EP3676000A1 - Catalyseur adsorbant passif d'oxyde d'azote à base de palladium-zéolite pour la purification de gaz d'échappement - Google Patents

Catalyseur adsorbant passif d'oxyde d'azote à base de palladium-zéolite pour la purification de gaz d'échappement

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Publication number
EP3676000A1
EP3676000A1 EP18758622.7A EP18758622A EP3676000A1 EP 3676000 A1 EP3676000 A1 EP 3676000A1 EP 18758622 A EP18758622 A EP 18758622A EP 3676000 A1 EP3676000 A1 EP 3676000A1
Authority
EP
European Patent Office
Prior art keywords
palladium
zeolite
catalyst
catalyst according
coating
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
EP18758622.7A
Other languages
German (de)
English (en)
Inventor
Christoph Hengst
Frank-Walter Schuetze
Michael Lennartz
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 EP3676000A1 publication Critical patent/EP3676000A1/fr
Pending legal-status Critical Current

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    • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/65—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the ferrierite type, e.g. types ZSM-21, ZSM-35 or ZSM-38, as exemplified by patent documents US4046859, US4016245 and US4046859, respectively
    • B01J29/66—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the ferrierite type, e.g. types ZSM-21, ZSM-35 or ZSM-38, as exemplified by patent documents US4046859, US4016245 and US4046859, respectively containing iron group metals, noble metals or copper
    • B01J29/67—Noble metals
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • 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
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/50—Zeolites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/90—Physical characteristics of catalysts
    • B01D2255/902—Multilayered catalyst
    • B01D2255/9025—Three layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/90—Physical characteristics of catalysts
    • B01D2255/904—Multiple catalysts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/90—Physical characteristics of catalysts
    • B01D2255/91—NOx-storage component incorporated in the catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/40—Nitrogen compounds
    • B01D2257/404—Nitrogen oxides other than dinitrogen oxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/01—Engine exhaust gases
    • B01D2258/012—Diesel engines and lean burn gasoline engines
    • 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
    • B01D53/944—Simultaneously removing carbon monoxide, hydrocarbons or carbon making use of oxidation catalysts
    • 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
    • B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
    • B01J2229/10—After treatment, characterised by the effect to be obtained
    • B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
    • B01J2229/183—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself in framework positions
    • 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
    • B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
    • B01J2229/30—After treatment, characterised by the means used
    • B01J2229/42—Addition of matrix or binder particles
    • 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
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0027—Powdering
    • B01J37/0036—Grinding
    • 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
    • B01J37/088—Decomposition of a metal salt
    • 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
    • F01N2370/00—Selection of materials for exhaust purification
    • F01N2370/02—Selection of materials for exhaust purification used in catalytic reactors
    • F01N2370/04—Zeolitic material
    • 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
    • F01N2610/00—Adding substances to exhaust gases
    • F01N2610/14—Arrangements for the supply of substances, e.g. conduits
    • F01N2610/1453—Sprayers or atomisers; Arrangement thereof in the exhaust apparatus
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • 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 passive nitrogen oxide adsorber for the passive incorporation of nitrogen oxides from the exhaust gas of a combustion engine, which comprises a palladium-coated 10-ring zeolite.
  • CO carbon monoxide
  • NO x nitrogen oxides
  • HC residual hydrocarbons
  • diesel soot particulate emissions
  • liquid phase adhering to the solid components is also referred to as "Soluble Organic Fraction SOF” or “Volatile Organic Fraction VOR.”
  • Soluble Organic Fraction SOF Soluble Organic Fraction SOF
  • Volatile Organic Fraction VOR Volatile Organic Fraction VOR
  • Soot particles can be removed very effectively with the help of particle filters from the exhaust gas.
  • Wall flow filters made of ceramic materials have proven particularly useful. These are from a variety of parallel
  • first channels Built up channels formed by porous walls.
  • the channels are mutually closed at one of the two ends of the filter, so that first channels are formed, which are open on the first side of the filter and closed on the second side of the filter, and second
  • the exhaust gas flowing into the first channels can only return the filter via the second channels
  • it must flow through the porous walls between the first and second channels. As the exhaust passes through the wall, the particles are retained.
