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WO2009118188A1 - Solutions solides et procédés de fabrication correspondant - Google Patents

Solutions solides et procédés de fabrication correspondant Download PDF

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Publication number
WO2009118188A1
WO2009118188A1 PCT/EP2009/002261 EP2009002261W WO2009118188A1 WO 2009118188 A1 WO2009118188 A1 WO 2009118188A1 EP 2009002261 W EP2009002261 W EP 2009002261W WO 2009118188 A1 WO2009118188 A1 WO 2009118188A1
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WO
WIPO (PCT)
Prior art keywords
nox
composite
oxide
nox scavenger
scavenger
Prior art date
Application number
PCT/EP2009/002261
Other languages
English (en)
Inventor
Barry W. L. Southward
Original Assignee
Umicore Ag & 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
Priority claimed from US12/240,170 external-priority patent/US20090246109A1/en
Priority claimed from US12/363,310 external-priority patent/US9403151B2/en
Priority claimed from US12/363,329 external-priority patent/US20100196217A1/en
Application filed by Umicore Ag & Co. Kg filed Critical Umicore Ag & Co. Kg
Publication of WO2009118188A1 publication Critical patent/WO2009118188A1/fr

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    • 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
    • B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
    • B01D53/945—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC] characterised by a specific catalyst
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    • 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
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Definitions

  • All of these technologies typically comprise PGM-contaming heterogeneous-phase catalysts containing particles of highly active precious metal (PGM) which are stabilised and dispersed on a refractory oxide support; e.g. alumina, of comparably low intrinsic activity.
  • PGM highly active precious metal
  • the DNT and DNPT may additionally contain alkali metal or alkaline earth metal oxides to facilitate regenerative adsorption of Nitrogen Oxides (NOx).
  • the CDPF, DNT and DNPT may also contain one or more Oxygen Storage (OS) materials.
  • the OS materials are based on CeO 2 or other redox active oxide and are employed to buffer the catalyst from local variations in the air/fuel ratio during catalyst regeneration or other transient e.g.
  • the trapped soot and also NO x are again converted into environmentally benign products (N 2 , CO 2 and H 2 O) by the introduction of 'sacrificial' fuel species into the exhaust to initiate the conversion of soot and simultaneously the reduction of the trapped NOx to N 2 during transient 'rich' condition present at this time.
  • oxygen ionic conductivity OIC
  • SOFC solid oxide fuel cells
  • OS oxygen storage
  • TWC three-way-conversion
  • electrochemical oxygen sensors oxygen ion pumps
  • structural ceramics of high toughness heating elements
  • electrochemical reactors steam electrolysis cells
  • electrochromic materials magnetohydrodynamic (MHD) generators
  • hydrogen sensors catalysts for methanol decomposition and potential hosts for immobilizing nuclear waste.
  • MHD magnetohydrodynamic
  • the term 'rare earth' means the 30 rare earth elements composed of the lanthanide and actinide series of the Periodic Table of Elements.
  • doped ZrO 2 partially stabilized ZrO 2 consists of tetragonal and cubic phases while the fully stabilized form exists in the cubic fluorite structure.
  • the amount of dopant required to fully stabilize the cubic structure for ZrO 2 varies with dopant type.
  • For Ca it is in the range of about 12-13 mole%, for Y 2 O 3 and Sc 2 O 3 it is greater than about 18 mole% of the Y or scandium (Sc), and for other rare earths (e.g., Yb 2 O 3 , Dy 2 O 3 , Gd 2 O 3 , Nd 2 O 3 , and Sm 2 O 3 ) it is in the range of about 16 - 24 mole% of ytterbium (Yb), Dy, gadolinium (Gd), Nd, and samarium (Sm).
  • Yb ytterbium
  • Dy gadolinium
  • Sm samarium
  • Solid solutions consisting of ZrO 2 , CeO 2 and trivalent dopants are used in three-way-conversion (TWC) catalysts as oxygen storage (OS) materials and are found to be more effective than pure CeO 2 both for higher oxygen storage capacity and in having faster response characteristics to air-to-fuel (A/F) transients.
  • TWC three-way-conversion
  • OS oxygen storage
  • A/F air-to-fuel
  • reports concerning the use of ceria-based catalysts for soot oxidation reveal new uses for solid solutions of CeO 2 with other elements where low temperature Ce 4+ ⁇ Ce 3+ redox activity may have significant importance.
  • Oxygen storage (OS) in exhaust catalyst applications arises due to the nature of the Ce 4+ ⁇ Ce 3+ redox cycle in typical exhaust gas mixtures.
  • Benefits of yttrium and other rare earth doped CeO 2 -ZrO 2 solid solutions compared to undoped CeO 2 and CeO 2 -ZrO 2 for TWC catalyst applications is due to improved Ce 4+ reducibility at relatively low temperatures and enhanced oxygen ion conductivity (OIC), i.e., mobility of oxygen in the oxygen sublattice.
