DE102008009672B4 - Hydrocarbon storage function SCR catalyst, its use and emission control system and its use - Google Patents
Hydrocarbon storage function SCR catalyst, its use and emission control system and its use Download PDFInfo
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- DE102008009672B4 DE102008009672B4 DE102008009672.5A DE102008009672A DE102008009672B4 DE 102008009672 B4 DE102008009672 B4 DE 102008009672B4 DE 102008009672 A DE102008009672 A DE 102008009672A DE 102008009672 B4 DE102008009672 B4 DE 102008009672B4
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- catalyst
- scr
- hydrocarbon storage
- scr catalyst
- oxidation
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Abstract
SCR-Katalysator, umfassend eine SCR-aktive Komponente, eine Kohlenwasserstoffspeicherkomponente und einen Oxidationskatalysator, wobei der Oxidationskatalysator als katalytisch aktive Komponente Rhodium enthält und die SCR-aktive Komponente einen Katalysator auf Basis von Vanadium, Wolfram und Titan umfasst und wobei die SCR-aktive Komponente und die Kohlenwasserstoffspeicherkomponente als Beschichtung auf einem Katalysatorträger vorliegt, der Oxidationskatalysator als Beschichtung im Austrittsbereich des SCR-Katalysators vorliegt und 15–20% der Fläche des SCR-Katalysators mit dem Oxidationskatalysator beschichtet sind, dadurch gekennzeichnet, dass die Kohlenwasserstoffspeicherkomponente ein Zeolith vom Typ MFI ist.An SCR catalyst comprising an SCR active component, a hydrocarbon storage component and an oxidation catalyst, wherein the oxidation catalyst comprises rhodium as the catalytically active component and the SCR active component comprises a vanadium, tungsten and titanium based catalyst and wherein the SCR active component and the hydrocarbon storage component is present as a coating on a catalyst support, the oxidation catalyst is present as a coating in the exit region of the SCR catalyst and 15-20% of the surface of the SCR catalyst is coated with the oxidation catalyst, characterized in that the hydrocarbon storage component is an MFI type zeolite ,
Description
Die vorliegende Erfindung betrifft einen SCR-Katalysator, umfassend eine SCR-aktive Komponente, eine Kohlenwasserstoffspeicherkomponente und einen Oxidationskatalysator, wobei der Oxidationskatalysator als katalytisch aktive Komponente Rhodium enthält und die SCR-aktive Komponente einen Katalysator auf Basis von Vanadium, Wolfram und Titan umfasst und wobei die SCR-aktive Komponente und die Kohlenwasserstoffspeicherkomponente als Beschichtung auf einem Katalysatorträger vorliegt, der Oxidationskatalysator als Beschichtung im Austrittsbereich des SCR-Katalysators vorliegt und 15–20% der Fläche des SCR-Katalysators mit dem Oxidationskatalysator beschichtet sind, dadurch gekennzeichnet, dass die Kohlenwasserstoffspeicherkomponente ein Zeolith vom Typ MFI ist. Die Erfindung betrifft ferner eine Katalysatoranordnung, welche den erfindungsgemäßen SCR-Katalysator umfasst.The present invention relates to an SCR catalyst comprising an SCR active component, a hydrocarbon storage component and an oxidation catalyst, wherein the oxidation catalyst contains rhodium as a catalytically active component and the SCR active component comprises a catalyst based on vanadium, tungsten and titanium and wherein the SCR active component and the hydrocarbon storage component are present as a coating on a catalyst support, the oxidation catalyst is present as a coating in the exit region of the SCR catalyst and 15-20% of the surface of the SCR catalyst is coated with the oxidation catalyst, characterized in that the hydrocarbon storage component Zeolite of the type MFI is. The invention further relates to a catalyst arrangement which comprises the SCR catalyst according to the invention.
Ein Abgassystem für Dieselverbrennungsmotoren besteht in der Regel aus den folgenden Komponenten:
- • DOC zur Oxidation von Kohlenwasserstoffen und als Kohlenwasserstoffspeicher im Kaltstart;
- • DPF zur Verminderung der Partikelemissionen;
- • optional ein H-Katalysator zur Harnstoffaufbereitung;
- • SCR-Katalysator zur Reduktion der Stickoxide;
- • Sperrkatalysator als Ammoniak-Oxidationskatalysator.
- • DOC for the oxidation of hydrocarbons and as hydrocarbon storage in cold start;
- • DPF to reduce particulate emissions;
- • optional H catalyst for urea processing;
- • SCR catalyst for the reduction of nitrogen oxides;
- • Blocking catalyst as ammonia oxidation catalyst.
Unter DOC (Diesel-Oxidationskatalysator) versteht der Fachmann einen Katalysator, welcher einerseits im Kaltstart eine Kohlenwasserstoff-Speicherfunktion erfüllt und im Normalbetrieb unverbrannte Kohlenwasserstoffe oxidiert. Die Behandlung der Abgase von Dieselverbrennungsmotoren mit Katalysatoren erfordert konzeptionelle Änderungen an den Katalysatormaterialien, da ein Dieselmotor im Gegensatz zu einem Benzinmotor immer unter Sauerstoffüberschuss betrieben wird und der Katalysator somit nie reduktiven Bedingungen ausgesetzt ist.DOC (Diesel Oxidation Catalyst) is understood by the person skilled in the art to mean a catalyst which, on the one hand, performs a hydrocarbon storage function during a cold start and oxidizes unburned hydrocarbons in normal operation. The treatment of the exhaust gases of diesel engines with catalytic converters requires conceptual changes to the catalyst materials, since a diesel engine is always operated in excess of oxygen, unlike a gasoline engine and thus the catalyst is never exposed to reductive conditions.