  • particle filters can be provided with catalytically active coatings.
  • EP1820561 Al describes the coating of a diesel particulate filter with a catalyst layer, which facilitates the burning of the filtered soot particles.
  • One known method for removing nitrogen oxides from exhaust gases in the presence of oxygen is Selective Catalytic Reduction (SCR) using ammonia on a suitable catalyst.
  • SCR Selective Catalytic Reduction
  • the nitrogen oxides to be removed from the exhaust gas are reacted with ammonia to nitrogen and water.
  • iron and in particular copper-exchanged zeolites can be used as SCR catalysts, see, for example, WO2008 / 106519 A1, WO2008 / 118434 A1 and WO2008 / 132452 A2.
  • SCR catalysts for the conversion of nitrogen oxides with ammonia contain no noble metals, in particular no platinum and no palladium. Namely, in the presence of these metals, the oxidation of ammonia with oxygen to nitrogen oxides would proceed preferentially and the SCR reaction
  • SCR catalysts this does not refer to the N H3-SCR reaction, but to the reduction of nitrogen oxides by means of hydrocarbons, however, the latter reaction is only slightly selective, so that instead of “SCR reaction "true” HC-DeNOx reaction "is called.
  • 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.
  • SCR catalysts have the disadvantage that they only work from an exhaust gas temperature of about 180 to 200 ° C and thus do not implement nitrogen oxides that are formed in the cold start phase of the engine.
  • nitrogen oxide storage catalysts for which the term “lean NOx trap” or “LNT is customary, are known, whose cleaning effect is based on the fact that in a lean operating phase of the engine, the nitrogen oxides from the storage material of the storage catalyst predominantly in shape are stored by nitrates and this decomposes again in a subsequent rich phase of operation of the engine and the thus released nitrogen oxides with the reducing
  • Exhaust gas components are converted to the storage catalyst to nitrogen, carbon dioxide and water. This procedure is described for example in SAE SAE 950809.
  • storage materials are in particular oxides, carbonates or
  • Hydroxides of magnesium, calcium, strontium, barium, the alkali metals, the rare earth metals or mixtures thereof in question Due to their basic properties, these compounds are able to form nitrates with the acidic nitrogen oxides of the exhaust gas and produce them in this way
  • nitrogen oxide storage catalysts generally contain noble metals such as platinum, palladium and / or rhodium as catalytically active components. Their task is, on the one hand, to oxidise NO to NO 2, CO and HC to CO 2 under lean conditions and, on the other hand, to reduce released NO 2 to nitrogen during the rich operating phases in which the nitrogen oxide storage catalyst is regenerated.
  • the US2014 / 322112 describes a zoning of the coating of the particulate filter with nitrogen oxide storage catalyst such that a zone, starting from the upstream end of the particulate filter in the
  • Operating phase of the engine stored and released in a subsequent rich operating phase is also referred to as active nitrogen oxide storage.
  • active nitrogen oxide storage also known as passive nitric oxide storage
  • nitrogen oxides are stored in a first temperature range and released again in a second temperature range, wherein the second temperature range at higher
  • Temperatures are the first temperature range.
  • passive nitrogen oxide storage catalysts are used, which are also referred to as PNA (for "passive NOx adsorber").
  • nitrogen oxides in particular at temperatures below 200 ° C., at which an SCR catalytic converter has not yet reached its operating temperature, can be stored and released again as soon as the SCR catalytic converter is ready for operation.
  • nitrogen oxides in particular at temperatures below 200 ° C., at which an SCR catalytic converter has not yet reached its operating temperature
  • a zeolite containing, for example, palladium and another metal, such as iron is known to use as a passive nitrogen oxide storage catalyst.
  • WO2015 / 085303 AI discloses passive nitrogen oxide storage catalysts containing a noble metal and a small pore molecular sieve with a maximum ring size of eight tetrahedral atoms.
