WO2020148784A1 - Catalyseur dénox à basse température et durable et son procédé de préparation - Google Patents

Catalyseur dénox à basse température et durable et son procédé de préparation Download PDF

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Publication number
WO2020148784A1
WO2020148784A1 PCT/IN2020/050046 IN2020050046W WO2020148784A1 WO 2020148784 A1 WO2020148784 A1 WO 2020148784A1 IN 2020050046 W IN2020050046 W IN 2020050046W WO 2020148784 A1 WO2020148784 A1 WO 2020148784A1
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Prior art keywords
zeolite
range
catalyst
slurry
type
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PCT/IN2020/050046
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English (en)
Inventor
Vishnuvarthan MUTHUSAMY
Matti Harkonen
Rajan Bosco
Arvind Kumar
Alok TRIGUNAYAT
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Ecocat India Pvt. Ltd.
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Publication of WO2020148784A1 publication Critical patent/WO2020148784A1/fr

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    • 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
    • B01D53/9404—Removing only nitrogen compounds
    • B01D53/9409—Nitrogen oxides
    • B01D53/9413—Processes characterised by a specific catalyst
    • B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/20—Reductants
    • B01D2251/206—Ammonium compounds
    • B01D2251/2067—Urea
    • 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
    • B01D2255/20761—Copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/50—Zeolites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/90—Physical characteristics of catalysts
    • B01D2255/911—NH3-storage component incorporated in the catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/90—Physical characteristics of catalysts
    • B01D2255/92—Dimensions
    • B01D2255/9207—Specific surface

