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WO1990008589A1 - Catalyseur de type perovskite et ses modes d'utilisation - Google Patents

Catalyseur de type perovskite et ses modes d'utilisation Download PDF

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Publication number
WO1990008589A1
WO1990008589A1 PCT/GB1990/000060 GB9000060W WO9008589A1 WO 1990008589 A1 WO1990008589 A1 WO 1990008589A1 GB 9000060 W GB9000060 W GB 9000060W WO 9008589 A1 WO9008589 A1 WO 9008589A1
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WO
WIPO (PCT)
Prior art keywords
perovskite
oxide
catalyst
deficiency
type
Prior art date
Application number
PCT/GB1990/000060
Other languages
English (en)
Inventor
Brian Ellis
Alan Ivor Foster
Original Assignee
The British Petroleum Company Plc
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 The British Petroleum Company Plc filed Critical The British Petroleum Company Plc
Publication of WO1990008589A1 publication Critical patent/WO1990008589A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/78—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali- or alkaline earth metals
    • 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
    • B01D53/9445—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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/72—Copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/20—Reductants
    • B01D2251/204—Carbon monoxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/10—Noble metals or compounds thereof
    • B01D2255/102—Platinum group metals
    • B01D2255/1026—Ruthenium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/206—Rare earth metals
    • B01D2255/2063—Lanthanum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/2073—Manganese
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20738—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20746—Cobalt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20761—Copper
    • 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
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • 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 novel mixed oxides with a perovskite-type structure.
  • Perovskite is a naturally occurring mineral of formula CaTi ⁇ 3. However many mixed oxides eg. BaTi03 are known which have the same structure. Perovskite-type mixed oxides correspond to a general formula ABO3. A normally corresponds to a relatively large cation eg. greater than 0.1 nm. B normally corresponds to a smaller cation e.g. smaller than 0.1 nm. Thus the A type cation corresponds to Ba in barium titanate and the B-type ion corresponds to Ti in barium titanate. (see J.B. Goodenough and J.M. Londo in "Landolt-B ⁇ rnstein" Vol 4. (1970)).
  • perovskite-type material is one which is isostructural with perovskite, i.e. in which the intensities of the X-ray diffraction lines and their positions substantially correspond to those of perovskite.
  • the oxides which have been investigated include those in which the cations of 3 or more metals are present in place of the 2 cations present in perovskite itself. These mixed oxides may have normal oxygen stoichiometry. • They may however be made in oxygen-deficient form i.e. where, in the formula ABO n , n is less than 3.
  • Gallagher et al, J. American Ceramic Soc, 60(1-2) 28-31 (1977) discloses the preparation of mixed oxides with the perovskite-type structure of formula aMn ⁇ _ x Cu x ⁇ 3_y, and their use in the oxidation of CO as a potential catalyst for the control for automotive emissions.
  • the value of y is not given in all cases but one or two nominal compositions are given in which 3-y is 2.96 or 2.93.
  • the oxygen deficiencies are thus only 0.04 to 0.07, and the compounds are only marginally oxygen deficient.
  • a novel mixed metal oxide has a perovskite-type structure characterised in that it has a general formula AB ⁇ 3_y in which A corresponds to a relatively large cation and B corresponds to a relatively smaller cation and y represents a calculated oxygen deficiency (y) of greater than 0.1, there are at least two transition metals in the B position of the perovskite-type structure AB ⁇ 3_y, one of which is Cu.
