WO2013060487A1 - Composition de catalyseur et procédé d'utilisation dans une réduction catalytique sélective d'oxydes d'azote - Google Patents

Composition de catalyseur et procédé d'utilisation dans une réduction catalytique sélective d'oxydes d'azote Download PDF

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Publication number
WO2013060487A1
WO2013060487A1 PCT/EP2012/058003 EP2012058003W WO2013060487A1 WO 2013060487 A1 WO2013060487 A1 WO 2013060487A1 EP 2012058003 W EP2012058003 W EP 2012058003W WO 2013060487 A1 WO2013060487 A1 WO 2013060487A1
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Prior art keywords
zeolite
catalyst composition
catalyst
beta
components
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PCT/EP2012/058003
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English (en)
Inventor
Alexandr Yu Stakheev
Marie GRILL
Arkady Kustov
Original Assignee
Haldor Topsøe A/S
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Publication date
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Priority to JP2014537523A priority Critical patent/JP6112734B2/ja
Priority to CA2853154A priority patent/CA2853154C/fr
Priority to CN201280052240.5A priority patent/CN103889569B/zh
Priority to IN2950CHN2014 priority patent/IN2014CN02950A/en
Priority to RU2014120917A priority patent/RU2608616C2/ru
Priority to BR112014008669-9A priority patent/BR112014008669B1/pt
Priority to US14/353,620 priority patent/US9168517B2/en
Priority to AU2012327482A priority patent/AU2012327482A1/en
Priority to EP12721442.7A priority patent/EP2771111A1/fr
Priority to KR1020147013999A priority patent/KR101789114B1/ko
Publication of WO2013060487A1 publication Critical patent/WO2013060487A1/fr

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/72Copper
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/92Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • B01D53/9404Removing only nitrogen compounds
    • B01D53/9409Nitrogen oxides
    • B01D53/9413Processes characterised by a specific catalyst
    • B01D53/9418Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation 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
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/92Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • B01D53/944Simultaneously removing carbon monoxide, hydrocarbons or carbon making use of oxidation catalysts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00Catalysts comprising molecular sieves
    • B01J29/04Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/70Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00Catalysts comprising molecular sieves
    • B01J29/04Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/70Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
    • B01J29/7007Zeolite Beta
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2251/00Reactants
    • B01D2251/20Reductants
    • B01D2251/206Ammonium compounds
    • B01D2251/2062Ammonia
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2255/00Catalysts
    • B01D2255/20Metals or compounds thereof
    • B01D2255/206Rare earth metals
    • B01D2255/2065Cerium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2255/00Catalysts
    • B01D2255/20Metals or compounds thereof
    • B01D2255/207Transition metals
    • B01D2255/2073Manganese
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2255/00Catalysts
    • B01D2255/20Metals or compounds thereof
    • B01D2255/207Transition metals
    • B01D2255/20738Iron
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2255/00Catalysts
    • B01D2255/20Metals or compounds thereof
    • B01D2255/207Transition metals
    • B01D2255/20761Copper
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2255/00Catalysts
    • B01D2255/20Metals or compounds thereof
    • B01D2255/209Other metals
    • B01D2255/2092Aluminium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2255/00Catalysts
    • B01D2255/40Mixed oxides
    • B01D2255/407Zr-Ce mixed oxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2255/00Catalysts
    • B01D2255/50Zeolites
    • B01D2255/502Beta zeolites