Definitions

  • the field of the present invention is related to Selective Catalytic Reduction (SCR) catalyst to abate NOx from the exhaust of a lean burn automotive engine. More particularly, this invention discloses a DeNOx catalyst consisting of one or more transition metal-doped loaded zeolite/zeolite-type materials, coated on honeycomb monolith and a method of preparing the same.
  • SCR Selective Catalytic Reduction
  • the major pollutants in automotive exhaust system include emissions such as oxides of Nitrogen (also known as NO x ), carbon monoxide, unburned hydrocarbons and particulate matter.
  • NO x plays a prominent role in the formation of smog, acid rain, ground level ozone and fine particulate matters (PM). It is therefore, become very imperative to drastically reduce or eliminate NO x emissions.
  • the legislative emission norms have globally become more and more stringent.
  • SCR SCR for reduction of NOx pollutants from vehicular emissions
  • zeolite/zeolite-type based catalysts for selective catalytic reduction of NO x to nitrogen (N 2 ) gas and steam/water (H 2 O).
  • N 2 nitrogen
  • H 2 O steam/water
  • the present invention discloses the composition and method to prepare a novel SCR catalyst, which not only gives a reasonably high, low-temperature NOx conversion but also high temperature structural stability and durability.
  • the primary objective of this invention is to formulate a SCR or DeNOx catalyst which can reduce the NO x emissions from the exhaust tail pipe of said automotive engines.
  • Another objective of the instant invention is to exhibit a reasonably high NOx conversion at low temperatures during cold start operations.
  • Yet another objective of the instant invention is to exhibit high temperature structural stability, during extremely long periods of operation on road.
  • Yet another objective of the instant invention is to be highly selective towards NO reduction to N2 compared to NO2, over a metal(s) loaded zeolite/zeolite-type based SCR catalysts during the entire temperature range of SCR system.
  • Yet another objective of this invention is to improve performance of the metal(s) or transition metal(s) or combination of metal(s) loading by inventive method on zeolite/zeolite-type based SCR catalysts during entire temperature range of SCR system.
  • Yet another objective of this invention is to recover >99% performance of the metal(s) loaded zeolite/zeolite-type based SCR catalysts after sulphur aging.
  • the instant invention discloses a metal(s) loaded zeolite/zeolite-type based catalyst and a method of manufacturing said metal(s) loaded zeolite/ zeolite-type based SCR catalyst.
  • the metal(s) loaded zeolite/zeolite-type based SCR catalyst include CHA structure type materials such as silico- aluminophosphates, aluminophosphates (A1PO-34, SAPO-34, MeAPO-34, MeAPSO-34, A1PO-47, SAPO-47, MeAPO-47, MeAPSO-47) and/or aluminosilicates loaded with metal elements such as transition metals Cu, Fe, Ni, Mn, Co, V, Ti and Zn or their combinations thereof.
  • aspects of the present invention include a method of making the metal(s) loading on zeolite/zeolite-type materials by wet and instant dry method.
  • the method includes a first step, in which an aqueous solution containing metal(s) is prepared by simple mixing of water and metal salts under stirring, a second step, in which, the zeolite/zeolite-type materials is added slowly with simultaneous mixing to the above solution, a third step, in which, the solution is stirred at elevated temperatures for few hours, a fourth step, in which, the solution is exposed suddenly at above water-evaporation temperatures until dryness, a fifth step, in which, the collected dried sample at ambient is heated in an oven again for few hours to remove any occluded water molecules and/or volatile components, a final step, in which, the sample is calcined for few hours and cooled to ambient temperature, preferably naturally.
  • aspects of the present invention include a method of making the metal(s) loaded zeolite/zeolite-type based SCR catalyst.
  • the method includes a first step, in which, a slurry of the metal(s) zeolite/zeolite-type mixture is prepared; a second optional step, in which, the slurry is coated on a honeycomb structure; a third step, in which, the slurry or the coated honeycomb is subjected to calcination; and a fourth step in which, the coated honeycomb monolith is post-treated by air- moisture mixture.
  • the post-treatment step includes heating the coated and calcined honeycomb monolith slowly from ambient to a high temperature while passing air-moisture mixture through it. After a holding period at the desired temperature, the said honeycomb monolith is allowed to reach ambient naturally.
  • One of the main advantages of this instant invention is that it will optionally eliminate/reduce the requirement/dependency of an upstream DOC (Diesel Oxidation Catalyst) in lean burn diesel engines.
  • DOC Diesel Oxidation Catalyst
  • Figures 1 illustrate preferred embodiment process for preparing, coating and post treating the transition metal(s) loaded zeolite/zeolite-type based SCR catalyst of the instant invention.
  • Figure 2 illustrate a comparative study of the X-Ray Diffraction (XRD) patterns of CuZ catalyst before and after post-treatment process.
  • Figure 3 illustrates a comparative NFb-TPD study of CuZ catalyst before and after post-treatment process.
  • Figure 4 illustrate a comparative solid state Al 27 MAS NMR study of CuZ catalyst before and after post-treatment process.
  • Figure 5 illustrate test results of NO x conversion efficiency over transition metal(s) loaded zeolite/zeolite-type based SCR catalyst such as CuZ, FeCuZ, FeZ and CuFeZ catalysts.
  • Figures 6A to 6C illustrate test results of NO x conversion efficiency Vs each mode in 7-mode cycle over CuZ catalyst, where Figure 6A shows the test results of NO x conversion efficiency, and where Figure 6B shows the test results of NO conversion efficiency, and where Figure 6C shows the test results of NO2 conversion efficiency.