Partikelfilter (DPF, Dieselpartikelfilter) werden eingesetzt, um Rußpartikel aus dem Abgas von Verbrennungsmotoren, speziell Dieselmotoren, herauszufiltern und so deren Ausstoß in die Atmosphäre zu vermindern. Dabei kommen verschiedene Filterkonzepte, wie z. B. so genannte „Wall-flow-Filter” oder Filter aus keramischen oder metallischen Schäumen zur Anwendung. Die eigentliche Schwierigkeit besteht aber nicht in der Filtration der Rußpartikel, sondern in der Regeneration der eingesetzten Filter. Kohlenstoffruß verbrennt je nach betriebsbedingter Zusammensetzung der Partikel spontan erst bei Temperaturen zwischen 500°C und 700°C. Diese Temperaturen werden aber z. B. von modernen Dieselmotoren im Allgemeinen nur bei Volllast erreicht.Particulate filters (DPF, diesel particulate filters) are used to filter soot particles from the exhaust gas of internal combustion engines, especially diesel engines, and thus to reduce their emission into the atmosphere. Here are various filter concepts, such. As so-called "wall-flow filter" or filters made of ceramic or metallic foams for use. The real difficulty is not in the filtration of the soot particles, but in the regeneration of the filter used. Carbon black burns spontaneously depending on the operational composition of the particles only at temperatures between 500 ° C and 700 ° C. These temperatures are but z. B. of modern diesel engines generally achieved only at full load.
Daher sind zusätzliche unterstützende Maßnahmen, beispielsweise zur Oxidation der aus dem Abgas abgetrennten Rußpartikel, notwendig. Dies kann durch Zusatz von Additiven oder durch eine katalytische Beschichtung der Filter oder Katalysatoren geschehen. Aus dem Stand der Technik sind Abgasreinigungskatalysatoren mit einer hohen Oxidationswirkung bekannt, so dass die Partikel bei einer tiefen Temperatur verbrannt werden können. Die Oberfläche der Filterkammer weist deshalb oft eine katalytisch aktive Beschichtung zur Beschleunigung der Verbrennung der auf dem Filter gesammelten Rußpartikel auf. Die katalytisch aktive Beschichtung oxidiert das im Abgas enthaltene Stickstoffmonoxid zu Stickstoffdioxid. Das entstandene Stickstoffdioxid verbessert dann die Oxidation der abgelagerten Partikel.Therefore, additional supporting measures, for example, for the oxidation of the separated from the exhaust soot particles, necessary. This can be done by adding additives or by a catalytic coating of the filters or catalysts. Exhaust gas purifying catalysts having a high oxidation effect are known in the prior art, so that the particles can be burned at a low temperature. Therefore, the surface of the filter chamber often has a catalytically active coating for accelerating the combustion of the soot particles collected on the filter. The catalytically active coating oxidizes the nitrogen monoxide contained in the exhaust gas to nitrogen dioxide. The resulting nitrogen dioxide then improves the oxidation of the deposited particles.
Mit SCR (selective catalytic reduction) wird die selektive katalytische Reduktion von Stickoxiden aus Abgasen von Verbrennungsmotoren (und auch Kraftwerken) bezeichnet. Mit einem SCR-Katalysator werden nur die Stickoxide NO und NO2 selektiv reduziert, wobei für die Reaktion gewöhnlich NH3 (Ammoniak) zugemischt wird. Als Reaktionsprodukt entstehen nur die unbedenklichen Stoffe Wasser und Stickstoff. Für den Einsatz in Kraftfahrzeugen ist das Mitführen von Ammoniak in Druckgasflaschen ein Sicherheitsrisiko. Deshalb werden gewöhnlich Vorläuferverbindungen des Ammoniaks eingesetzt, die im Abgasstrang der Fahrzeuge unter Ammoniakbildung zersetzt werden. Bekannt in diesem Zusammenhang ist beispielsweise die Verwendung von Ad-Blue®, welches eine etwa 32,5%-ige eutektische Lösung von Harnstoff in Wasser ist. Andere Ammoniakquellen sind beispielsweise Ammoniumcarbamat, Ammoniumformiat oder Harnstoffpellets. Oftmals wird deshalb auch noch ein Hydrolysekatalysator (H-Kat) eingesetzt, welcher aus den Vorläufersubstanzen NH3 generiert.Selective catalytic reduction (SCR) refers to the selective catalytic reduction of nitrogen oxides from exhaust gases of combustion engines (and also power plants). With an SCR catalyst, only the nitrogen oxides NO and NO 2 are selectively reduced, with NH 3 (ammonia) usually added to the reaction. The reaction product is only the harmless substances water and nitrogen. For use in motor vehicles, carrying ammonia in pressurized gas cylinders poses a safety risk. Therefore, precursor compounds of ammonia are usually used, which are decomposed in the exhaust line of the vehicles with formation of ammonia. Known in this context is, for example, the use of Ad- Blue® , which is an approximately 32.5% eutectic solution of urea in water. Other sources of ammonia include ammonium carbamate, ammonium formate or urea pellets. Often therefore also a hydrolysis catalyst (H-Cat) is used, which generates from the precursors NH 3 .
Vor der eigentlichen SCR-Reaktion muss aus Harnstoff zunächst Ammoniak gebildet werden. Dies geschieht in zwei Reaktionsschritten, die zusammengefasst als Hydrolysereaktion bezeichnet werden. Zunächst werden in einer Thermolysereaktion NH3 und Isocyansäure gebildet. Anschließend wird in der eigentlichen Hydrolysereaktion Isocyansäure mit Wasser zu Ammoniak und Kohlendioxid umgesetzt.Before the actual SCR reaction, ammonia must first be formed from urea. This is done in two reaction steps, collectively referred to as the hydrolysis reaction. First, NH 3 and isocyanic acid are formed in a thermolysis reaction. Isocyanic acid is then reacted with water to form ammonia and carbon dioxide in the actual hydrolysis reaction.
Zur Vermeidung von festen Ausscheidungen ist es erforderlich, dass die zweite Reaktion durch die Wahl geeigneter Katalysatoren und genügend hoher Temperaturen (ab 250°C) ausreichend schnell erfolgt. Moderne SCR-Reaktoren übernehmen gleichzeitig die Funktion des Hydrolysekatalysators.To avoid solid precipitates, it is necessary that the second reaction by the choice of suitable catalysts and sufficiently high temperatures (from 250 ° C) is sufficiently fast. Modern SCR reactors simultaneously take over the function of the hydrolysis catalyst.