  • the value of 3.5+ for Co and Fe is used on the basis of the existence of perovskite-type oxides in which this is observed i.e.
  • the catalyst of the present invention is defined on the basis of calculated oxygen deficiency.
  • the calculated oxygen deficiency will generally correspond comparatively closely to the measured oxygen deficiency (where this can be determined) for catalysts subjected to heating during or after preparation to temperatures of not more than 900°C.
  • Preferred catalysts according to the invention are thus those in which temperatures of 900 ⁇ C have not been exceeded during the catalyst preparation or subsequently.
  • the predicted oxygen deficiency is preferably from 0.1 to 0.5, more preferably from 0.2 to 0.5.
  • the A positions are preferably occupied by La cations together with cations of metals of Groups IA or IIA of the Periodic Table.
  • An example of a suitable IIA metal is strontium.
  • the requirement for oxygen-deficiency will generally mean that there will be A site cations from at least two different metals e.g. La and Sr as indicated above.
  • the preferred molar ratio where there are two A site metals is in the range 0.1 to 0.9.
  • the molar ratio of Cu to the other transition metal is preferably in the range 0.1 to 0.9.
  • the ratio of the A site to the B site cations must be consistent with the requirements for calculated oxygen-deficiency requirements set out above.
  • Examples of the transition metals which may be present in the B position in addition to Cu are Fe, Co, Mn, V and Ru, Group VA and VIIA.
  • the mixed oxides may be prepared by controlled precipitation by addition of metal salt aqueous solutions (e.g. nitrates) and base aqueous solutions (e.g. sodium or potassium carborates).
  • the precipitates after filtration and washing may be calcined e.g. at temperatures in the range 650-750 ⁇ C.
  • the calcination step is preferably carried out in air.
  • the process for the conversion of NO to N2 by passing a gas containing CO and NO over catalysts at elevated temperatures and in the substantial absence of molecular oxygen is characterised in that the catalyst is a mixed oxide catalyst which has a perovskite-type structure with a calculated oxygen-deficiency y of greater than 0.1, and has at least two transition metals in the B position of the perovskite-type related structure AB ⁇ 3_y, one of which is Cu.
  • elevated temperatures which may be used are those in the range 100 to 1000"C.
  • a process for the oxidation of oxidisable vapour comprises passing the vapour in an oxygen-containing atmosphere over a catalyst which is a mixed metal oxide which has a perovskite-type structure with a calculated oxygen-deficiency y of greater than 0.1, and has at least two transition metals in the B position of the perovskite-type related structure ABQ3_ y , one of which is Cu.
  • elevated temperatures which may be used are those in the range 100 to 1000"C.
  • the above described processes are particularly suitable for application to the exhaust gases produced by internal combustion engines, in particular to the exhaust gases produced by automobile engines. They are particularly suitable for application to exhaust gases from gasoline engines.
  • the catalytic material preferably comprises predominantly perovskite-type material e.g. greater than 90% wt/wt. Preferably it comprises at least 90% wt/wt of perovskite-type material.
  • the catalyst material may, of course, be supported on inactive carriers or supports as is well-known in the art.
  • the aim of the experiment was to co-precipitate the component metals as carbonates/oxides using the method of constant-pH precipitation.
  • a fixed pH is chosen which correlates with the pH required for precipitation of each metal component, information derived from literature sources.
  • distilled water was placed in a large beaker (typically 300 ml) with stirring from a overhead stirrer ("Silverson") plus pH measurement using an immersible pH electrode connected to a pH meter.
  • the starting pH of the water was monitored and was typically