  • Passive nitrogen oxide storage catalysts are also in DE102016112065A1, DE102014118096A1, DE102015119913A1, DE102008010388A1 and
  • the present invention relates to a catalyst comprising a carrier substrate of length L, palladium and a zeolite whose major channels are formed by 10 tetrahedrally coordinated atoms.
  • Zeolites are two- or three-dimensional structures whose smallest structures Si0 4 and Al0 4 tetrahedra can be considered. These tetrahedra combine to form larger structures, with two each connected via a common oxygen atom.
  • rings of different sizes can be formed, for example rings of four, six or even nine tetrahedrally coordinated silicon or aluminum atoms.
  • the different zeolite types are often defined by the largest ring size, because this size determines which guest molecules can and can not penetrate into the zeolite structure. It is common to distinguish large pore zeolites with a maximum ring size of 12, medium pore zeolites with a maximum ring size of 10 and small pore zeolites with a maximum ring size of 8.
  • Zeolites are further subdivided into structure types by the Structure Commission of the International Zeolite Association, each of which has a three-letter code, see, for example, Atlas of Zeolite
  • the catalyst according to the invention preferably comprises zeolites whose largest channels are formed by 10 tetrahedrally coordinated atoms and which correspond to the structural types * MRE, AEL, AFO, AHT, BOF, BOZ, CGF, CGS, CSV, DAC, EUO, FER, HEU, IFW, IMF, ITH, ITR, JRY, JST, LAU, MEL, MFS, MTT, MVY, MWW, NES, OBW, -PAR, PCR, PON, PSI, RRO, SFF, SFG, STF, STI, STW, -SVR, SZR, TER, TONE, TUN, UOS, WEI or -WEN belong.
  • Zeolites of the structural type AEL are AIPO-11 and SAPO-11. Structure-type zeolites AFO are AIPO-41 and SAPO-41. A zeolite of the structural type AHT is AIPO-H2. CGS-type zeolites are TUN-1 and TsG-1. DAC zeolites are Dachiardite and Svetlozarit. Structure-type zeolites EU-1 are EU-1, TPZ-3 and ZSM-50. Zeolites of the structural type FER are ferrierite, FU-9, ISI-6, NU-23, Sr-D and ZSM-35. Zeolites of the structural type HEU are heulandite, clinoptilolite and LZ-219.
  • a structural-type zeolite IMF is IM-5.
  • ITH-type zeolites are ITQ-13 and IM-7.
  • Structural-type zeolites are Laumontite and Leonhardite.
  • Zeolites of the structural type MEL are ZSM-11, SSZ-46 and TS-2. Zeolites from
  • Structure type MFS are ZSM-57 and COK-5. Structure-type zeolites MTT are ZSM-23, EU-13, ISI-4 and KZ-1. MWW-type zeolites are MCM-22, ERB-1, ITQ-1, PSH-3 and SSZ-25. Zeolites of the structural type NES are NU-87 and Gottardite. A zeolite of the structural type OBW is OSB-2. A zeolite of the structure type -PAR is Partheit. A zeolite of the structural type PON is IST-1. A zeolite of the structural type RRO is RUB-41. A zeolite of the structural type SFF is SSZ-44. A zeolite of the structural type SFG is SSZ-58.
  • STF-type zeolites are SSZ-35, ITQ-9 and Mu-26.
  • STI-type zeolites are stilbite, barrerite, stellite and TNU-10.
  • a zeolite of the structural type SZR is SUZ-4.
  • a zeolite of the structural type TER is terranovaite.
  • TON type zeolites are theta-1, ISI-1, KZ-2, NU-10 and ZSM-22.
  • a TUN-type zeolite is TNU-9.
  • a zeolite of the structure type WEI is Weinebeneit.
  • a zeolite of the structural type -WEN is Wenkit.
  • the catalyst according to the invention particularly preferably comprises zeolites whose largest channels are formed by 10 tetrahedrally coordinated atoms and which belong to the structural type MEL, MTT, MWW or SZR.
  • the catalyst according to the invention particularly preferably comprises zeolites whose largest channels are formed by 10 tetrahedrally coordinated atoms and which belong to the structural type FER.