  • OIC oxygen ion conductivity
  • Solid solutions with substantially cubic structures were found to have advantages over other crystal structures, and are used herein as host matrices as shown in US 6,585,944 and US 6,387,338, the entire disclosures of which are relied on and incorporated herein by reference.
  • CeO 2 and to a lesser extent ThO 2 , based systems are preferentially acknowledged as active redox couple systems.
  • the term 'redox active' could equally apply to any metal oxide or mixed metal oxide system that undergoes oxidation-reduction during normal vehicular operation conditions.
  • the metal oxide/mixed metal oxide can provide or accept electrons under the exhaust temperature/composition regimes that are generated during catalyst operation.
  • the OS/OIC function is significantly enhanced by platinum group metals (PGM) such as palladium (Pd), platinum (Pt), and rhodium (Rh).
  • PGM platinum group metals
  • Rh platinum group metals
  • the reduction of the Ce 4+ to Ce 3+ in doped CeO 2 -ZrO 2 solid solutions occurs at lower temperatures and improves TWC catalyst efficiency in reducing HC, CO, and nitrogen oxides (NOx) pollutants.
  • Oxygen storage (OS) materials are also employed in diesel-based exhaust treatment applications such as Catalysed Diesel Particulate Filters (CDPFs), Diesel NOx Traps (DNTs), and Diesel NOx Particulate Traps (DNPTs) to convert undesirable constituents of the exhaust stream into less undesirable molecules.
  • CDPFs Catalysed Diesel Particulate Filters
  • DNTs Diesel NOx Traps
  • DNPTs Diesel NOx Particulate Traps
  • the exhaust stream is changed to a fuel rich environment via active regeneration systems.
  • Active regeneration systems employ an exhaust stream monitoring component and a fuel injection component that are jointly employed to produce the fuel -rich transient environment by injecting diesel fuel into the exhaust stream when directed by exhaust conditions.
  • the fuel rich environment produced promotes the release of trapped nitrates as NO x and also promotes the release of oxygen from the OS, which then catalytically react, in the presence of an appropriate catalytic metal e.g. Rh or Pd, with CO and H 2 present in the exhaust stream to form CO 2 , H 2 O, and N 2 .
  • the thermal transient produced initiates the combustion in the case of the CDPF or DNPT.
  • active regeneration systems are generally effective at reducing the amount of NOx emissions, these systems are expensive, increase fuel consumption, are susceptible to sulfur poisoning, and generally inefficient at scavenging NOx with respect to NOx adsorber loading.
  • active regeneration systems also exhibit several manufacturing related shortcomings, such as, poor dispersion of NOx adsorber materials and high catalyst loadings.
  • the NOx adsorbers employed can be toxic or strong oxidizers (e.g., barium nitrates and potassium nitrates, respectively).
  • active regeneration systems are incapable of reducing NOx emissions and soot at low operating temperatures, such as, during start-up conditions where a bulk of emissions are released into the environment.
  • cerium-oxide exhaust treatment materials articles employing said materials, as well as methods for making and using the same. More particularly, the present invention relates to a NOx adsorber comprising a solid solution, wherein the solid solution comprises a cubic fluorite structure as determined by conventional x-ray diffraction method; and, a NOx scavenger disposed within the cubic fluorite structure, wherein the NOx scavenger is formed from oxides, and the oxides thereof are formed from an element, or an oxide of an element, selected from the group consisting of alkali metals, alkaline earth metals, transition metals and mixtures thereof.
  • the cubic fluorite structure comprises a material selected form the group consisting of ceria, zirconia, thorium and mixtures thereof.
  • a stabiliser can also be included, preferably a metal or metal oxide.
  • the metal of stabilisers is, one or more elements selected from the group of rare earths consisting of scandium (Sc), yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu) and mixtures thereof.
  • the metal oxide is a rare earth metal oxide.
  • the composite OS-NOx adsorber further comprises a catalytic metal selected from the group comprising platinum, palladium, iridium, silver, rhodium, ruthenium and mixtures thereof.
  • a catalytic metal selected from the group comprising platinum, palladium, iridium, silver, rhodium, ruthenium and mixtures thereof.
  • the solid solution of a substantially cubic fluorite structure of the NOx absorber is preferably cerium oxide or zirconium oxide or mixtures thereof.
  • the solid solution of a substantially cubic fluorite structure contains a highly dispersed NOx scavenger.
  • the NOx scavenger is incorporated within the structure of the oxygen storage material, without forming any discrete phases detectable by conventional X-Ray Diffraction method, is a metal or metal oxide capable of forming nitrates at temperatures that are less than or equal to about 200°C, preferably less than or equal to about 300°C and more preferably greater than about 400°C, and capable of reducing the nitrates at temperatures that are greater than about 200 0 C, preferably greater than about 300 0 C, and more preferably greater than about 400 0 C.
  • a composite catalyst comprising a NOx adsorber including a solid solution, wherein the solid solution comprises a cubic fluorite structure; and, a NOx scavenger disposed within the cubic fluorite structure, wherein the NOx scavenger is formed from oxides, wherein the oxides comprise an element selected from the group consisting of alkali metals, alkaline earth metals, transition metals and mixtures thereof; and a platinum group metal deposited on said NOx adsorber.