Das durch die Thermohydrolyse entstandene Ammoniak reagiert am SCR-Katalysator nach den folgenden Gleichungen:
Bei niedrigen Temperaturen (< 300°C) läuft der Umsatz überwiegend über Reaktion (2) ab. Für einen guten Niedertemperaturumsatz ist es deshalb erforderlich, ein NO2:NO-Verhältnis von etwa 1:1 einzustellen. Unter diesen Umständen kann die Reaktion (2) bereits bei Temperaturen ab 170–200°C erfolgen.At low temperatures (<300 ° C), the conversion proceeds predominantly via reaction (2). For a good low-temperature conversion, it is therefore necessary to set a NO 2 : NO ratio of about 1: 1. Under these circumstances, reaction (2) can take place at temperatures as low as 170-200 ° C.
Die Oxidation von NO zu NOX erfolgt in einem vorgelagerten Oxidationskatalysator der für einen optimalen Wirkungsgrad erforderlich ist.The oxidation of NO to NO X takes place in an upstream oxidation catalyst which is required for optimum efficiency.
Wird mehr Reduktionsmittel dosiert, als bei der Reduktion mit NOX umgesetzt wird, so kann es zu einem unerwünschten NH3-Schlupf kommen. Die Entfernung des NH3 kann durch einen zusätzlichen Oxidationskatalysator hinter dem SCR-Katalysator erzielt werden. Dieser Sperrkatalysator oxidiert das gegebenenfalls auftretende Ammoniak zu N2 und H2O. Darüber hinaus ist eine sorgfältige Applikation der Harnstoffdosierung unerlässlich.If more reducing agent is metered than is reacted during the reduction with NO X , undesired NH 3 slip may occur. The removal of the NH 3 can be achieved by an additional oxidation catalyst downstream of the SCR catalyst. This barrier catalyst oxidizes the possibly occurring ammonia to N 2 and H 2 O. In addition, careful application of the urea dosage is essential.
Eine für die SCR-Katalyse wichtige Kenngröße ist das so genannte Feedverhältnis α, definiert als das molare Verhältnis von zudosiertem NH3 zu dem im Abgas vorhandenen NOX. Bei idealen Betriebsbedingungen (kein NH3-Schlupf, keine Nebenreaktionen, keine NH3-Oxidation) ist α direkt proportional zur NOX-Reduktionsrate:
Bei α = 1 wird theoretisch eine einprozentige NOX-Reduktion erreicht. Im praktischen Einsatz kann bei einem NH3-Schlupf von < 20 ppm eine NOX-Reduktion von 90% im stationären und instationären Betrieb erzielt werden.An important parameter for SCR catalysis is the so-called feed ratio α, defined as the molar ratio of metered NH 3 to the NO X present in the exhaust gas. Under ideal operating conditions (no NH 3 slip, no side reactions, no NH 3 oxidation), α is directly proportional to the NO x reduction rate:
At α = 1 theoretically a one percent NO x reduction is achieved. In practical use, with NH 3 slip of <20 ppm, a NO x reduction of 90% in stationary and transient operation can be achieved.
Durch die vorgelagerte Hydrolysereaktion wird bei den heutigen SCR-Katalysatoren ein NOX-Umsatz > 50% erst bei Temperaturen oberhalb von ca. 250°C erreicht, optimale Umsatzraten werden im Temperaturfenster von 250–450°C erzielt.Due to the upstream hydrolysis reaction, an NO X conversion of> 50% is achieved in today's SCR catalysts only at temperatures above about 250 ° C, optimum conversion rates are achieved in the temperature window of 250-450 ° C.
Die Dosierstrategie ist bei Katalysatoren mit hohem NH3-Speichervermögen von großer Wichtigkeit, da die NH3-Speicherfähigkeit von SCR-Katalysatoren des Standes der Technik typischerweise mit steigender Temperatur abnimmt.The dosing strategy is of great importance in high NH 3 storage capacity catalysts because the NH 3 storage capability of prior art SCR catalysts typically decreases with increasing temperature.
Derzeit werden sowohl im Kraftwerksbereich als auch im Automobilbereich überwiegend SCR-Katalysatoren auf Basis von Titandioxid, Vanadiumpentaoxid und Wolframoxid eingesetzt. Auch ist die Verwendung von SCR-Katalysatoren auf Basis von Zeolithen im Stand der Technik bekannt. In diesem Fall fungiert der Zeolith jedoch lediglich als SCR-aktive Komponente.At present, SCR catalysts based on titanium dioxide, vanadium pentaoxide and tungsten oxide are predominantly used both in the power plant sector and in the automotive sector. Also, the use of SCR catalysts based on zeolites is known in the art. In this case, however, the zeolite functions only as an SCR-active component.
Ferner wird gemäß Stand der Technik häufig ein Ammoniak-Sperrkatalysator verwendet, welcher überschüssiges Ammoniak aus dem SCR-Katalysator oxidiert, da Ammoniak sehr schädlich für die Gesundheit und die Umwelt ist.Further, in the prior art, an ammonia trap catalyst is often used which oxidizes excess ammonia from the SCR catalyst since ammonia is very detrimental to health and the environment.
Wie zu erkennen ist, umfasst ein modernes Abgassystem eine Vielzahl von Komponenten welche gewöhnlich am Fahrzeugboden im Abgasstrang integriert sind. Da dort der zur Verfügung stehende Raum begrenzt ist, wäre es somit wünschenswert, wenn der zur Verfügung stehende Raum effektiver genutzt werden könnte.As can be seen, a modern exhaust system includes a plurality of components which are usually integrated on the vehicle floor in the exhaust line. Since the available space is limited there, it would be desirable if the available space could be used more effectively.