  • the second stage involved the computer-controlled addition of both base and mixed metal component solutions to the water in the beaker so as to bring about precipitation at constant pH.
  • the pH of the water was increased to the desired level by a controlled addition of base.
  • an aliquot of metal solution typically 3 ml was added to the stock solution. This depressed the pH slightly due to the metal nitrate or acetate solution being acidic.
  • the computer then restored the pH to the original level by controlled base addition.
  • the amount of base necessary to achieve this is exactly equal to that needed to precipitate the metal ions present, plus the small extra amount required to raise the pH to the original level. In this way, complete precipitation was ensured without the use of excessive quantities of base which might contaminate the precipitate.
  • the products of the above preparation were studied using powder X-ray diffraction and were found to contain predominantly material of perovskite structure (believed to be greater than 90%). The presence of extraneous phases, such as CuO, SrC03, Mn3U was detected in all cases but was sufficiently small to allow subsequent catalyst testing. Analysis by X-ray fluorescence revealed good compositional purity and confirmed that levels of potassium impurity from the preparation process were less than 3 mole %.
  • Catalyst test apparatus and methods The apparatus used for catalytic testing of the samples consisted of three main parts, the inlet gas-handling system, the catalytic reactor with furnace and the gas chromatograph analysis system. The operation of each of these sections can be described as follows: The input gases (10% CO/10% NO in He) were mixed as required using mass flow controllers and could be admitted into the catalytic reactor or analysed separately via a by-pass.
  • a second injection was made onto a similar column containing "Porapak QS", which was used to separate co 2» N 2» and N 2°* Total analysis time was 9 minutes. All chromatographic data was analysed and recorded by a computing integrator.
  • the catalytic activity for the CO/NO reaction was measured as a function of temperature for several novel Cu-M perovskite oxides prepared according to the invention. Table 1 shows the results expressed as the temperature for 50% conversion of CO to CO2 and NO to N2 as a result of CO/NO reaction. All the catalysts are seen to have good activity for promoting this reaction.
  • Examples 4 and 5 Some of the perovskite catalysts prepared according to the invention and described in Example 1 were tested under conditions of increased gas throughout (GHSV) and reduced concentration of the active components (CO and NO). The conditions used (0.5% v / v CO, 0.5 V / V NO,
  • GHSV 30,000 h -i GHSV 30,000 h -i
  • Example 4-5 The activity under the conditions used for Example 4-5 of a catalyst not according to the invention is shown in Table 4. Its lower activity is apparent; production of nitrous oxide (N2O) was also observed, an undesirable result. The results are shown in Table 4.
  • perovskites prepared according to the invention and described in Examples 1-3 were tested for their activity in the oxidation of carbon monoxide and hydrocarbons that are difficult and easy respectively to oxidise.
  • the conditions used GHSV •* ⁇ 30,000h ⁇ l, 0.5% of CO, 0.1% methane 0.1% propylene and 1.0% by volume oxygen were selected to be representative of the type of exhaust gas with which an oxidation catalyst might be employed.
  • Perovskite catalysts not according to the invention were tested under the same conditions as used in Examples 6-8.
  • the results (Table 6) show that these catalysts are not as active as those prepared according to the invention and containing Fe or Co (Table 5). This is notwithstanding the fact that the perovskite La ⁇ _ x Sr x COJ.Q O3 (x - about 0.3) is claimed to be particularly active for methane oxidation (H. Akai, T. Yamada, K. Eguchi and T. Seijama; Applied Catalysis 2 (1986), 265).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Biomedical Technology (AREA)
  • Environmental & Geological Engineering (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Catalysts (AREA)