  • the cubic fluorite structure comprises a material selected from the group consisting of ceria, zirconia, thorium and mixtures thereof.
  • a stabiliser such as a metal or metal oxide, can also be added to the composite catalyst.
  • the platinum/precious group metal is a catalytic metal selected from the group comprising platinum, palladium, iridium, silver, rhodium, ruthenium and mixtures thereof.
  • the composite catalyst can also include an oxygen storage material such as cerium oxide or zirconium oxide and mixtures thereof.
  • the composite catalyst of this invention can be deposited by conventional means and methods on any suitable inert carrier which are well known in the art. Preferably, an inert ceramic or metal honeycomb carrier can be used. Pellets of an inert material can also be used as the carrier. Any suitable conventional housing or canister can be used to retain the composite catalyst of the present invention.
  • Figure 1 is a graph illustrating the impact of 'Contact Efficiency' on the 'direct' catalytic oxidation of artificial soot analogue (Printex U) by conventional Cubic Fluorite - based CeZr solid solution/mixed oxide.
  • Figure 2 is a graph illustrating the impact of engine soot loading conditions on the catalytic performance of a conventional Pt-OSl-Al 2 O 3 washcoat for the direct catalytic soot oxidation as examined in a synthetic gas bench (SGB) 'burn-out' experiment;
  • Figure 3 is a graph referring to the SGB temperature programmed reaction profile of the reaction of an intimate mixture of 0.75% Pt-Al 2 O 3 -OSl: Printex U (4:1) in the presence of 100 ppm NO;
  • Figure 4 is a graph of the SGB temperature programmed reaction profile of the reaction of an intimate mixture of 0.75% Pt-Al 2 O 3 -OSl: Printex U (4:1) in the absence of NO;
  • Figure 5 is the X-Ray Diffraction patterns for OS2 ( ⁇ ) and OS3 (O),
  • Figure 6 is a graph of the SGB temperature programmed reaction profile of the reaction of an intimate mixture of 0.75% Pt-Al 2 O 3 -OS 2 : Printex U (9:1); Key: X -CO conversion, + - HC conversion, * - NO 2 make, T - bed temperature.
  • Figure 7 is a graph of the SGB temperature programmed reaction profile of the reaction of an intimate mixture of 0.75% Pt-Al 2 O 3 -OS3: Printex U (9:1); Key: X - CO conversion, + - HC conversion, * - NO 2 make, T - bed temperature
  • Figure 8 illustrates the XRD patterns for OS4 ( ⁇ ) and OS5 (O);
  • Figure 9 is a graph referring to the 'fresh' NO 2 storage and release for OS4 and OS5 materials using 2% Pt and 2% Pd promoted materials;
  • Figure 10 is a graph referring to the 'aged' NO 2 storage and release for OS4 and OS5 materials using 2% Pt and 2% Pd promoted materials;
  • Figure 11 shows the SGB performance of an intimate mixture of 2% Pt- A1 2 O 3 -OS4: Printex U (9:1);
  • Figure 12 depicts the SGB temperature programmed reaction profile of the reaction of an intimate mixture of 2% Pt-Al 2 O 3 -OS5: Printex U (9:1);
  • Figure 13 records the XRD patterns for OS6 (D) and OS7 (O),
  • Figure 14 illustrates the SGB temperature programmed reaction profile of the reaction of an intimate mixture of 0.75% Pt-Al 2 O 3 -OSo: Printex U (9:1);
  • Figure 15 is a graph of the SGB temperature programmed reaction profile of the reaction of an intimate mixture of 0.75% Pt- A1 2 O 3 -OS7: Printex U (9:1);
  • Figure 16 shows the SGB temperature programmed reaction profiles of the reaction of a) an intimate mixture of 0.75% Pt- A1 2 O 3 -OS7: Printex U (9:1) versus b) an intimate mix of 0.75% Pt- Al 2 O 3 -OSl impregnated with 10% SrO: Printex U (9:1);
  • Figure 17 is a table of the CO light-off, Temperature of peak rate of soot combustion and CO slip during soot combustion for 0.75% Pt- Al 2 O 3 -OS systems for OS7, OSl +10% SrO, OSl+10% K 2 O or OSl+10Ag 2 O; and
  • Figure 18 shows the Temperature of peak soot combustion and XRD characteristics for composite OS-NOx scavengers containing a CaO NOx scavenger.
  • composite 0S/N0x adsorber solid solutions and exhaust gas treatment devices comprising the same.
  • the composite OS-NOx storage materials are disclosed that comprise a substantially cubic structure; e.g., Fluorite structure as determined by conventional x-ray diffraction method, having a NOx scavenger incorporated therein.
  • the resulting composite cubic NOx adsorber is capable of adsorbing NOx and forming a nitrate that can decompose under normal operating temperatures of the exhaust stream to release NOx.