Beispiele für die Kombination von SCR-Katalysatoren und Kohlenwasserstoffspeicherkomponenten sind aus den Druckschriften
Die Aufgabe wird gelöst durch einen SCR-Katalysator, umfassend eine SCR-aktive Komponente, eine Kohlenwasserstoffspeicherkomponente und einen Oxidationskatalysator, wobei der Oxidationskatalysator als katalytisch aktive Komponente Rhodium enthält und die SCR-aktive Komponente einen Katalysator auf Basis von Vanadium, Wolfram und Titan umfasst und wobei die SCR-aktive Komponente und die Kohlenwasserstoffspeicherkomponente als Beschichtung auf einem Katalysatorträger vorliegt, der Oxidationskatalysator als Beschichtung im Austrittsbereich des SCR-Katalysators vorliegt und 15–20% der Fläche des SCR-Katalysators mit dem Oxidationskatalysator beschichtet sind, dadurch gekennzeichnet, dass die Kohlenwasserstoffspeicherkomponente ein Zeolith vom Typ MFI ist.The object is achieved by an SCR catalyst comprising an SCR active component, a hydrocarbon storage component and an oxidation catalyst, wherein the oxidation catalyst contains rhodium as the catalytically active component and the SCR active component comprises a catalyst based on vanadium, tungsten and titanium and wherein the SCR active component and the hydrocarbon storage component are present as a coating on a catalyst support, the oxidation catalyst is present as a coating in the exit region of the SCR catalyst and 15-20% of the surface of the SCR catalyst coated with the oxidation catalyst, characterized in that the hydrocarbon storage component is an MFI type zeolite.
Die Aufgabe wird ferner gelöst durch ein Abgasreinigungssystem welches
- • einen Rußpartikelfilter (DPF) und
- • einen SCR-Katalysator umfasst und dadurch gekennzeichnet ist, dass der SCR-Katalysator eine SCR-aktive Komponente, eine Kohlenwasserstoffspeicherkomponente und einen Oxidationskatalysator umfasst, wobei der Oxidationskatalysator als katalytisch aktive Komponente Rhodium enthält und die SCR-aktive Komponente einen Katalysator auf Basis von Vanadium, Wolfram und Titan umfasst und wobei die SCR-aktive Komponente und die Kohlenwasserstoffspeicherkomponente als Beschichtung auf einem Katalysatorträger vorliegt, der Oxidationskatalysator als Beschichtung auf dem Katalysatorträger im Austrittsbereich des SCR-Katalysators aufgebracht ist, 15–20% der Fläche des SCR-Katalysators mit dem Oxidationskatalysator beschichtet sind und die Kohlenwasserstoffspeicherkomponente ein Zeolith vom Typ MFI ist.
- • a particulate filter (DPF) and
- Comprising an SCR catalyst and characterized in that the SCR catalyst comprises an SCR active component, a hydrocarbon storage component and an oxidation catalyst, wherein the oxidation catalyst contains rhodium as catalytically active component and the SCR active component contains a catalyst based on vanadium , Tungsten and titanium and wherein the SCR active component and the hydrocarbon storage component is present as a coating on a catalyst support, the oxidation catalyst as a coating on the Catalyst support is applied in the exit region of the SCR catalyst, 15-20% of the surface of the SCR catalyst are coated with the oxidation catalyst and the hydrocarbon storage component is an MFI type zeolite.
Überaschend konnte gefunden werden, dass mehrere Katalysatorfunktionen in einzelnen Katalysatorbauteilen kombiniert werden können, wodurch eine enorme Verringerung des Raumbedarfs resultiert.Surprisingly, it could be found that several catalyst functions can be combined in individual catalyst components, resulting in a huge reduction in space requirements.
Geeignete Katalysatorträger können metallische oder keramische Träger sein. Bevorzugt ist der Katalysatorträger ein monolithischer Träger.Suitable catalyst supports may be metallic or ceramic supports. Preferably, the catalyst support is a monolithic support.
Der erfindungsgemäße SCR-Katalysator umfasst eine Kohlenwasserstoffspeicherkomponente, welche ein Zeolith vom Typ MFI ist. Die Kohlenwasserstoffspeicherkomponente kann einen Zeolithen vom Typ MFI in der H-Form oder einen metallausgetauschten Zeolithen vom Typ MFI umfassen. Die Herstellungsverfahren für einen metallausgetauschten Zeolith vom Typ MFI, beispielsweise über Fest- oder Flüssigphasenaustausch, sowie für einen Zeolith vom Typ MFI in der H-Form sind dem Fachmann bekannt.The SCR catalyst of the invention comprises a hydrocarbon storage component which is an MFI type zeolite. The hydrocarbon storage component may comprise an MFI zeolite in H-form or a metal-exchanged MFI zeolite. The production processes for a metal-exchanged MFI type zeolite, for example by solid or liquid phase exchange, and for an H-form MFI zeolite are known to those skilled in the art.
Ein metallausgetauschter Zeolith vom Typ MFI hat ferner den Vorteil, dass dieser bi-funktionell ist, d. h. dass er sowohl eine SCR-Aktivität als auch eine Kohlenwasserstoffspeicheraktivität besitzt.A metal-exchanged MFI type zeolite also has the advantage of being bi-functional, i. H. that it has both an SCR activity and a hydrocarbon storage activity.
Die SCR-aktive Komponente umfasst weiterhin einen Katalysator auf Basis von Vanadium, Wolfram und Titan.The SCR active component further comprises a catalyst based on vanadium, tungsten and titanium.
Unter dem Begriff „Zeolith” wird im Rahmen der vorliegenden Erfindung gemäß der Definition der International Mineralical Association (D. S. Coombs et al., Canadian Mineralogist, 35, 1979, 1571) eine kristalline Substanz aus der Gruppe der Aluminiumsilikate mit einer Raumnetzstruktur der allgemeinen Formel
Das Verhältnis von Si/Al = y/x beträgt immer > 1 gemäß der sog. „Löwenstein-Regel”, die das benachbarte Auftreten zweier benachbarter negativ geladener AlO4-Tetraeder verbietet. Dabei stehen bei einem geringen Si/Al-Verhältnis zwar mehr Austauschplätze für Metall zur Verfügung, der Zeolith wird jedoch zunehmend thermisch instabiler.The ratio of Si / Al = y / x is always> 1 according to the so-called "Löwenstein rule", which prohibits the adjacent occurrence of two adjacent negatively charged AlO 4 tetrahedra. Although there are more exchange sites for metal available at a low Si / Al ratio, the zeolite is becoming increasingly thermally unstable.