Abstract

L'invention concerne un oxyde de métal mélangé présentant une structure ABO¿3-y¿ du type perovskite, dans laquelle A correspond à un cation relativement grand et B correspond à un cation relativement petit, ayant un manque d'oxygène y d'au moins 0,1 , et ayant au moins deux métaux de transition dans la position B, l'un étant Cu. L'oxyde est utile dans la transformation de NO en N¿2? dans des mélanges contenant CO et NO.
PCT/GB1990/000060 1989-01-24 1990-01-16 Catalyseur de type perovskite et ses modes d'utilisation WO1990008589A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB898901514A GB8901514D0 (en) 1989-01-24 1989-01-24 Perovskite-type catalyst
GB8901514.3 1989-01-24

Publications (1)

Publication Number Publication Date
WO1990008589A1 true WO1990008589A1 (fr) 1990-08-09

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GB (1) GB8901514D0 (fr)
WO (1) WO1990008589A1 (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0788828A3 (fr) * 1996-02-09 1997-08-27 Isuzu Ceramics Res Inst
US5851501A (en) * 1995-05-09 1998-12-22 Daimler-Benz Ag Process for absorbing and desorbing nitrogen oxides in exhaust gases
EP0923990A1 (fr) * 1997-12-09 1999-06-23 Honda Giken Kogyo Kabushiki Kaisha Catalyseur composite pour le traitement de gaz d'échappement
WO1999061138A1 (fr) * 1998-05-27 1999-12-02 Electric Power Research Institute, Inc. Catalyseur permettant d'extraire des oxydes d'azote de flux d'echappement en l'absence d'agent reducteur
US6580000B1 (en) 2002-06-06 2003-06-17 Ak Research Company Process for the manufacture of alkoxysilanes and alkoxy orthosilicates
US20110076212A1 (en) * 2008-10-03 2011-03-31 Gm Global Technology Operations, Inc. Methods and systems for oxidizing nitric oxide in a gas stream
US7964167B2 (en) * 2008-10-03 2011-06-21 GM Global Technology Operations LLC Method and architecture for oxidizing nitric oxide in exhaust gas from hydrocarbon fuel source with a fuel lean combustion mixture
US8268274B2 (en) 2008-10-03 2012-09-18 GM Global Technology Operations LLC Catalyst combinations and methods and systems for oxidizing nitric oxide in a gas stream

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3865923A (en) * 1973-03-19 1975-02-11 Ethyl Corp Catalyst
US4080433A (en) * 1975-03-10 1978-03-21 University Of Southern California Process for the catalytic oxidation of hydrocarbons with the oxides of nitrogen

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3865923A (en) * 1973-03-19 1975-02-11 Ethyl Corp Catalyst
US4080433A (en) * 1975-03-10 1978-03-21 University Of Southern California Process for the catalytic oxidation of hydrocarbons with the oxides of nitrogen

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5851501A (en) * 1995-05-09 1998-12-22 Daimler-Benz Ag Process for absorbing and desorbing nitrogen oxides in exhaust gases
EP0788828A3 (fr) * 1996-02-09 1997-08-27 Isuzu Ceramics Res Inst
US5728643A (en) * 1996-02-09 1998-03-17 Isuzu Ceramics Research Institute Co., Ltd. NOx decomposition catalyst and exhaust gas purifier using said catalyst
EP0923990A1 (fr) * 1997-12-09 1999-06-23 Honda Giken Kogyo Kabushiki Kaisha Catalyseur composite pour le traitement de gaz d'échappement
US6261990B1 (en) 1997-12-09 2001-07-17 Honda Giken Kogyo Kabushiki Kaisha Composite catalyst for purification of exhaust gas
WO1999061138A1 (fr) * 1998-05-27 1999-12-02 Electric Power Research Institute, Inc. Catalyseur permettant d'extraire des oxydes d'azote de flux d'echappement en l'absence d'agent reducteur
US6580000B1 (en) 2002-06-06 2003-06-17 Ak Research Company Process for the manufacture of alkoxysilanes and alkoxy orthosilicates
US6680399B2 (en) 2002-06-06 2004-01-20 Ak Research Company Process for the manufacture of alkoxysilanes and alkoxy orthosilicates
US20110076212A1 (en) * 2008-10-03 2011-03-31 Gm Global Technology Operations, Inc. Methods and systems for oxidizing nitric oxide in a gas stream
US7964167B2 (en) * 2008-10-03 2011-06-21 GM Global Technology Operations LLC Method and architecture for oxidizing nitric oxide in exhaust gas from hydrocarbon fuel source with a fuel lean combustion mixture
US8268274B2 (en) 2008-10-03 2012-09-18 GM Global Technology Operations LLC Catalyst combinations and methods and systems for oxidizing nitric oxide in a gas stream
US8377400B2 (en) * 2008-10-03 2013-02-19 GM Global Technology Operations LLC Methods and systems for oxidizing nitric oxide in a gas stream

Also Published As

Publication number Publication date
AU4845790A (en) 1990-08-24
GB8901514D0 (en) 1989-03-15

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