  • the catalyst according to the invention very particularly preferably comprises zeolites whose largest channels are formed by 10 tetrahedrally coordinated atoms and which belong to the structure type MWW.
  • Particularly preferred zeolites belonging to the structure type MEL are known from the literature. Thus, ZSM-11 is described in Nature 275, 119-120, 1978, SSZ-46 in US 5,968,474 and TS-2 in BE 1001038.
  • zeolites belonging to the structure type MWW are known from the literature.
  • SSZ-25 is described in US 4,826,667, MCM-22 in Zeolites 15, Issue 1, 2-8, 1995, ITQ-1 in US 6,077,498 and PSH-3 in US 4,439,409.
  • zeolites belonging to the structure type FER are known from the literature.
  • ZSM-35 is described in US 4,107,196, NU-23 in EP 103981 Al, FU-9 in EP 55529 Al, ISI-6 in US 4,695,440 and ferrierite for example in US 3,933,974, US 4,000,248 and US 4,251,499.
  • the catalyst according to the invention is preferred free of zeolites, whose largest channels are not formed by 10 tetrahedrally coordinated atoms.
  • the catalyst according to the invention does not comprise zeolites of the structural type LTL.
  • the catalyst according to the invention comprises palladium.
  • the palladium is preferably present as a palladium cation in the zeolite structure, that is in ion-exchanged form.
  • the palladium may also be wholly or partly present as palladium metal and / or as palladium oxide in the zeolite structure and / or on the surface of the zeolite structure.
  • the palladium may be present in amounts of from 0.01% to 20% by weight, based on the sum of the weights of zeolite and palladium and calculated as palladium metal.
  • Palladium is preferably present in amounts of from 0.5 to 10% by weight, more preferably from 1.5 to 10% by weight or 1.5 to 4% by weight and most preferably from 1.5 to 2% by weight. -% before, based on the sum of the weights of zeolite and palladium and calculated as palladium metal.
  • the catalyst according to the invention preferably contains no further metal other than palladium, in particular neither copper nor iron, nor platinum.
  • a preferred catalyst according to the invention comprises a structure-type zeolite MWW, for example MCM-22, ERB-1, ITQ-1, PSH-3 or SSZ-25, and palladium as the sole metal in an amount of 1.5 to 10% by weight. , based on the sum of the weights of zeolite and palladium and calculated as palladium metal, as well as no zeolite whose largest channels are not formed by 10 tetrahedrally coordinated atoms.
  • this catalyst according to the invention does not comprise any
  • the catalyst according to the invention comprises a support body. This may be a flow-through substrate or a wall-flow filter.
  • a wall-flow filter is a support body comprising channels of length L extending in parallel between a first and a second end of the channel
  • Wall flow filters which are alternately closed either at the first or at the second end and which are separated by porous walls.
  • a flow-through substrate differs from a wall-flow filter in that the channels of length L are open at both ends.
  • the pores of the wall-flow filter are so-called open pores, that is to say they have a connection to the channels. Furthermore, the pores are usually interconnected. On the one hand, this enables the light coating of the inner pore surfaces and on the other hand easy passage of the exhaust gas through the porous walls of the wall flow filter.
  • Flow substrates are known in the art as well as wall flow filters and are available on the market. They consist for example of silicon carbide, aluminum titanate or cordierite.
  • support bodies can be used, which are constructed of corrugated sheets of inert materials.
  • Suitable inert materials are, for example, fibrous materials having an average fiber diameter of 50 to 250 pm and an average
  • Fiber length from 2 to 30 mm.
  • fibrous materials are heat-resistant and consist of silicon dioxide, in particular of
  • sheets of said fiber materials are corrugated in a known manner and the individual corrugated sheets are formed into a cylindrical monolithically structured body with the body passing channels.
  • a monolithic structured body having a criss-cross corrugation structure is formed.
  • undulating i. be arranged flat leaves.
  • Carrier bodies of corrugated sheets can be coated directly with the catalyst according to the invention, but they are preferably initially coated with an inert material, for example titanium dioxide, and only then with the catalytic material.