  • the OS/redox active system are previously defined (e.g.
  • the OS materials described herein are conventional binary, tertiary, quaternary, etc. compositions based on CeZr solid solutions containing a substantially phase pure Cubic Fluorite lattice (as determined by conventional X-Ray Diffraction (XRD) method).
  • the NOx scavenger is preferentially added during the conventional co-precipitation synthesis process and may include any metal (or metal oxide) capable of introducing NOx scavenging function; e.g. Group I the alkali metals, Group II the alkaline earth metals or transition metals. That is, appropriate elements for this application include, but are not limited to, alkali metals, e.g. Na, K, alkaline Earth Metals, e.g.
  • transition metals we mean the 38 elements in Groups 3 through 12 of the Periodic Table of Elements.
  • the composite OS cubic NOx scavengers described herein differ significantly from conventional NOx adsorbers employed to date in that they do not employ a conventional bulk oxide e.g. alkali metal, alkaline earth metal etc. but rather provide NOx functionality by the use of specifically engineered composite crystal structures.
  • the mechanism by which the composite cubic OS NOx scavenger functions is generally comparable i.e. the trapping NOx on surface atoms of the oxide as a nitrate salt during fuel-lean conditions, followed by decomposition and reduction to N 2 in fuel-rich transients.
  • the composite cubic OS-NOx scavenger can be employed in catalysts for exhaust gas treatment applications.
  • a catalyst system can employ a precious metal catalyst (e.g., Pt, Rh, and other platinum group metals) to react the released NO and NO 2 to form less undesirable emissions, such as CO 2 , O 2 and N 2 .
  • a precious metal catalyst e.g., Pt, Rh, and other platinum group metals
  • the NOx scavenger can be defined as any bulk metal oxide or metal salt capable of forming a stable nitrate under the conditions existing in a Diesel I.C.E. exhaust.
  • the composite cubic NOx scavenger is capable of forming nitrates at temperatures that are less than or equal to about 200 0 C and reducing the nitrates at temperatures that are greater than about 200°C, or more specifically, less than or equal to about 300°C and greater than about 30O 0 C, and even more specifically, less than or equal to about 400 0 C and greater than about 400 0 C.
  • the NOx scavenger can be defined as any bulk/surface nitrate which may be regenerably decomposed to its prior oxide or salt under the conditions existing during the active regeneration cycle of the catalysed Diesel particulate filter.
  • Other preferred elements include those of the Group IB (Copper family), e.g. Cu, Ag, Au, with Ag being demonstrated as having a particular efficacy for this NOx scavenging function (e.g. see SAE paper 2008-01-0481).
  • composite cubic NOx scavengers provide an intrinsically far higher dispersion of trapping component than non-cubic, i.e. conventional, impregnation-type NOx adsorbers.
  • the efficiency of NOx storage per mol.% of the NOx adsorbing material is greater for the composite cubic NOx material than non-cubic NOx adsorbers. Therefore, less material is employed during manufacture, which decreases production costs and provides for reduced backpressure during operation, thereby improving engine performance and efficiency.
  • This higher capacity provides further benefit since it will allow the vehicle to run longer under 'lean' conditions without the tailpipe NOx (NOx slip) exceeding permitted values before requiring the rich regeneration cycle. This means fewer regeneration cycles per 1000 km; i.e. lower fuel penalty/decreased operational cost.
  • Another particular benefit of the cubic NOx adsorbers compared to the non- cubic NOx adsorbers is that when sulfur is trapped within the NOx adsorber lattice, unstable sulfides are formed, due to their high atomic dispersion and thus, higher surface energy, which enable for the lower temperature desulfation of the cubic NOx adsorber.
  • a further especial benefit of the composite cubic OS-NOx adsorber is its ability to facilitate lower temperature particulate combustion. This is achieved for the CDPF/DNPT, since the composite materials disable the de-coupling mechanism of NO 2 , thereby retaining higher contact efficiency between the catalyst and soot (as described in SAE paper 2008-01-0481) and this, in turn, enables the catalyst to provide an active and direct mechanism for soot oxidation, thereby decreasing the temperature required during the regeneration cycle to achieve complete soot burn - again, an operating cost saving due to decreased fuel penalty (and decreased ash deposition, oil dilution, etc.)
  • the solid solution can comprise the cubic NOx adsorber and additional components, such as stabilisers, catalysts, oxygen storage components and other additives contributing their expected function.
  • the NOx adsorber can be present in an amount of about 0.01 mol% to about 25 mol%, or more specifically, about 0.1 mol% to about 15 mol%, or, even more specifically about 0.5 mol% to about 10 mol%, and yet more specifically, about 1 mol% to about 5 mol%.
  • Stabilisers can be employed within the solid solution to alter the properties and/or function of the NOx adsorber.
  • the stabilizer can be metals and/or metal oxides. Exemplary metals are the rare earths and comprise scandium (Sc), yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu) and mixtures thereof.
  • La and Y can be present in the solid solution; in another example, the stabilizer can comprise yttrium and a rare earth metal.