Die Zeolithstruktur enthält Hohlräume, Kanäle, die für jeden Zeolithen charakteristisch sind. Die Zeolithe werden gemäß ihrer Topologie in verschiedene Strukturen eingeteilt. Das Zeolithgerüst enthält offene Hohlräume in Form von Kanälen und Käfigen, die normalerweise mit Wassermolekülen und zusätzlichen Gerüstkationen besetzt sind, die ausgetauscht werden können. Auf ein Aluminiumatom kommt eine überschüssige negative Ladung, die durch diese Kationen kompensiert wird. Das Innere des Porensystems stellt die katalytisch aktive Oberfläche dar. Je mehr Aluminium und je weniger Silizium ein Zeolith enthält, desto dichter ist die negative Ladung in seinem Gitter und desto polarer seine innere Oberfläche. Die Porengröße und Struktur wird neben den Parametern bei der Herstellung, d. h. Verwendung bzw. Art von Templaten, pH, Druck, Temperatur, Anwesenheit von Impfkristallen, durch das Si/Al-Verhältnis bestimmt, das den größten Teil des katalytischen Charakters eines Zeolithen ausmacht.The zeolite structure contains voids, channels that are characteristic of each zeolite. The zeolites are classified into different structures according to their topology. The zeolite framework contains open cavities in the form of channels and cages that are normally occupied by water molecules and additional framework cations that can be exchanged. An aluminum atom has an excess negative charge which is compensated by these cations. The interior of the pore system represents the catalytically active surface. The more aluminum and the less silicon a zeolite contains, the denser the negative charge in its lattice and the more polar its internal surface. The pore size and structure is in addition to the parameters in the production, d. H. Use or type of templates, pH, pressure, temperature, presence of seed crystals, determined by the Si / Al ratio, which accounts for most of the catalytic character of a zeolite.
Durch Anwesenheit von zwei- oder dreiwertigen Kationen als Tetraederzentrum im Zeolithgerüst erhält der Zeolith eine negative Ladung in Form von sog. Anionenstellen, in deren Nachbarschaft sich die entsprechenden Kationenpositionen befinden.The presence of divalent or trivalent cations as a tetrahedral center in the zeolite framework gives the zeolite a negative charge in the form of so-called anion sites, in the vicinity of which the corresponding cation positions are located.
Die negative Ladung wird durch den Einbau von Kationen in die Poren des Zeolithmaterials kompensiert. Die Zeolithe unterscheidet man hauptsächlich nach der Geometrie der Hohlräume, die durch das starre Netzwerk der SiO4/AlO4-Tetraeder gebildet werden. Die Eingänge zu den Hohlräumen werden von 8, 10 oder 12 Ringen gebildet, der Fachmann spricht hier von eng-, mittel- und weitporigen Zeolithen. Bestimmte Zeolithe zeigen einen gleichförmigen Strukturaufbau, z. B. die ZSM-5- oder die MFI-Topologie, mit linearen oder zickzack-förmig verlaufenden Kanälen, bei anderen schließen sich hinter den Porenöffnungen größere Hohlräume an, z. B. bei den Y- oder A-Zeolithen, mit den Topologien FAO und LTA.The negative charge is compensated by the incorporation of cations in the pores of the zeolite material. The zeolites are mainly distinguished by the geometry of the cavities formed by the rigid network of SiO 4 / AlO 4 tetrahedra. The entrances to the cavities are formed by 8, 10 or 12 rings, the expert speaks here of narrow, medium and large pore zeolites. Certain zeolites show a uniform structure structure, e.g. For example, the ZSM-5 or the MFI topology, with linear or zigzag-shaped channels, in others close behind the pore openings larger cavities, z. As in the Y or A zeolites, with the topologies FAO and LTA.
Vorzugsweise befindet sich das Zeolithmaterial vom Typ MFI der Kohlenwasserstoffspeicherkomponente an der Katalysatoreintrittsseite. Dies hat den Vorteil, dass der Katalysator damit auch die Funktion eines H-Katalysators (Hydrolyse-Katalysator) übernehmen kann, da der Zeolith vom Typ MFI auch ein Hydrolyse-Katalysator ist. Dadurch kann eine weitere Katalysatorfunktion in den SCR-Katalysator integriert werden, wodurch die Notwendigkeit eines optionalen Hydrolyse-Katalysators entfällt.Preferably, the MFI type zeolite material of the hydrocarbon storage component is at the catalyst entry side. This has the advantage that the catalyst can thus also assume the function of an H catalyst (hydrolysis catalyst), since the MFI type zeolite is also a hydrolysis catalyst. As a result, a further catalytic function can be integrated into the SCR catalyst, eliminating the need for an optional hydrolysis catalyst.
Gemäß der Anordnung des erfindungsgemäßen Abgasreinigungssystems soll der SCR-Katalysator zwischen dem Rußpartikelfilter (DPF) und dem Oxidationskatalysator angeordnet sein. Gemäß der erfindungsgemäßen Anordnung des Abgasreinigungssystems soll der Oxidationskatalysator ein Bestandteil des SCR-Katalysators sein. Dazu liegt der Oxidationskatalysator als Beschichtung auf dem Katalysatorträger des SCR-Katalysators vor. Die Beschichtung befindet sich an der Austrittsseite des SCR-Katalysators, wobei 15–20%, besonders bevorzugt etwa 20% der Fläche des SCR-Katalysators mit dem Oxidationskatalysator beschichtet ist.According to the arrangement of the exhaust gas purification system according to the invention, the SCR catalytic converter should be arranged between the soot particle filter (DPF) and the oxidation catalytic converter. According to the inventive arrangement of the exhaust gas purification system, the oxidation catalyst is a Be part of the SCR catalyst. For this purpose, the oxidation catalyst is present as a coating on the catalyst support of the SCR catalyst. The coating is on the exit side of the SCR catalyst with 15-20%, more preferably about 20% of the area of the SCR catalyst coated with the oxidation catalyst.