  • Figures 7A and 7B illustrate test results of NO x conversion efficiency Vs temperatures over CuZ catalyst, where Figure 7A shows the test results of NO x conversion efficiency between post-treated and 3 cycles of sulphur aged at 200°C for 20 hours, where Figure 7B shows the test results of NO x conversion efficiency between post-treated and 3 cycles of regeneration at 650°C after each sulphur aged cycles.
  • SAPO Silico-aluminophosphate
  • A1PO Aluminophosphate
  • the present invention discloses a transition metal(s) loaded zeolite/zeolite-type SCR catalyst.
  • the performance of transition metal(s) loaded catalyst is attributed to the change in acidic nature of the zeolite/zeolite-type based SCR catalyst by (1) the choice of the method of preparation of the said catalyst, (2) coating of this material on honeycomb monolith and (3) post-treatment process.
  • the performance of the transition metal(s) loaded zeolite/zeolite-type SCR catalyst is attributed to (1) judicious selection of zeolite/zeolite-type material(s), (2) choice of transition metal(s) and their combinations, (3) metal doping/loading, (4) incorporating suitable binding agent(s) and (5) optionally, incorporating promoter(s).
  • the present invention discloses transition metal(s) loading on zeolite/zeolite-type materials and a method of manufacturing said metal(s) loaded zeolite/zeolite-type SCR catalyst.
  • It is a preferred embodiment to prepare the metal(s) loading by wet and instant dry method comprising the steps of: a) Preparing an aqueous solution containing metal(s) by mixing of water and metal salts under stirring,
  • step b) Adding slowly the zeolite/zeolite-type materials with simultaneous mixing to the solution of step a),
  • the DeNO x catalyst by preparing a slurry of metal(s) loaded zeolite/zeolite-type material, with a binder and optionally with a promoter; optionally coating said slurry on a honeycomb structure monolith, subjecting the said slurry for calcination and then having a post treatment step.
  • the post treatment is by heating slowly from ambient temperature to high temperature while passing air-moisture mixture through it, holding for a period at the desired high temperature in the presence of air- moisture mixture, and finally cooling to ambient temperature in the presence of air-moisture mixture to obtain the DeNO x catalyst with enhanced properties.
  • the transition metal(s) loaded zeolite/zeolite-type based SCR catalyst involves the use of microporous zeolite (aluminosilicates type) or zeolite-type (silico- aluminophosphates/aluminophosphates type) and loaded with Cu (copper) or Fe (Iron) or combinations thereof.
  • the Cu (copper) content in the transition metal(s) loaded zeolite/zeolite -type based SCR catalyst is in the range of 0.01 to 0.02 Mol %.
  • the Fe (Iron) content in the transition metal(s) loaded zeolite/zeolite-type based SCR catalyst is in the range of 0.003 to 0.005 mol %.
  • composition of the zeolite/zeolite-type in the transition metal(s) loaded zeolite based SCR catalyst is in the range of 45 to 95 wt%, preferably between 80% and 90%.
  • composition of a binder such as zirconium sol or silica sol or alumina sol or titania sol or their combinations thereof, in the transition metal(s) loaded zeolite/zeolite-type based SCR catalyst is in the range of 5 to 55 wt%, preferably between 10% and 20%.
  • promoters such as titania, zirconia, ceria-zirconia, silica, alumina, silica-alumina, alkaline and alkaline earth metals incorporated either individually or in combinations thereof, on the transition metal(s) loaded zeolite/zeolite-type based SCR catalyst, is in the range of 0.1 to 15 wt%.
  • the metal(s) loaded zeolite/zeolite-type based SCR catalyst is made by the process illustrated in the flow chart shown in Figure 1 and is described as below.
  • the said process includes a first step, in which an aqueous solution containing metal(s) is prepared by simple mixing of water and metal salts under stirring, a second step, in which, the zeolite/zeolite-type materials is added slowly with simultaneous mixing to the above solution, a third step, in which, the solution is stirred at elevated temperatures for few hours, a fourth step, in which, the solution is exposed suddenly at above water-evaporation temperatures until dryness, a fifth step, in which, the collected dried sample at ambient is re-heated in an oven again for few hours to remove any occluded water molecules and/or volatile components, a final step, in which, the sample is calcined for few hours and cooled naturally.
  • the slurry mixture includes a first slurry of the above described metal(s) loaded zeolite/zeolite-type materials and water and a second slurry of a suitable binder and water, optionally, a promoter.
  • the two slurries are mixed together.
  • the mixed slurry has a solid concentration of 10 to 45% and a viscosity (cP) ⁇ 2500.
  • the particle size distribution of the slurry D50 (pm) ranges between 1.5 to 7.5 pm, preferably in the range of 2.0 pm to 4.5 pm.
  • the pH of the slurry is maintained in between 2.5 to 6.5, preferably 3.0 to 4.0.
  • the slurry is coated on a honeycomb monolith structure.
  • the honeycomb monolith structure can be ceramic or metallic.
  • the ceramic substrates may be either a flow-through type or a wall-flow filter type.
  • the slurry or the coated honeycomb is subjected to calcination for 4 to 10 hours with the temperature ranging between 400°C-600°C.
  • transition metal(s) loaded zeolite/zeolite-type based SCR catalyst (coated on honeycomb monolith) is placed inside a furnace and heated up to designated temperatures. An air stream containing 4.5 to 15% of moisture content is forced through the furnace with heating, holding and cooling steps.
  • transition metal(s) loaded zeolite/zeolite-type based SCR catalyst after air- moisture mixture post-treatment process exhibit enhanced NO x conversion efficiency even at low temperatures as compared to transition metal loaded zeolite/zeolite-type based SCR catalyst without the air-moisture mixture posttreatment process.