Definitions

  • the present invention relates to catalyst composition for use in selective reduction of nitrogen oxides in off-gases by reaction with ammonia or a precursor thereof.
  • Catalysts for NH 3 -SCR i.e. selective reduction of nitrogen oxides (NOx) by use of ammonia as reductant are well known in the art.
  • Those catalysts include zeolitic material, op ⁇ tionally promoted with copper or iron
  • the catalyst composition and method of this invention shall further include soot and hydrocarbon oxidation activity simultaneously with the DeNOx activity.
  • catalyst composition comprising a one or more acidic zeolite or zeotype components physically ad- mixed with one ore more redox active metal compounds shown an improved activity in the selective reduction of nitrogen oxides and oxidation of hydrocarbons, CO and soot contained in off-gas.
  • redox active metal compounds as used herein re ⁇ lates to metal compounds which reversibly can be oxidized and reduced in terms of changes in oxidation number, or oxidation state, of the metal atom or compound.
  • the present invention pro ⁇ vides a catalyst composition for selective reduction of nitrogen oxides and soot oxidation comprising one or more acidic zeolite or zeotype components selected from the group consisting of BEA, MFI, FAU, FER, CHA, MOR or mixtures thereof physically admixed with one ore more redox active metal compounds selected from the group consisting of Cu/Al 2 0 3 , Mn/Al 2 0 3 , Ce0 2 -Zr0 2 , Ce-Mn/Al 2 0 3 and mixtures thereof.
  • Catalyst compositions prepared by mechanical mixing of the above mentioned zeolites or zeotype materials and redox metal components mixing according to the invention exhibit a pronounced synergistic effect. DeNO x activity of such composite catalysts significantly exceeds activity of their individual components.
  • the acidic zeolite or zeotype component can be used in pro- tonic form or promoted with Fe .
  • the weight ratio between the zeolite components and the redox components is between 1:1 to 1:50
  • the redox components are dispersed on a support selected from the group consisting of of AI2O3, T 1 O2 , S 1 O2 , Ce02 , r02 or mixtures thereof.
  • the mean molar ratio Si/Al of the zeolite components according to the invention is from 5 to 100.
  • the above described catalyst composition according to the invention can be utilised as coating material or as coat on structured bodies of metallic, ceramic, metal oxide, SiC or silica materials or fibres.
  • the invention provides furthermore a monolithic structured body being coated with a catalyst composition according to anyone of the above disclosed embodiments of the invention.
  • the monolithic structured body is preferably made from me ⁇ tallic, ceramic, metal oxide, SiC or silica fiber materi ⁇ als .
  • the monolithic structured body may be in form of a particle filter, e.g. a honeycomb structured filter or a wall flow filter .
  • the catalyst composition is coated on the body in of two or several separate catalyst layers in series or as two or several catalyst layers in parallel and wherein the layers have different compositions or layer thicknesses.
  • amount of expensive zeolite/zeotype com ⁇ ponent in the composite catalyst can be significantly re ⁇ substituted by its replacement with equivalent volume of redox component.
  • overall volume of the catalyst re- mains constant, but the amount of zeolite component can be decreased by 2-5 times, without notable sacrificing DeNO x performance.
  • Ce-Mn/Al 2 03 component is used for the catalyst preparation, notable improvement of NOx conversion at Treact ⁇ 250°C is observed despite decreased amount of zeolite component.
  • the invention provides additionally a method for the selec ⁇ tive reduction of nitrogen oxides and oxidation of soot contained in an off-gas comprising the step of contacting the off-gas in presence of ammonia with a catalyst composi ⁇ tion comprising one or more acidic zeolite or zeotype com ⁇ ponents selected from the group consisting of BEA, MFI, FAU, FER, CHA, MOR or mixtures thereof physically admixed with one ore more redox active metal compounds selected from the group consisting of CU/AI 2 O 3 , ⁇ / ⁇ 2 ⁇ 3 , Ce0 2 ⁇ Zr0 2 , Ce-Mn/Al 2 03 and mixtures thereof.
  • the acidic zeolite or zeotype component can be used in pro- tonic form or promoted with Fe
  • the one or more redox active metal compounds are dispersed on a support se ⁇ lected from the group consisting of AI2O3, T1O2, S1O2, Zr02 or mixtures thereof.