  • exemplary oxides are rare earth oxides, such as La 2 O 3 , Y 2 O 3 , Pr 6 O 11 , Nd 2 O 3 , and the like.
  • rare earth oxide stabilisers can enhance the reduction of the NOx from a cerium oxide lattice.
  • stabilisers can be present in the solid solution in amounts that are less than or equal to about 20 mol%, or more specifically, about 0.5 mol% to about 15 mol%, or, even more specifically about 5 mol% to about 15 mol%.
  • Catalytic metals can be employed within the solid solution to reduce the NOx released by the cubic NOx adsorber to NO.
  • exemplary catalytic metals comprise transition metals (e.g., Pt, Rh, Ru, Pd, Ag, and the like).
  • the concentration of the components employed to form the cubic NOx adsorber or solid solution can be tailored to modify the properties thereof. For example, a sufficient amount of zirconium can be employed in a solid solution to minimize the reduction energies of Ce 4+ and minimize activation energy so as to provide enhanced mobility of oxygen within the lattice.
  • Additional oxygen storage materials can be added to the solid solution to provide an oxygen storage function.
  • Exemplary oxygen storage materials are CeO 2 and ZrO 2 .
  • a solid solution can comprise less than or equal to about 95 mole percent (mol%), or more specifically about 30 mol% to about 90 mol%, or even more specifically about 50 mol% to about 85 mol% zirconium, less than or equal to about 50 mol%, or more specifically about 0.5 mol% to about 45 mol%, or even more specifically about 5 mol% to about 40 mol% cerium.
  • a catalyst system can be formed wherein a solid solution comprises a cubic NOx adsorber, an oxygen storage material, and catalytic metals.
  • the solid solution has a substantially cubic crystal structure, particularly a cubic fluorite crystal structure as characterized by powder X-ray diffraction (XRD) analysis of the cation sublattice, even for compositions that have in excess of 50 mole percent (mol%) zirconium.
  • XRD powder X-ray diffraction
  • a composite cubic OS-NOx scavenger or a solid solution comprising a cubic NOx adsorber can be employed in an exhaust gas treatment device, e.g., disposed on/in an inert substrate or carrier.
  • Exhaust gas treatment devices can generally comprise housing or canister components that can be easily attached to an exhaust gas conduit and comprise a substrate for treating exhaust gases.
  • the housing components can comprise an outer 'shell', which can be capped on either end with funnel-shaped 'end-cones' or flat 'end-plates', which can comprise 'snorkels' that allow for easy assembly to an exhaust conduit.
  • Housing components can be fabricated of any materials capable of withstanding the temperatures, corrosion, and wear encountered during the operation of the exhaust gas treatment device, such as, but not limited to, ferrous metals or ferritic stainless steels (e.g., martensitic, ferritic, and austenitic stainless materials, and the like).
  • ferrous metals or ferritic stainless steels e.g., martensitic, ferritic, and austenitic stainless materials, and the like.
  • a retention material Disposed within the shell can be a retention material ('mat' or 'matting'), which is capable of supporting a substrate, insulating the shell from the high operating temperatures of the substrate, providing substrate retention by applying compressive radial forces about it, and providing the substrate with impact protection.
  • the matting is typically concentrically disposed around the substrate forming a substrate/mat sub-assembly.
  • Various materials can be employed for the matting and the insulation. These materials can exist in the form of a mat, fibres, preforms, or the like, and comprise materials such as, but not limited to, intumescent materials (e.g., a material that comprises vermiculite component, i.e., a component that expands upon the application of heat), non-intumescent materials, ceramic materials (e.g., ceramic fibers), organic binders, inorganic binders, and the like, as well as combinations comprising at least one of the foregoing materials.
  • intumescent materials e.g., a material that comprises vermiculite component, i.e., a component that expands upon the application of heat
  • non-intumescent materials e.g., ceramic materials that comprises vermiculite component, i.e., a component that expands upon the application of heat
  • ceramic materials e.g., ceramic fibers
  • Non- intumescent materials include materials such as those sold under the trademarks 'NEXTEL' and 'INTERAM 1101HT' by the '3M' Company, Minneapolis, Minnesota, or those sold under the trademark, 'FIBERFRAX' and 'CC-MAX' by the Unifrax Co., Niagara Falls, New York, and the like.
  • Intumescent materials include materials sold under the trademark 'INTERAM' by the '3M' Company, Minneapolis, Minnesota, as well as those intumescent materials which are also sold under the aforementioned 'HBERFRAX' trademark.
  • Substrates or carriers can comprise any material designed for use in a spark ignition or diesel engine environment having the following characteristics: (1) capability of operating at temperatures up to about 600 0 C and up to about l,000°C for some applications, depending upon the device's location within the exhaust system (e.g., manifold mounted, close coupled, or underfloor) and the type of system (e.g., gasoline or diesel); (2) capability of withstanding exposure to hydrocarbons, nitrogen oxides, carbon monoxide, particulate matter
  • Some suitable inert ceramic materials include cordierite, silicon carbide, metal, metal oxides (e.g., alumina, and the like), glasses, and the like and mixtures comprising at least one of the foregoing materials.