  • an inert material for example titanium dioxide
  • the zeolite and the palladium are in the form of a coating on the carrier substrate.
  • the coating may extend over the entire length L of the carrier substrate or only over a part thereof.
  • the coating may be on the surfaces of the input channels, on the surfaces of the output channels, and / or in the porous wall between input and output channels.
  • autoboss catalysis By coating, the person skilled in the art of autoboss catalysis understands a material zone, which is also called washcoats, and is generally applied to the support body by means of an aqueous suspension.
  • Catalysts according to the invention in which the zeolite and the palladium are present in the form of a coating on the carrier substrate can be prepared by methods familiar to the person skilled in the art, for example by the customary dip coating methods or pumping and suction coating methods followed by thermal aftertreatment ( calcination). It is known to the person skilled in the art that, in the case of wall-flow filters, their average pore size and the average particle size of the materials to be coated are superimposed on one another
  • the average particle size of the materials to be coated can also be chosen such that they are located in the porous walls that form the channels of the wall-flow filter, that is to say that a coating of the inner pore surfaces takes place (in-wall coating).
  • the mean particle size of the materials to be coated must be small enough to penetrate into the pores of the wall flow filter.
  • the zeolite and the palladium are coated over the entire length L of the carrier substrate, with no further catalytically active coating on the carrier substrate.
  • the carrier substrate may also carry one or more further catalytically active coatings.
  • the carrier substrate may comprise, in addition to a coating comprising the zeolite and the palladium, a further coating which is active in oxidation-catalytically.
  • the oxidation-catalytically active coating comprises, for example, platinum, palladium or platinum and palladium on a carrier material.
  • the mass ratio of platinum to palladium for example, at 4: 1 to 14: 1.
  • Suitable carrier materials are all those familiar to the person skilled in the art for this purpose. They have a BET surface area of 30 to 250 m 2 / g, preferably from 100 to 200 m 2 / g (determined according to DIN 66132) and are in particular alumina, silica, magnesium oxide, titanium oxide, and mixtures or mixed oxides of at least two of these Materials. Preference is given to aluminum oxide, magnesium / aluminum mixed oxides and aluminum / silicon mixed oxides. If alumina is used, it is particularly preferably stabilized, for example with 1 to 6 wt .-%, in particular 4 wt .-%, lanthanum oxide.
  • the coating comprising the zeolites and the palladium
  • coating A the oxidation-catalytically active coating
  • coating B the oxidation-catalytically active coating
  • both coatings may be coated over the entire or only over a part of the length L of the carrier substrate.
  • coating A may extend from 10 to 80% of its length L and coating B, starting from the other end of the supporting body 10 to 80% of its length LA.
  • L LA + LB
  • LA the length of the coating A
  • LB the length of the coating B.
  • L> LA + LB can also apply if part of the support body remains free of coatings. In the latter case, between the coatings A and B remains a gap which is at least 0.5 cm long, that is for example 0.5 to 1 cm.
  • the coatings A and B may also both be coated over the entire length L.
  • the coatings A and B may also both be coated over the entire length L.
  • Coating B directly on the carrier substrate and the coating A on coating B are present.
  • the coating A may also be present directly on the carrier substrate and the coating B on the coating A.
  • a coating extends over the entire length of the support body and the other only over a part thereof.
  • a zeolite of the type FER, MEL, MTT, MWW or SZR, in particular MWW, which is occupied by 1 to 2% by weight, in particular 1.5 to 2% by weight, of palladium lies directly on the
  • Carrier substrate over its entire length L and on this coating is a platinum or platinum and palladium in the mass ratio of 4: 1 to 14: 1 containing coating also over the entire length L.
  • the lower layer for example Pd-FER or Pd-MWW
  • the upper layer in an amount of 50 to 100 g / l Carrier substrate before.
  • the carrier substrate is a wall-flow filter
  • the coatings can on the walls of the input channels, on the walls of the output channels or in the walls between input and output channels.