  • the cata ⁇ lyst composition is contacted with the off-gas at a tem ⁇ perature below 250°C.
  • excess of ammonia is selectively oxidized to nitrogen by contact with the catalyst composition.
  • Example 1 Synergistic effect in NH 3 -DeNOx over Ce02-Zr02 + H-Beta zeolite catalyst compositions.
  • the pow ⁇ ders were thoroughly grinded in agate mortar for 10-15 min, followed by pelletization . The pellets were crushed and sieved collecting 0.2 - 0.4 mm fraction for catalytic test.
  • pelletized 74wt%Ce0 2 -26wt%Zr0 2 , H-Beta, and Fe- Beta zeolite were used as reference samples.
  • the catalysts were tested in the NH 3 -DeNOx in the tempera- ture range of 150-550 °C.
  • the test was performed under fol ⁇ lowing conditions: decreasing reaction temperature with a rate of 2°C/min, feed gas composition: 500 ppm NO, 540 ppm N3 ⁇ 4, 10 vol % O 2 , 6 vol% H 2 O, balanced with 2 to obtain a total flow of 300 mL/min.
  • NO x conversion over composite catalyst is similar to NO x conversion over commercial Fe-Beta zeolite (Fe-Beta) at 230-550°C, and exceeds NO x conversion over Fe-Beta zeolite at 150-200°C.
  • a first sample was prepared by mixing 74wt%Ce0 2 ⁇ 26wt%Zr0 2 and Fe-Beta zeolite powders at a weight ratio of 3.3. This weight ratio results in a volume ratio of 74wt%Ce02 ⁇
  • 26wt%Zr0 2 /Fe-Beta components in composite catalyst 1/1.
  • a second sample was prepared by mixing 74wt%Ce0 2 ⁇ 26wt%Zr0 2 and Fe-Beta powders at a weight ratio of 10.
  • For the second sample volume ratio of 74wt%Ce0 2 ⁇ 26wt%Zr0 2 /Fe-Beta zeolite equals 3/1.
  • the first sample with 1/1 volume component ratio [0.065g 74%Ce0 2 -Zr0 2 + 0.02g Fe-Beta zeolite].
  • the second sample with 3/1 volume component ratio [0.197g 74%Ce0 2 -Zr0 2 + 0.02g Fe-Beta zeolite].
  • Reference sample 0.02 g Fe-Beta zeolite.
  • the catalysts were tested in NH 3 -DeNO x within the tempera ⁇ ture range of 150-550 °C.
  • the test was performed under fol ⁇ lowing conditions: decreasing reaction temperature with a rate of 2°C/min, feed gas composition: 500 ppm NO, 540 ppm NH 3 , 10 vol % 0 2 , 6 vol% H 2 0, balanced with N 2 to obtain a total flow of 300 mL/min.
  • [Ce0 2 -Zr0 2 + Fe-Beta zeolite] composite catalysts showed enhanced DeNO x activity within low-temperature range (150-300°C), which significantly ex ⁇ ceeded activity of individual Fe-Beta zeolite, as shown in Fig. 2. It is important to note that the activity of [Ce0 2 ⁇ Zr0 2 + Fe-Beta zeolite] is improved when the amount of Ce02 ⁇ Zr02 component was increased.
  • a first sample was prepared by mixing 74wt%Ce02 ⁇ 26wt%Zr02 and Fe-Beta powders at a weight ratio of 3.3. In this case volume ratio of 74wt% Ce02 ⁇ 26wt% Zr02 /Fe-Beta zeolite equals 1/1.
  • a second sample was prepared by mixing 74wt%Ce0 2 ⁇ 26wt%Zr0 2 and Fe-Beta zeolite powders at a weight ratio of 15.5. For the second sample volume ratio of 74wt%Ce02 ⁇ 26wt%Zr02 and Fe-Beta zeolite components equals 5/1.
  • a third sample was prepared by was prepared by mixing
  • Second sample [0.109g 74wt%Ce02 ⁇ Zr0 2 + 0.007g Fe-Beta zeolite].
  • Reference sample 0.02 g Fe beta-zeolite.
  • Feed gas composition 540 ppm NH 3 , 500 ppm NO, 10 % 0 2 , 6 % H 2 0 balance with N 2 .
  • the powders were thoroughly grinded in agate mortar for 10-15 min, followed by pelleti- zation. The pellets were crushed and sieved collecting 0.2 - 0.4 mm fraction for catalytic test. Similarly pelletized Fe-Beta was used as reference.
  • the catalysts were tested in the NH 3 -DeNOx in the tempera ⁇ ture range of 150-550 °C.
  • the test was performed under fol ⁇ lowing conditions: decreasing reaction temperature with a rate of 2°C/min, feed gas composition: 500 ppm NO, 540 ppm NH 3 , 10 vol % O 2 , 6 vol% 3 ⁇ 40, balanced with 2 to obtain a total flow of 300 mL/min.
  • Catalyst load 0.04g Fe-Beta and
  • the first sample with 1/1 weight component ratio [0.040g 10wt%Cu/Al 2 O 3 + 0.040g H-Beta].
  • the second sample with 1/1 weight component ratio [0.040g 10wt%Cu/Al 2 O 3 + 0.040g H-ZSM-5].
  • the third sample with 1/1 weight component ratio [0.040g 10wt%Cu/Al 2 O 3 + 0.040g H-ferrierite ] .
  • Reference samples 0.040 g H-Beta; 0.040g H-ZSM-5, or H- ferrierite, or 0.040 g 10wt%Cu/Al 2 O 3 .
  • the catalysts were tested in NH 3 -DeNO x within the tempera ⁇ ture range of 150-550 °C. The test was performed under fol ⁇ lowing conditions: decreasing reaction temperature with a rate of 2°C/min, feed gas composition: 500 ppm NO, 540 ppm NH 3 , 10 vol % 0 2 , 6 vol% H 2 0, balanced with N 2 to obtain a total flow of 300 mL/min.
  • GHSV 270, 000 h "1 .

