhaust gases of lean-operated
  • the present invention thus also relates to a method for
  • a reducing agent is particularly ammonia in question, with particular advantage to nitrogen oxides containing exhaust gas not ammonia itself, but an ammonia precursor, in particular urea,
  • the catalyst of the invention is used as part of an exhaust gas purification system which, for example, in addition to the catalyst according to the invention arranged upstream
  • Oxidation catalyst and a diesel particulate filter comprises.
  • the catalyst according to the invention can also be used as a coating on the
  • the present invention thus also relates to an exhaust gas purification system for treating diesel exhaust gas in the flow direction of the exhaust gas
  • Suitable for the inventive exhaust gas purification system oxidation catalysts in particular platinum, palladium or platinum and palladium supported on, for example, alumina, and diesel particulate filter are known in the art and available on the market.
  • the exhaust gas purification system according to the invention comprises a device arranged downstream of the catalyst according to the invention for dosing in the reducing agent.
  • the injection device can be chosen arbitrarily by the person skilled in the art, suitable devices being able to be taken from the literature (see, for example, T. Mayer, Solid-SCR System Based on Ammonium Carbamate, Dissertation, TU Kaiserslautern, 2005).
  • a reducing agent in particular ammonia as such or in the form of a compound is introduced into the exhaust gas stream via the injection device, from which ammonia is formed at the ambient conditions.
  • aqueous solutions of urea or ammonium formate in question, as well as solid ammonium carbamate As such, for example, aqueous solutions of urea or ammonium formate in question, as well as solid ammonium carbamate.
  • the reducing agent or a precursor thereof is kept in stock in a entrained container which is connected to the injection device.
  • Figure 1 Nitrogen oxide conversions in the standard SCR reaction, measured on the inventive catalysts Kl and K2 compared to the comparative catalysts VK1, VK2, VK3 and VK4 in the fresh state (K1f, K2f, VKlf, VK2f, VK3f, VK4f).
  • FIG. 2 Nitrogen oxide conversions in the standard SCR reaction, measured on the novel catalyst K1 and K2 in comparison with the comparative catalysts VK1, VK2, VK3 and VK4 in the aged state (Kla, K2a, VKla, VK2a, VK3a, VK4a).
  • FIG. 3 Nitrogen oxide conversions in the rapid SCR reaction, measured on the inventive catalyst K1 and K2 in comparison to the comparative catalysts VK1, VK2, VK3 and VK4 in the fresh state (Klf, K2f, VKlf, VK2f, VK3f and VK4f).
  • FIG. 4 Nitrogen oxide conversions in the rapid SCR reaction, measured on the inventive catalyst K1 and K2 in comparison with the comparative catalysts VK1, VK2, VK3 and VK4 in the aged state (Kla, K2a, VKla, VK2a, VK3a, VK4a).
  • Figure 5 Nitrogen oxide conversions in the standard SCR reaction at 200 ° C and rapid SCR reaction at 300 ° C against the W0 3 content, measured on the novel catalyst Kl and K2 in comparison to the comparative catalysts VK5 and VK6 in fresh and aged condition.
  • FIG. 6 Nitrogen oxide conversions in the standard SCR reaction at 200 ° C. and rapid SCR reaction at 300 ° C. against the CeO 2 content, measured on the inventive catalyst Kl in comparison to the comparative catalysts VK 3 and VK 7 in fresh and aged State.
  • Figure 7 Nitrogen oxide conversions in the standard SCR reaction at 200 ° C and rapid SCR reaction at 300 ° C against the Nb 20s content, measured on the catalyst of the invention Kl compared to the comparative catalysts VK2, VK8 and VK9 in fresh and aged condition.
  • Titanium dioxide in the anatase form was dispersed in water and then
  • Vanadium dioxide (VO2), tungsten trioxide (WO 3 ), ceria (CeO 2 ) and Ammoniumnioboxalat added in amounts such that a catalyst composition 85.98 wt .-% TiO 2, 4.53 wt .-% SiO 2 , 3.75 wt %
  • V2O 5 1.00% by weight of WO 3 , 2.00% by weight of CeO 2 and 2.75% by weight of Nb 2 O 5 .
  • the mixture was stirred vigorously and finally ground in a commercially available stirred ball mill.
  • Titanium dioxide in the anatase form was dispersed in water and then vanadium dioxide (VO 2) and tungsten trioxide (WO 3) were added in amounts such that a catalyst of the composition 90.49% by weight of TiO 2 , 4.76% by weight of SiO 2 , 3, 75 wt .-% V2O5, 1.00 wt .-% WO3 results.
  • the mixture was stirred vigorously and finally stirred in a commercially available stirred ball mill.
  • VKla The VK1 obtained according to b) was subjected to a hydrothermal aging for 48 hours at 700 ° C. in a gas atmosphere (10% O 2, 10% H 2 O, remainder N 2). The catalyst VK1 is then aged and is referred to below as VKla.