  • NFb-TPD results exhibit an improvement of 12 - 17% in the ammonia adsorption capacity after air-moisture mixture post-treatment process.
  • the NFb-TPD profile ( Figure 3) also exhibits the presence of stronger acid sites after air-moisture mixture post-treatment process at the high temperature range of 300 - 500°C is attributed to the formation of strong acid sites either from the healed defective ones or masked ones or both. These acid sites where later identified to be the come from tetrahedral A1 sites (attributed to Br0nsted acid type) by Al 27 MAS NMR technique.
  • Surface area is an indicator of the available area on the support material on which the incoming feed gas can diffuse and react with the active sites therein. Once post-treated, the surface area of the transition metal(s) zeolite/zeolite-type found to be enhanced by 10 - 12 %. This is again could be attributed to healing of defect sites.
  • Solid state Al 27 MAS NMR studies on transition metal(s) loaded zeolite/zeolite- type based SCR catalyst before and after air-moisture mixture post-treatment process were recorded.
  • the NMR profile clearly, exhibits enhanced tetrahedral Al (AfrO species (chemical shift 54 ppm) after post-treatment process in comparison to the one before by more than 3/2 fold, while the octahedral Al (A ⁇ td) species (chemical shift 0-10 ppm) as well as pentahedral Al (Afr) species (chemical shift 18 ppm) are reduced after post-treatment process.
  • Copper containing zeolite/zeolite-type materials were prepared by wet and instant dry method.
  • An aqueous solution of copper salt containing 0.015 mol of Cu was prepared by simple mixing of water and copper salt with stirring for 15 minutes.
  • a defined amount of zeolite or zeolite- type powder samples were added slowly for 30 minutes with simultaneous mixing.
  • This solution was stirred at elevated temperatures of 70°C to 80°C for 5 to 6 hours and then exposed suddenly to temperatures >1 10°C.
  • the solution was stirred at elevated temperature of 75°C for preferably 5.5 hours prior to the sudden exposure to preferable temperatures of 190°C.
  • Iron/Copper containing zeolite/zeolite-type materials were prepared by the wet and instant dry method.
  • the CuZ-1 was prepared by the same procedure as mentioned in the Example 1.
  • the calcined and finely grounded CuZ powder sample of defined amount was added slowly for 30 minutes with simultaneous mixing into an aqueous solution of iron salt containing 0.004 mol of Fe which was pre-prepared by simple mixing of water and Iron salt with stirring for 15 minutes.
  • This solution was stirred at elevated temperatures such as 70°C to 80°C for 5 to 6 hours and then exposed suddenly to temperatures >1 10°C.
  • the solution was stirred at elevated temperature of 75°C for preferably 5.5 hours prior to the sudden exposure to preferable temperatures of 190°C.
  • Iron containing zeolites/zeolite-type materials were prepared by the wet and instant dry method.
  • An aqueous solution of iron salt containing 0.004 mol of Fe was prepared by simple mixing water and of Iron salt and stirred for 15 minutes.
  • defined amount of zeolite/zeolite-type powders were added slowly for 30 minutes with simultaneous mixing.
  • This solution was stirred at elevated temperatures of 70°C to 80°C for 5 to 6 hours and then exposed suddenly to temperatures >1 10°C.
  • the solution was stirred at elevated temperature of 75°C for preferably 5.5 hours prior to the sudden exposure to preferable temperatures of 190°C.
  • Iron/Copper containing zeolite/zeolite-type materials were prepared by wet and instant dry method.
  • the FeZ was prepared by the same procedure as mentioned in the Example 2.
  • the calcined and finely grounded FeZ zeolite/zeolite-type powder sample of defined amount was added slowly for 30 minutes with simultaneous mixing into an aqueous solution containing of copper salt containing 0.015 mol of Cu which was pre-prepared by simple mixing of water and copper salt with stirring for 15 minutes.
  • This solution was stirred at elevated temperatures such as 70°C to 80°C for 5 to 6 hours and then exposed to temperatures >1 10°C.
  • the solution was stirred at elevated temperature of 75°C for preferably 5.5 hours prior to the sudden exposure to preferable temperatures of 190°C.
  • the prepared CuZ containing zeolite/zeolite-type powder samples were re-slurried with water and suitable binder under controlled pH conditions. This slurry was stirred vigorously for 3 to 5 hours (preferably 4 hours) and coated on ceramic honeycomb monolith having 400 cpsi cell density and 4 mil wall thickness. The coated ceramic honeycomb was post-treated as discussed elsewhere.
  • Figure 6A discloses the transient 7 mode test results of NO x conversion efficiency before and after post-treatment process over CuZ.
  • the results in Table 4 were obtained at varying temperature, space velocities and feed gas concentrations for each mode.
  • Figure 6B discloses the results of selective NO reduction efficiency of before and after post-treatment process over CuZ catalyst.
  • Figure 6C discloses the results of NO2 reduction efficiency before and after posttreatment process over CuZ catalyst.
  • the post-treated catalyst was treated at 200°C for 20 hours in S0 2 environment and then regenerated by heating to 650°C.
  • the catalyst was tested, as mentioned in Example 6, before and after each sulphur aging cycles and also after each regeneration cycle for a total 3 cycles.
  • Figure 7A and Figure 7B discloses the results of steady state three cycles of NOx conversion after sulphur aging for post-treated CuZ catalyst and its subsequent regeneration of the same as mentioned in Example 8.
  • Table 5 discloses that the NOx conversion drops for each of the three cycles of sulphur aging catalysts. Furthermore, Table 5 also discloses that the NOx conversion restored back to its initial conversion after regeneration for each sulfur aged catalysts.