Der Oxidationskatalysator am Ende des Abgassystems übernimmt zwei Aufgaben. Zum einen die Oxidation der unverbrannten Kohlenwasserstoffe (HC) und Kohlemonoxide (CO) und zum anderen die Oxidation von NH3, der nicht bei der SCR-Reaktion umgesetzt wurde (NH3-Schlupf). Die unverbrannten Kohlenwasserstoffe der Kaltstartphase werden bei erhöhter Temperatur desorbiert und treffen dann auf den Oxidationskatalysator und werden zu CO2 umgesetzt. Durch diese Kombination kann der Ammoniak-Sperrkatalysator in den Oxidationskatalysator integriert werden, was wiederum eine Raumeinsparung mit sich bringt.The oxidation catalyst at the end of the exhaust system performs two tasks. On the one hand, the oxidation of the unburned hydrocarbons (HC) and carbon monoxide (CO) and on the other the oxidation of NH 3 , which was not implemented in the SCR reaction (NH 3 -slip). The unburned hydrocarbons of the cold start phase are desorbed at elevated temperature and then hit the oxidation catalyst and are converted to CO 2 . By this combination, the ammonia barrier catalyst can be integrated into the oxidation catalyst, which in turn brings a space saving.
Der DPF, der SCR-Katalysator und der Oxidationskatalysator sind als Beschichtungskatalysator ausgebildet. Allgemein können Katalysatoren in Vollkatalysatoren und Beschichtungskatalysatoren eingeteilt werden. Während Vollkatalysatoren zu über 50% aus einem katalytisch aktiven Material bestehen, bestehen Beschichtungskatalysatoren aus einem Katalysatorträgerkörper, der aus einem Metall oder einer Keramik bestehen kann, wobei die Oberfläche des Katalysatorträgerkörpers mit einer Beschichtung versehen ist. Die Beschichtung wird mittels einer sog. Washcoat-Suspension, d. h. einer Aufschlämmung in einem fluiden Medium auf den Katalysatorträger aufgetragen. Gewöhnlich wird anschließend die aufgetragene Washcoat-Suspension getrocknet und kalziniert. Die Beschichtung kann anschließend mit einer weiteren katalytisch aktiven Komponente imprägniert werden, wobei die aktiven Komponenten auch in der Washcoat-Suspension gelöst sein können oder zuvor auf den Metalloxidpartikeln aufgebracht worden sein. Der Vorteil von Beschichtungskatalysatoren besteht in der einfachen Herstellung, die mit einem geringen verfahrenstechnischen Aufwand verbunden ist. In Abgasreinigungsanlagen können mehrere einzelne Katalysatoren durch Parallelschaltung zu großen Katalysatoren kombiniert werden. Ein weiterer Vorteil von Beschichtungskatalysatoren ist, dass geringere Mengen an teuren Aktivkomponenten erforderlich sind.The DPF, the SCR catalyst and the oxidation catalyst are formed as a coating catalyst. In general, catalysts can be classified as full catalysts and coating catalysts. While full catalysts consist of more than 50% of a catalytically active material, coating catalysts consist of a catalyst carrier body, which may consist of a metal or a ceramic, wherein the surface of the catalyst carrier body is provided with a coating. The coating is applied by means of a so-called washcoat suspension, i. H. a slurry applied in a fluid medium on the catalyst support. Usually, the applied washcoat suspension is then dried and calcined. The coating can then be impregnated with a further catalytically active component, wherein the active components may also be dissolved in the washcoat suspension or have been previously applied to the metal oxide particles. The advantage of coating catalysts is the ease of production, which is associated with a low procedural effort. In emission control systems, several individual catalysts can be combined by parallel connection to large catalysts. Another advantage of coating catalysts is that smaller amounts of expensive active components are required.
In einer nicht erfindungsgemäßen Ausführungsform umfasst die Beschichtung des Beschichtungskatalysators (SCR und Oxidationskatalysator) einen mit Eisen dotierten Zeolithen und ein Metalloxid, wobei die Menge an eisendotierten Zeolithen in der Trockenmasse der Beschichtung zwischen 3 und 80 Gew.-%, bevorzugt zwischen 5 und 75 Gew.-% und am meisten bevorzugt zwischen 10 und 70 Gew.-% liegt.In a non-inventive embodiment, the coating of the coating catalyst (SCR and oxidation catalyst) comprises an iron-doped zeolite and a metal oxide, wherein the amount of iron-doped zeolites in the dry mass of the coating between 3 and 80 wt .-%, preferably between 5 and 75 wt % and most preferably between 10 and 70% by weight.
Bevorzugt ist das Metalloxid ausgewählt aus der Gruppe bestehend aus Aluminiumoxid, Siliziumoxid, Eisenoxid, Ceroxid, Zirkoniumoxid und einem aus den Metalloxiden ausgewählten Mischoxid. Diese Metalloxide gewährleisten die Herstellung eines Katalysators mit einer hohen Oberfläche. Ferner sind die ausgewählten Metalloxide besonders kostengünstig.The metal oxide is preferably selected from the group consisting of aluminum oxide, silicon oxide, iron oxide, cerium oxide, zirconium oxide and a mixed oxide selected from metal oxides. These metal oxides ensure the production of a high surface area catalyst. Furthermore, the selected metal oxides are particularly inexpensive.
Der Oxidationskatalysator umfasst Rhodium als katalytisch aktive Komponente.The oxidation catalyst comprises rhodium as a catalytically active component.
Gemäß der erfindungsgemäßen Katalysatoranordnung soll der Partikelfilter (DPF) als erste Komponente des Abgasreinigungssystems angeordnet sein.According to the catalyst arrangement according to the invention, the particulate filter (DPF) should be arranged as the first component of the exhaust gas purification system.