  • Some suitable inert ceramic materials include cordierite, silicon carbide, metal, metal oxides (e.g., alumina, and the like), glasses, and the like and mixtures comprising at least one of the foregoing materials.
  • Some suitable inert ceramic materials include
  • 'Celcor' commercially available from Corning, Inc., Corning, New York.
  • These materials can be in the form of foils, perform, mat, fibrous material, monoliths (e.g., a honeycomb structure, and the like), other porous structures (e.g., porous glasses, sponges), foams, pellets, particles, molecular sieves, and the like (depending upon the particular device), and combinations comprising at least one of the foregoing materials and forms, e.g., metallic foils, open pore alumina sponges, and porous ultra-low expansion glasses.
  • these substrates can be coated with oxides and/or hexaaluminates, such as stainless steel foil coated with a hexaaluminate scale.
  • the substrate can have any size or geometry, the size and geometry are preferably chosen to optimise surface area in the given exhaust gas emission control device design parameters.
  • the substrate has a honeycomb geometry, with the combs through- channel having any multi-sided or rounded shape, with substantially square, triangular, pentagonal, hexagonal, heptagonal, or octagonal or similar geometries preferred due to ease of manufacturing and increased surface area.
  • the exhaust gas treatment devices can be assembled utilizing various methods. Three such methods are the stuffing, clamshell, and tourniquet assembly methods.
  • the stuffing method generally comprises pre-assembling the matting around the substrate and pushing, or stuffing, the assembly into the shell through a stuffing cone.
  • the stuffing cone serves as an assembly tool that is capable of attaching to one end of the shell. Where attached, the shell and stuffing cone have the same cross-sectional geometry, and along the stuffing cone's length, the cross-sectional geometry gradually tapers to a larger cross-sectional geometry. Through this larger end, the substrate/mat sub-assembly can be advanced which compresses the matting around the substrate as the assembly advances through the stuffing cone's taper and is eventually pushed into the shell.
  • Exhaust gas treatment devices comprising the cubic NOx adsorber or solid solutions comprising cubic NOx adsorbers can be employed in exhaust gas treatment systems to provide a NOx adsorption function, or more specifically to reduce a concentration of undesirable constituents in the exhaust gas stream.
  • an exemplary catalyst system can be formed utilizing a cubic NOx adsorber, a catalyst(s), and an oxygen storage material, wherein the catalyst system is disposed on a substrate, which is then disposed within a housing. Disposing the substrate to an exhaust gas stream can then provide at least a NOx storage function, and desirably even reduce the concentration of at least one undesirable constituent contained therein.
  • a CDPF or DNPT can comprise a porous substrate having alternating channels.
  • the alternating channels comprise upstream channels and downstream channels, which both have an upstream end and a downstream end.
  • the upstream channels are configured such that its upstream end is open and allows exhaust gas to flow therethrough.
  • the downstream end of the upstream channels is blocked, which does not allow exhaust gas to flow therethrough.
  • the downstream channels are configured such that its upstream end is blocked, which does not allow exhaust gas to flow therethrough.
  • the downstream end of the downstream channels is open, which allows exhaust gas to flow therethrough.
  • the exhaust gas flowing from the upstream channels passes through the walls of the substrate to the downstream channels.
  • a solid solution can be dispersed within the upstream channels and downstream channels, and possibly within the substrate (e.g., depending upon the application method, porosity of the substrate, the size of the solid solution granules, and other variables).
  • cubic NOx adsorbers provide an intrinsically far higher dispersion of trapping component than non-cubic NOx adsorbers.
  • the efficiency of NOx storage per mol% of the NOx adsorbing material is greater for the cubic NOx adsorber than non-cubic NOx adsorbers. Therefore, less material is employed during manufacture, which decreases production costs and provides for reduced backpressure during operation, thereby improving engine performance and efficiency.
  • Another particular benefit of the composite cubic OS-NOx scavenger compared to the non-cubic NOx adsorbers is that when sulfur is trapped within the NOx adsorber lattice, unstable sulfides are formed, due to their high atomic dispersion and thus, higher surface energy, which enable for the lower temperature desulfation of the cubic NOx adsorber.
  • Coated parts and a blank reference were wrapped in mat and loaded in metal retaining sleeves, weighed after mat burn-out (2h 550 0 C in static oven) and loaded into a converter can specially designed to accommodate three mini-filters: 2 coated parts plus 1 blank cordierite as internal reference.
  • the parts were soot loaded on the engine dyno using a Chevrolet 6.5L diesel engine. Soot loading was performed using either a low load (Mass Air Row of 21 g/sec) or high load (MAF 63 g/s) and a target filter inlet temperature of 200 0 C. These two cases represent soot with either a significant SOF loaded under low engine out NOx or low SOF/' dry' soot loaded with high engine out NOx. During loading backpressure was constantly monitored using a ⁇ P sensor and flow was controlled using a butterfly valve. In all cases, soot-loading rate was ca. 4g/hour with total loading times of 3-4 hours.