  • the carrier substrate is the zeolite, whose largest channels are from 10
  • tetrahedrally coordinated atoms are formed, palladium and a matrix component formed.
  • catalyst substrates used inert materials can be used. These are, for example, silicates, oxides, nitrides or carbides, with particular preference being given to magnesium-aluminum silicates.
  • the extruded carrier substrate comprising the zeolites, the largest channels of which are formed of tetrahedrally coordinated atoms, and palladium may in embodiments of the present invention be coated with one or more catalytically active coatings, for example with the above-described oxidation-catalytically active coating.
  • the catalyst of the invention is outstandingly useful as a passive nitrogen oxide storage catalyst, i. it is able to store nitrogen oxides at temperatures below 200 ° C and to recycle them at temperatures above 200 ° C.
  • the present invention thus also relates to the use of a
  • a catalyst comprising a carrier substrate of length L, palladium and a zeolite, the largest channels of which are formed by 10 tetrahedrally coordinated atoms, as a passive nitrogen oxide storage catalyst containing nitrogen oxides in stores a first temperature range and in a second
  • the present invention relates to the use of a catalyst comprising a carrier substrate of length L, a structure-type zeolite MWW, for example MCM-22, ERB-1, ITQ-1, PSH-3 or SSZ-25, and palladium as the sole metal in in an amount of 1.5 to 10% by weight, based on the sum of the weights of zeolite and palladium and calculated as palladium metal, and no zeolites whose largest channels are not formed by 10 tetrahedrally coordinated atoms.
  • a catalyst comprising a carrier substrate of length L, a structure-type zeolite MWW, for example MCM-22, ERB-1, ITQ-1, PSH-3 or SSZ-25, and palladium as the sole metal in in an amount of 1.5 to 10% by weight, based on the sum of the weights of zeolite and palladium and calculated as palladium metal, and no zeolites whose largest channels are not formed by 10 tetrahedrally coordinated atoms
  • the catalyst according to the invention in combination with a downstream SCR catalyst, allows nitrogen oxides over the entire
  • Temperature range of the exhaust gas including the cold start temperatures to implement effectively.
  • the present invention thus also relates to an exhaust gas system comprising a) a catalyst tetrahedrally coordinating a carrier substrate of length L, palladium and a zeolite whose largest channels of 10
  • Atoms are formed, includes and
  • the SCR catalyst in the exhaust system according to the invention can in principle be selected from all in the SCR reaction of nitrogen oxides with
  • Catalysts based on zeolites in particular transition metal-exchanged zeolites.
  • SCR catalysts that have a small pore zeolite with a maximum
  • Ring size of eight tetrahedral atoms and a transition metal included used.
  • SCR catalysts are described, for example, in WO2008 / 106519 A1, WO2008 / 118434 A1 and WO2008 / 132452 A2.
  • large and medium pore zeolites can be used, in particular those of the structure type BEA come into question.
  • iron BEA and copper BEA are of interest.
  • zeolites belong to the framework types BEA, AEI, CHA, KFI, ERI, LEV, MER or DDR and are particularly preferred with cobalt, iron, copper or mixtures of two or three of these metals
  • zeolites also includes molecular sieves, sometimes referred to as "zeolite-like" compounds
  • Preferred zeolites are furthermore those which have a SAR (silica-to-alumina ratio) value of from 2 to 100, in particular from 5 to 50.
  • SAR silicon-to-alumina ratio
  • the zeolites or molecular sieves contain transition metal, in particular in amounts of from 1 to 10% by weight, in particular from 2 to 5% by weight, calculated as metal oxide, ie for example as Fe 2 O 3 or CuO.
  • Preferred embodiments of the present invention include SCR catalysts with copper, iron or copper and iron exchanged zeolites or beta-type molecular sieves (BEA), chabazite type (CHA) or Levyne type (LEV).
  • BEA beta-type molecular sieves
  • CHA chabazite type
  • LEV Levyne type
  • Corresponding zeolites or molecular sieves are
  • the exhaust system according to the invention is located between the catalyst, which is a carrier substrate of length L,
  • 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).