Für einen DPF sind eine Vielzahl von mit katalytisch aktiven Materialien beschichteten Trägern für Abgasfilter bzw. Abgaskatalysatoren bekannt. Vorzugsweise sind die katalytisch aktiven Schichten (geträgerter Katalysator) ausgewählt aus Aluminium-, Cer-, Wolfram-, Titan- und Zirkonoxid, die noch zusätzlich katalytisch aktive Edelmetalle zur Oxidation von Kohlenwasserstoffen, zur Oxidation von CO und von abgelagerten organischen Partikeln, wie z. B. Ruß und dergleichen enthalten.For a DPF, a large number of carriers coated with catalytically active materials for exhaust gas filters or catalytic converters are known. Preferably, the catalytically active layers (supported catalyst) are selected from aluminum, cerium, tungsten, titanium and zirconium, which additionally catalytically active precious metals for the oxidation of hydrocarbons, for the oxidation of CO and deposited organic particles such. As carbon black and the like.
Die Katalytisch aktiven Metalloxide oder ihre Hydroxide sind im Wesentlichen wasserunlöslich. Bevorzugt ist es daher, Aluminiumoxide als wässrige Aufschlämmung mit wasserlöslichen Salzen der Oxide, insbesondere Nitrate, Chloride, Hydroxide, Sulfite, Acetate oder Komplexverbindungen der katalytisch aktiven Metalle auf Substrate aufzubringen bzw. diese damit zu imprägnieren und diese Salze anschließend bei hohen Temperaturen zu zersetzen, wobei deren Oxide entstehen.The catalytically active metal oxides or their hydroxides are essentially water-insoluble. It is therefore preferred to apply aluminum oxides as an aqueous slurry with water-soluble salts of the oxides, in particular nitrates, chlorides, hydroxides, sulfites, acetates or complex compounds of the catalytically active metals on substrates or to impregnate them with these and then decompose these salts at high temperatures, wherein their oxides are formed.
Bevorzugt ist ferner eine kontinuierliche Regeneration des Partikelfilters, ohne dass z. B. eine periodische Nacheinspritzung von Kraftstoff zur Erhöhung der Abgastemperatur erforderlich ist. Um die Effizienz des Katalysators zu erhöhen, sollte daher eine große Oberfläche bereitgestellt werden, damit die katalytisch aktiven Zentren mit den Rußpartikeln in Berührung kommen können. Die dabei notwendige große Oberfläche wird beispielsweise dadurch erzeugt, dass eine Schicht eines Katalysatorträgers, wie beispielsweise oberflächenreiches gamma-Aluminiumoxid oder Titanoxid, auf einem Filtermaterial abgelagert wird und ein Metall, insbesondere ein Metall der Platingruppe, das als aktive Spezies für die Oxidation von Partikelmaterial bekannt ist, mittels einer Metallsalzlösung oder Metallkomplexverbindung in den Filter integriert wird.Furthermore, a continuous regeneration of the particulate filter is preferred, without z. B. a periodic post-injection of fuel to increase the exhaust gas temperature is required. In order to increase the efficiency of the catalyst, therefore, a large surface should be provided so that the catalytically active centers may come into contact with the soot particles. The large surface area required is generated, for example, by depositing a layer of a catalyst support, such as high surface area gamma-alumina or titania, on a filter material and a metal, particularly a platinum group metal, known as an active species for the oxidation of particulate matter is integrated into the filter by means of a metal salt solution or metal complex compound.
Für die katalytische Beschichtung von derartigen Substraten, insbesondere mit innerer Oberfläche, d. h. also poröse Substrate bzw. Metallmonolithe mit im Wesentlichen durchgehenden Kanälen, werden wie vorstehend schon ausgeführt unterschiedliche Beschichtungsverfahren und Beschichtungsmaterialien unter Verwendung von so genannten „washcoats” (worunter üblicherweise meist wässrige Aufschlämmungen von Feststoffen verstanden werden) verwendet. For the catalytic coating of such substrates, in particular with inner surface, ie, porous substrates or metal monoliths with substantially continuous channels, as already stated above, different coating methods and coating materials using so-called "washcoats" (which usually usually aqueous slurries of Solids).
Bevorzugte „Washcoats” im Sinne dieser Erfindung können eine Vielzahl von Oxiden umfassen, die katalytisch aktiv sind, wie beispielsweise La2O3, Co2O3, Nd2O3, TiO2, ZrO2, CeO2 etc., allein oder in Kombination.For the purposes of this invention, preferred "washcoats" may comprise a multiplicity of oxides which are catalytically active, for example La 2 O 3 , Co 2 O 3 , Nd 2 O 3 , TiO 2 , ZrO 2 , CeO 2, etc., alone or in combination.
Weitere bevorzugte Kombinationen umfassen beispielsweise ein Aluminiumoxid mit hoher Oberfläche, des Weiteren Zinkoxid und wenigstens ein Edelmetall aus der Gruppe bestehend aus Palladium, Platin, Rhodium oder einer Kombination davon, die ebenfalls auf einem monolithischen Träger mittels eines Washcoats aufgebracht werden.Further preferred combinations include, for example, a high surface area alumina, further zinc oxide, and at least one noble metal selected from the group consisting of palladium, platinum, rhodium, or a combination thereof, also applied to a monolithic carrier by means of a washcoat.
Weitere einfache Verfahren, wie das Eintauchen des Katalysatorträgers in einen Washcoat und das Entfernen von überschüssigem Washcoat durch Ausblasen mit Luft, sind ebenfalls aus dem Stand der Technik bekannt, wie auch Beschichtungsverfahren unter Einsatz von Zentrifugen. Ebenso ist auch die Möglichkeit des Besprühens poröser Formkörper mit einem Washcoat vorgeschlagen worden. Als Beschichtung werden zumeist in der Regel auf Aluminiumoxid basierende Washcoats eingesetzt, die durch ihre große Oberfläche charakterisiert sind.Other simple methods, such as immersing the catalyst support in a washcoat and removing excess washcoat by air blowing, are also known in the art, as are coating techniques using centrifuges. Likewise, the possibility of spraying porous moldings with a washcoat has also been proposed. The coating used is generally generally aluminum oxide-based washcoats, which are characterized by their large surface area.