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Biomedical Technology (AREA)
  • Combustion & Propulsion (AREA)
  • Health & Medical Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Crystallography & Structural Chemistry (AREA)
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  • Exhaust Gas Treatment By Means Of Catalyst (AREA)
  • Exhaust Gas After Treatment (AREA)

Abstract

La présente invention a trait à une composition de catalyseur destinée à la réduction sélective d'oxydes d'azote et à l'oxydation de suies, ladite composition comprenant un mélange physique d'un ou de plusieurs composants de type zéolite ou de zéolite acide avec un ou plusieurs composés de métal actif d'oxydo-réduction. L'invention a également trait à un procédé destiné à la réduction sélective d'oxydes d'azote et à l'oxydation de suies par le biais de l'utilisation de la composition de catalyseur.
PCT/EP2012/058003 2011-10-24 2012-05-02 Composition de catalyseur et procédé d'utilisation dans une réduction catalytique sélective d'oxydes d'azote WO2013060487A1 (fr)

Priority Applications (10)

Application Number Priority Date Filing Date Title
JP2014537523A JP6112734B2 (ja) 2011-10-24 2012-05-02 触媒組成物および窒素酸化物の選択的触媒還元における使用方法
CA2853154A CA2853154C (fr) 2011-10-24 2012-05-02 Composition de catalyseur et procede d'utilisation dans une reduction catalytique selective d'oxydes d'azote
CN201280052240.5A CN103889569B (zh) 2011-10-24 2012-05-02 用于选择性催化还原氮的氧化物的催化剂组合物及方法
IN2950CHN2014 IN2014CN02950A (fr) 2011-10-24 2012-05-02
RU2014120917A RU2608616C2 (ru) 2011-10-24 2012-05-02 Каталитическая композиция и способ применения в селективном каталитическом восстановлении оксидов азота
BR112014008669-9A BR112014008669B1 (pt) 2011-10-24 2012-05-02 Composição de catalisador e método para utilização em reduções catalíticas de óxidos de nitrogênio
US14/353,620 US9168517B2 (en) 2011-10-24 2012-05-02 Catalyst composition and method for use in selective catalytic reduction of nitrogen oxides
AU2012327482A AU2012327482A1 (en) 2011-10-24 2012-05-02 Catalyst composition and method for use in selective catalytic reduction of nitrogen oxides
EP12721442.7A EP2771111A1 (fr) 2011-10-24 2012-05-02 Composition de catalyseur et procédé d'utilisation dans une réduction catalytique sélective d'oxydes d'azote
KR1020147013999A KR101789114B1 (ko) 2011-10-24 2012-05-02 질소 산화물의 선택적 촉매 환원에서 사용하기 위한 촉매 조성물 및 방법

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
PCT/EP2011/005344 WO2013060341A1 (fr) 2011-10-24 2011-10-24 Composition de catalyseur s'utilisant dans la réduction catalytique sélective d'oxydes d'azote
EPPCT/EP2011/005344 2011-10-24

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PCT/EP2011/005344 WO2013060341A1 (fr) 2011-10-24 2011-10-24 Composition de catalyseur s'utilisant dans la réduction catalytique sélective d'oxydes d'azote
PCT/EP2012/058003 WO2013060487A1 (fr) 2011-10-24 2012-05-02 Composition de catalyseur et procédé d'utilisation dans une réduction catalytique sélective d'oxydes d'azote

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JP (1) JP6112734B2 (fr)
KR (1) KR101789114B1 (fr)
CN (1) CN103889569B (fr)
AU (1) AU2012327482A1 (fr)
BR (1) BR112014008669B1 (fr)
CA (1) CA2853154C (fr)
CL (1) CL2014000993A1 (fr)
IN (1) IN2014CN02950A (fr)
MX (1) MX2014004494A (fr)
RU (1) RU2608616C2 (fr)
WO (2) WO2013060341A1 (fr)

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CL2014000993A1 (es) 2014-08-22
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AU2012327482A1 (en) 2014-05-15
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CA2853154C (fr) 2018-04-03
BR112014008669B1 (pt) 2019-07-02
RU2608616C2 (ru) 2017-01-23
IN2014CN02950A (fr) 2015-07-03
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