  • the ammonia can be introduced via the injection device as such or in the form of a compound in the exhaust stream from which ammonia is formed at 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 SCR catalyst is preferably in the form of a coating on a supporting body, which may be a flow-through substrate or a wall-flow filter and may consist, for example, of silicon carbide, aluminum titanate or cordierite.
  • the support body itself may consist of the SCR catalyst and a matrix component as described above, that is, in extruded form.
  • the present invention also relates to a method for purifying exhaust gases of motor vehicles which are operated with lean-burn engines, such as diesel engines, characterized in that the exhaust gas is passed through an exhaust system according to the invention.
  • a zeolite of the structural type FER is impregnated with 3% by weight of palladium (from commercially available palladium nitrate) ("incipient
  • Ceramic substrate (flow-through substrate) over its entire length coated by a conventional method.
  • the washcoat loading is 50 g / L, based on the Pd-containing zeolite (equivalent to 54 g / L including binder), which corresponds to a precious metal loading of 42.5 g / ft 3 Pd.
  • the catalyst thus obtained is calcined at 550 ° C.
  • Example 1 is repeated with the difference that the ceramic substrate is coated with 100 g / l Pd-containing zeolite (corresponds to 108 g / L including binder). This corresponds to a noble metal loading of 85 g / ft 3 Pd.
  • Example 1 is repeated with the difference that the ceramic substrate is coated with 200 g / l Pd-containing zeolite (corresponds to 216 g / L including binder). This corresponds to a noble metal loading of 170 g / ft 3 Pd.
  • Example 4 Example 2 is repeated with the difference that the zeolite is impregnated with 1.5% by weight of palladium. This corresponds to a noble metal loading of 42.5 g / ft 3 Pd.
  • Example 5
  • Example 3 is repeated with the difference that the zeolite is impregnated with 1.5% by weight of palladium. This corresponds to a noble metal loading of 85 g / ft 3 Pd.
  • Example 6 is repeated with the difference that the zeolite is impregnated with 1.5% by weight of palladium. This corresponds to a noble metal loading of 85 g / ft 3 Pd.
  • Example 3 is repeated with the difference that the zeolite is impregnated with 0.75 wt .-% palladium. This corresponds to a noble metal loading of 42.5 g / ft 3 Pd.
  • Example 7
  • the catalyst obtained according to Example 5 is also coated in a further step by a conventional method also over its entire length with a washcoat containing platinum supported on alumina.
  • the washcoat loading of the second layer is 75 g / L, the platinum loading is 20 g / ft 3 .
  • the catalyst of Example 7 is combined with a second coated flow-through substrate to form an exhaust system.
  • the second flow-through substrate is exchanged with a zeolite of the structure type chabazite exchanged with 3% by weight of copper (calculated as CuO).
  • the washcoat loading of the second flow substrate is 150 g / L.
  • Example 1 is repeated with the difference that a structure-type zeolite MWW was used.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Biomedical Technology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Toxicology (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Catalysts (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)
  • Exhaust Gas After Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

L'invention concerne un catalyseur qui comprend un substrat de support, du palladium et une zéolite dont les canaux de taille supérieure sont formés par 10 atomes coordonnés de façon tétraédrique; l'utilisation de ce catalyseur en tant qu'adsorbant passif d'oxyde d'azote ; un système d'échappement contenant ce dernier et un catalyseur SCR ; et un procédé de purification de gaz d'échappement de véhicules à moteur à l'aide de ce système d'échappement.
EP18758622.7A 2017-08-31 2018-08-24 Catalyseur adsorbant passif d'oxyde d'azote à base de palladium-zéolite pour la purification de gaz d'échappement Pending EP3676000A1 (fr)

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EP17188770 2017-08-31
PCT/EP2018/072868 WO2019042883A1 (fr) 2017-08-31 2018-08-24 Catalyseur adsorbant passif d'oxyde d'azote à base de palladium-zéolite pour la purification de gaz d'échappement

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CN111032215A (zh) 2020-04-17
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JP2020531240A (ja) 2020-11-05
KR20200045550A (ko) 2020-05-04

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