Dabei werden in dem auf beispielsweise Aluminiumoxid basierenden Washcoat Metalle wie die Metalle der Platingruppe, z. B. durch Lösung, Totalabsorption oder durch Tränken mit Edelmetall-haltigen Lösungen oder durch Einarbeiten in den Washcoat vor der Beschichtung, integriert.Here are in the example based on alumina washcoat metals such as the metals of the platinum group, z. B. by solution, total absorption or by impregnation with precious metal-containing solutions or by incorporation into the washcoat prior to coating integrated.
Die für die Partikeloxidation zur Verfügung stehende Oberfläche hat einen erheblichen Einfluss auf den katalytischen Umsatz und insbesondere auf die Langzeitstabilität des Katalysators. Es ist bekannt, dass zur Erhöhung der Stabilität der Aluminiumoxidoberfläche den Washcoats oft stabilisierende Elemente, wie z. B. Cer oder Lanthan, beigemischt werden können.The surface available for the particle oxidation has a considerable influence on the catalytic conversion and in particular on the long-term stability of the catalyst. It is known that to increase the stability of the alumina surface washcoats often stabilizing elements such. As cerium or lanthanum, can be added.
Durch die erfindungsgemäße Katalysatoranordnung, wobei verschiedene katalytische Funktionen in einzelnen Bauteilen kombiniert wurden, konnte ersichtlich eine Verringerung des Raumbedarfs für ein Abgassystem erreicht werden.Due to the catalyst arrangement according to the invention, wherein different catalytic functions were combined in individual components, a reduction in the space requirement for an exhaust gas system could obviously be achieved.
Zusammengefasst werden konnte eine SCR-aktive Komponente, die einen Katalysator auf Basis von Vanadium, Wolfram und Titan umfasst, eine Kohlenwasserstoffspeicherkomponente, die ein Zeolith vom Typ MFI ist, und ein Oxidationskatalysator, der als katalytisch aktive Komponente Rhodium enthält, in einem Bauteil (SCR-Katalysator).In summary, an SCR-active component comprising a catalyst based on vanadium, tungsten and titanium, a hydrocarbon storage component which is an MFI-type zeolite, and an oxidation catalyst containing rhodium as a catalytically active component in one component (SCR -Catalyst).
Zusammengefasst werden konnten ferner der Oxidationskatalysator und der Ammoniak-Sperrkatalysator in einem Bauteil (Oxidationskatalysator).In addition, the oxidation catalyst and the ammonia barrier catalyst could be combined in one component (oxidation catalyst).
Der erfindungsgemäße SCR-Katalysator und das Abgasreinigungssystem können zur Abgasbehandlung von Abgasen von Verbrennungsmotoren verwendet werden. Verbrennungsmotoren im Sinne dieser Erfindung sind beispielsweise Dieselmotoren oder Stationärmotoren.The inventive SCR catalyst and the exhaust gas purification system can be used for exhaust gas treatment of exhaust gases of internal combustion engines. Internal combustion engines in the context of this invention are, for example, diesel engines or stationary engines.
Die Erfindung soll nun anhand einiger Beispiele, welche nicht als einschränkend auf den Umfang der Erfindung zu verstehen sind, unter Bezugnahme auf die Figuren näher erläutert werden.The invention will now be described with reference to some examples, which are not to be understood as limiting the scope of the invention, with reference to the figures.
Ausführungsbeispiel (nicht erfindungsgemäß)Embodiment (not according to the invention)
Anordnung 1 (siehe Fig. 1):Arrangement 1 (see Fig. 1):
In diesem Fall trägt der SCR-Katalysator (
DPF (
Als DPF (
SCR-Katalysator (
Für den SCR-Katalysator (
Harnstoffdosierung (
Die Einrichtung zur Harnstoffdosierung (
Claims (12)
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DE102008009672.5A DE102008009672B4 (en) | 2008-02-18 | 2008-02-18 | Hydrocarbon storage function SCR catalyst, its use and emission control system and its use |
PCT/EP2009/000623 WO2009103406A1 (en) | 2008-02-18 | 2009-01-30 | Scr catalyst comprising a hydrocarbon accumulator function and catalyst assembly |
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DE102008009672.5A DE102008009672B4 (en) | 2008-02-18 | 2008-02-18 | Hydrocarbon storage function SCR catalyst, its use and emission control system and its use |
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US10252252B2 (en) | 2012-08-17 | 2019-04-09 | Johnson Matthey Public Limited Company | Zeolite promoted V/TiW catalysts |
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CN102665910B (en) * | 2009-11-19 | 2014-07-02 | 揖斐电株式会社 | Honeycomb structure and exhaust gas purification apparatus |
DE102010047415A1 (en) * | 2010-10-02 | 2012-04-05 | Volkswagen Ag | Method for operating an internal combustion engine and for the execution of the method set up control device |
DE102010050312A1 (en) * | 2010-11-03 | 2012-05-03 | Süd-Chemie AG | Ammonia oxidation catalyst with low N2O by-product formation |
DE102012209852A1 (en) | 2012-06-12 | 2013-12-12 | Robert Bosch Gmbh | Exhaust gas purification system for arrangement in exhaust section of exhaust gas system of diesel internal combustion engine in motor vehicle, has input-oxidation catalyzer for oxidation of hydrocarbons and carbon monoxide |
EP3024574B1 (en) * | 2013-07-26 | 2021-11-24 | Johnson Matthey Public Limited Company | Tungsten/titania oxidation catalyst |
DE102015205843A1 (en) * | 2015-03-31 | 2016-10-06 | Johnson Matthey Catalysts (Germany) Gmbh | Catalyst, in particular for exhaust gas purification |
KR101703624B1 (en) | 2015-09-30 | 2017-02-07 | 현대자동차 주식회사 | Exhaust gas processing system |
KR101896334B1 (en) * | 2016-11-28 | 2018-09-07 | 현대자동차 주식회사 | Device for purifying exhaust gas |
CN108786783A (en) * | 2018-06-11 | 2018-11-13 | 上海电力学院 | The SCR catalyst and preparation method thereof that a kind of resistant to potassium for denitrating flue gas poisons |
CN116440945B (en) * | 2023-03-02 | 2024-04-30 | 昆明贵研催化剂有限责任公司 | Multi-effect catalyst for hydrogen internal combustion engine and preparation method thereof |
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