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

Abstract

L'invention concerne un catalyseur dénox revêtu sur un monolithe en nid d'abeilles comprenant un type zéolite/zéolite de type à structure CHA préchargé avec un ou des métaux de transition avec des performances améliorées. Le catalyseur est soumis à un processus de post-traitement pour obtenir les performances améliorées. Le catalyseur ainsi traité est caractérisé en utilisant XRD, NH3-TPD, surface et A127 MAS RMN et présente une activité à basse température améliorée et une stabilité thermique élevée en raison de la modification de l'acidité de surface et de l'augmentation des sites A1 de cadres tétraédriques catalytiquement actifs.
PCT/IN2020/050046 2019-01-16 2020-01-16 Catalyseur dénox à basse température et durable et son procédé de préparation WO2020148784A1 (fr)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112807936A (zh) * 2020-12-25 2021-05-18 锦科绿色科技(苏州)有限公司 沸石转轮自动生产线与沸石涂层制备方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6706660B2 (en) * 2001-12-18 2004-03-16 Caterpillar Inc Metal/metal oxide doped oxide catalysts having high deNOx selectivity for lean NOx exhaust aftertreatment systems
US8865120B2 (en) * 2010-12-11 2014-10-21 Umicore Ag & Co., Kg Process for the production of metal doped zeolites and zeotypes and application of same to the catalytic remediation of nitrogen oxides

Patent Citations (2)

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US6706660B2 (en) * 2001-12-18 2004-03-16 Caterpillar Inc Metal/metal oxide doped oxide catalysts having high deNOx selectivity for lean NOx exhaust aftertreatment systems
US8865120B2 (en) * 2010-12-11 2014-10-21 Umicore Ag & Co., Kg Process for the production of metal doped zeolites and zeotypes and application of same to the catalytic remediation of nitrogen oxides

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I.M. SAAID, A.R. MOHAMED AND S.BHATIA: "CATALYTIC ACTIVITY OF ZSM-5 ZEOLITE LOADED WITH TRANSITION METALS FOR THE SELECTIVE CATALYTIC REDUCTION OF NOx", AJSTD, vol. 19, no. 2, 2002, pages 15 - 31, XP055727334, DOI: 10.29037/ajstd.335 *
J.A.Z. PIETERSE ET AL.: "Evaluation of Fe-zeolite catalysts prepared by different methods for the decomposition of N2O", APPLIED CATALYSIS B: ENVIRONMENTAL, vol. 51, 24 April 2004 (2004-04-24), pages 215 - 228, XP002330137, DOI: 10.1016/j.apcatb.2004.02.013 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112807936A (zh) * 2020-12-25 2021-05-18 锦科绿色科技(苏州)有限公司 沸石转轮自动生产线与沸石涂层制备方法
CN112807936B (zh) * 2020-12-25 2023-02-10 锦科绿色科技(苏州)有限公司 沸石转轮自动生产线与沸石涂层制备方法

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