  • the first solid solution comprised the composition: (OS2) 34 mol% CeO 2 , 9.5 mol% Nd 2 O 3 , 4.5 mol% Pr 6 O 11 , 10 mol% SrO, and 42 mol% ZrO 2
  • the second solid solution comprised the composition: (0S3) 44 mol% CeO 2 , 9.5 mol% Nd 2 O 3 , 4.5 mol% Pr 6 O 11 , 10 mol% SrO, and 32 mol% ZrO 2 .
  • compositions were first dissolved in 500 millilitres (ml) of deionised water.
  • the resulting homogeneous solution was precipitated slowly under vigorous stirring by addition of 1.35 litters (L) of 4 molar (M) ammonium hydroxide (NH4OH) to form a precipitate of mixed metal hydrous oxides.
  • the reaction mixture was additionally stirred for 3 hours.
  • the precipitate in the form of powder
  • the dried powder was then ground, and calcined at about 700 0 C for 6 hours.
  • Figure 5 is a graph of the X-Ray Diffraction patterns of the resulting powders OS2 (D) and OS3 (O). This data confirmed the original syntheses were not successful in incorporating SrO into the Cubic Fluorite lattice due to the formation of a stable and separate SrCO 3 phase.
  • Figure 8 illustrates the XRD patterns for OS4 ( ⁇ ) and OS5 (O) confirming that Sr was incorporated into the Cubic Fluorite lattice.
  • the first NOx trap comprised a substrate with 1:1 OS4: Al 2 O 3 and 2 wt.% Pt disposed thereon.
  • the second NOx trap comprised a substrate having 1:1 0S4: Al 2 O 3 and 2 wt.% Pd disposed thereon.
  • the third NOx trap comprised a substrate having 1:1 0S5: Al 2 O 3 and 2 wt.% Pt disposed thereon.
  • the fourth NOx trap comprised a substrate having 1:1 OS5:A1 2 O 3 and 2 wt.% Pd disposed thereon.
  • the NOx traps were formed by first preparing a washcoat of the respective solid solution and the respective catalyst (e.g., the 0S4 mixed with Al 2 O 3 to which 2 wt.% Pt from Platinum nitrate precursor was added). The washcoat was then disposed on cordierite substrates, which were then calcined at about 540°C.
  • the respective catalyst e.g., the 0S4 mixed with Al 2 O 3 to which 2 wt.% Pt from Platinum nitrate precursor was added.
  • the washcoat was then disposed on cordierite substrates, which were then calcined at about 540°C.
  • the NOx traps were then individually tested on a diesel testing apparatus wherein an exhaust gas of known composition was passed through the substrate and the NO 2 produced from each substrate was measured with respect to temperature, as illustrated in Figures 9 and 10 attached hereto.
  • the exhaust gas passed through the substrates comprised 100 ppm (parts per million) NO, 10 vol.% (volumetric %) O 2 , 3.5 vol.% CO 2 , 3.5 vol.% H 2 O, and the balance being N 2 .
  • platinum is capable of converting a greater amount of NO to NO 2 than palladium during operation as the NO released by the NOx adsorber at temperatures below about 400 0 C are not converted by palladium, although not bound by theoretical hypotheses.
  • OS7 is superior wrt CO light-off (50% CO conversion @ 192 for OS7 vs 232°C for OS 1+SrO, note a comparable benefit was seen for HC but the data is omitted to assist with clarity of the figure).
  • OS7 material also exhibited a decrease in the soot combustion temperature (360 vs 375 0 C) and a significant benefit with CO slip during soot burn (1000 ppm vs ca. 4000 ppm CO for OS 1+SrO).
  • the data confirm the use of the composite material is a novel invention and clearly greater than a simple sum of its parts.
  • composite cubic solid solutions produced having strontium oxide or similar oxide NOx scavenger therein can adsorb NOx at low operating temperatures (e.g., below 350 0 C) and release NOx at higher operating temperatures (e.g., above 350 0 C).
  • the solid solutions can provide added catalytic functions, whereon NO is oxidized to NO 2 fuel-lean operation or, conversely, NOx is chemically converted/reduced to nitrogen under fuel- rich conditions.
  • the washcoat employed utilized less NOx adsorber (by wt.%) than the barium oxide NOx adsorbers currently employed.
  • these NOx adsorbers will exhibit a higher resistance to sulfur poisoning and can be desulfated at a lower temperature than non- lattice based NOx adsorbers.
  • the strontium-based NOx adsorber employed does not present the toxicity concerns as compared to barium or potassium oxides.
  • ranges are inclusive and independently combinable (e.g., ranges of 'up to about 25 wt.%, or, more specifically, about 5 wt.% to about 20 wt.%,' is inclusive of the endpoints and all intermediate values of the ranges of 'about 5 wt.% to about 25 wt.%,' etc.).