  • Titanium dioxide in the anatase form was dispersed in water and then vanadium dioxide (VO 2 ), tungsten trioxide (WO 3) and ceria (CeO 2 ) were added in amounts such that a catalyst of the composition 88.59 wt.% TiO 2 , 4.66 wt. % SiO 2 , 3.75 wt% V2O5, 1.00 wt% WO3, and 2.00 wt% CeO 2 .
  • the mixture was stirred vigorously and finally stirred in a commercially available stirred ball mill.
  • the dispersion obtained in a) was in the usual manner to a
  • VK2a The VK2 obtained according to b) was subjected to a hydrothermal aging for 48 hours at 700 ° C. in a gas atmosphere (10% O 2, 10% H 2 O, balance N 2). Catalyst VK2 is then aged and is referred to below as VK2a. Comparative Example 3
  • Titanium dioxide in the anatase form was dispersed in water and then vanadium dioxide (VO 2), tungsten trioxide (WO 3) and ammonium niobium oxalate were added in amounts such that a catalyst of the composition 87.88% by weight of TiO 2 , 4.63% by weight of SiO 2 , 3.75% by weight of V2O5, 1.00% by weight of WO3 and 2.75% by weight of Nb 2 O 5 .
  • the mixture was stirred vigorously and finally ground in a commercially available stirred ball mill.
  • VK3a The VK3 obtained according to b) was subjected to a hydrothermal aging for 48 hours at 700 ° C. in a gas atmosphere (10% O 2, 10% H 2 O, remainder N 2). The catalyst VK3 is then aged and is referred to below as VK3a. Comparative Example 4
  • VK4a The catalyst obtained according to b) VK4 was 48 hours at 700 ° C in a gas atmosphere (10% O2, 10% H2O, balance N2) subjected to a hydro- thermal aging. The catalyst VK4 is then aged and is referred to below as VK4a.
  • VK6a The catalyst obtained according to b) VK6 was 48 hours at 700 ° C in a gas atmosphere (10% O2, 10% H2O, balance N2) subjected to a hydro- thermal aging. Catalyst VK6 is then aged and is referred to below as VK6a. Comparative Example 7
  • VK7a The catalyst obtained according to b) VK7 was 48 hours at 700 ° C in a gas atmosphere (10% O2, 10% H2O, balance N2) subjected to a hydro- thermal aging. Catalyst VK7 is then aged and is referred to below as VK7a.
  • VK8a The catalyst obtained according to b) VK8 was 48 hours at 700 ° C in a gas atmosphere (10% O2, 10% H2O, balance N2) subjected to a hydro- thermal aging. Catalyst VK8 is then aged and is referred to below as VK8a.
  • VK9a The catalyst obtained according to b) VK8 was 48 hours at 700 ° C in a gas atmosphere (10% O2, 10% H2O, balance N2) subjected to a hydro- thermal aging. Catalyst VK9 is then aged and is referred to below as VK9a.
  • Table 1 summarizes the compositions of the catalysts of the examples mentioned. The composition of the catalyst according to the invention is not limited to explicitly shown examples.
  • Table 1 Compositions of the catalysts from the examples
  • the nitrogen oxide concentrations of the model gas were detected after passing through the catalyst with a suitable analysis. From the known, metered nitrogen oxide contents, which were verified during conditioning at the beginning of the respective test run with a pre-catalytic exhaust gas analysis, and the measured
  • Nitrogen oxide conversion based on the ratio of NH3 to NO, over the catalyst for each temperature measurement point calculated as follows:
  • Table 2 shows the NOx conversion in the standard SCR reaction for the examples described above.
  • Table 2 NOx conversion in the standard SCR reaction
  • Table 3 shows the NOx conversion in the fast SCR reaction for the examples described above.
  • K2 was varied above 0.50 wt.% (VK5), 1.00 wt.% (KI) and 2.00 wt.% (VK6).
  • the results of the influence of the WO 3 content are shown in FIG. 5.
  • the influence of CeO 2 content of the catalyst on the NOx conversion in the standard SCR reaction at 200 ° C and in the rapid SCR reaction at 300 ° C in the fresh and aged state is shown in Table 5.
  • the amounts of V2O5, WO3 and Nb 2 O 5 were kept constant at 3.75 wt.%, 1.00 wt.% And 2.75 wt.%, Respectively, while the CeO 2 content was 0.00 wt .-%
  • VK3 was varied over 2.00 wt.% (KI) and 2.00 wt.% (VK7).
  • Nb20s content of the catalyst is shown in Table 6.
  • the amounts of V2O5, WO3, and CeO 2 were constant at 3.75 wt .-%, 1.00 wt .-% and 2.00 wt .-% retained, while the Nb 2 O 5 content of 0.00 wt.-
  • VK2 was varied over 2.75 wt.% (K1), 4.00 wt.% (VK8) and 7.00 wt.% (VK9).

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Abstract

La présente invention concerne un catalyseur, qui contient au moins un oxyde de vanadium, au moins un oxyde de tungstène, au moins un oxyde de cérium, au moins un oxyde de titane et au moins un oxyde de niobium, ainsi qu'un système d'échappement doté dudit catalyseur.
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