  • the modifier 'about' used in connection with a quantity is inclusive of the stated value and has the meaning dictated by the context (e.g., includes the degree of error associated with measurement of the particular quantity).
  • '(s)' as used herein is intended to include both the singular and the plural of the term that it modifies, thereby including one or more of that term (e.g., the colorant(s) includes one or more colorants).
  • 'combination' is inclusive of blends, mixtures, alloys, reaction products, and the like.

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Abstract

La présente invention concerne un capteur de NOx à base d'oxydes métalliques mixtes, cristallin, monophasique et composite, qui forme une solution solide présentant une structure cristalline monophasique bien définie, tel que déterminé par le biais d'une méthode par diffraction des rayons X classique; ainsi qu'un capteur de NOx placé dans la structure d'oxyde monophasique, sans formation de phase discrète de rayons X supplémentaire. Le capteur de NOx est composé d'oxydes d'un élément choisi dans le groupe formé par les métaux alcalins, les métaux alcalinoterreux, les métaux de transition, les métaux des terres rares et des mélanges de ceux-ci. L'oxyde monophasique susmentionné peut présenter une structure de fluorine cubique et il est avantageux d'utiliser le capteur de NOx à base d'oxyde cubique composite pour contrôler des émissions, à la fois de nature gazeuse et solide ou particulaire, de combustions internes, notamment de moteurs fonctionnant selon le principe de l'allumage par compression.
PCT/EP2009/002261 2008-03-27 2009-03-27 Solutions solides et procédés de fabrication correspondant WO2009118188A1 (fr)

Applications Claiming Priority (9)

Application Number Priority Date Filing Date Title
US3987908P 2008-03-27 2008-03-27
US61/039,879 2008-03-27
US61/308,879 2008-03-27
US12/240,170 2008-09-29
US12/240,170 US20090246109A1 (en) 2008-03-27 2008-09-29 Solid solutions and methods of making the same
US12/363,329 2009-01-30
US12/363,310 US9403151B2 (en) 2009-01-30 2009-01-30 Basic exchange for enhanced redox OS materials for emission control applications
US12/363,329 US20100196217A1 (en) 2009-01-30 2009-01-30 Application of basic exchange os materials for lower temperature catalytic oxidation of particulates
US12/363,310 2009-01-30

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WO2009118188A1 true WO2009118188A1 (fr) 2009-10-01

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PCT/US2009/038403 WO2010002486A2 (fr) 2008-03-27 2009-03-26 Régulation continue des suies de diesel avec une pénalité minimale de contre-pression à l’aide de substrats d’écoulement conventionnels et d’un catalyseur actif d’oxydation directe des suies disposé sur ceux-ci
PCT/EP2009/002261 WO2009118188A1 (fr) 2008-03-27 2009-03-27 Solutions solides et procédés de fabrication correspondant
PCT/EP2009/002263 WO2009118190A2 (fr) 2008-03-27 2009-03-27 Application de matériaux de stockage d'oxygène (os) d'échange basique pour une oxydation catalytique de matières particulaires à basse température
PCT/EP2009/002262 WO2009118189A1 (fr) 2008-03-27 2009-03-27 Échange basique pour des matériaux de stockage d'oxygène (os) redox évolués destinés à des applications de contrôle des émissions

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PCT/EP2009/002262 WO2009118189A1 (fr) 2008-03-27 2009-03-27 Échange basique pour des matériaux de stockage d'oxygène (os) redox évolués destinés à des applications de contrôle des émissions

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WO2011085923A1 (fr) * 2009-12-21 2011-07-21 Bernhard Kahlert Catalyseur piège à no2
US9205378B2 (en) 2009-12-21 2015-12-08 Bernhard Kahlert NO2 slip catalyst
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US8980209B2 (en) 2012-12-12 2015-03-17 Basf Corporation Catalyst compositions, catalytic articles, systems and processes using protected molecular sieves
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CN104415744A (zh) * 2013-09-10 2015-03-18 湖南稀土金属材料研究院 多元镨基储氧材料Pr-Zr-Tb-Y-Sc的制备方法
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KR20100135858A (ko) 2010-12-27
CN102006923A (zh) 2011-04-06
WO2009118189A1 (fr) 2009-10-01
WO2009118190A4 (fr) 2010-03-18
WO2010002486A3 (fr) 2010-03-25
JP2011515221A (ja) 2011-05-19
CN101980778A (zh) 2011-02-23
WO2009118190A2 (fr) 2009-10-01
WO2009118190A3 (fr) 2010-01-21
CN102006923B (zh) 2014-08-27
BRPI0909377A2 (pt) 2017-06-13
JP2011526197A (ja) 2011-10-06
BRPI0909386A2 (pt) 2015-10-06
WO2010002486A2 (fr) 2010-01-07
WO2009118189A4 (fr) 2009-11-19
EP2268395A2 (fr) 2011-01-05
EP2259870A4 (fr) 2017-11-15
KR20160129913A (ko) 2016-11-09
CN102112223A (zh) 2011-06-29
KR20110008190A (ko) 2011-01-26

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