WO2013060341A1 - Composition de catalyseur s'utilisant dans la réduction catalytique sélective d'oxydes d'azote - Google Patents
Composition de catalyseur s'utilisant dans la réduction catalytique sélective d'oxydes d'azote Download PDFInfo
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- WO2013060341A1 WO2013060341A1 PCT/EP2011/005344 EP2011005344W WO2013060341A1 WO 2013060341 A1 WO2013060341 A1 WO 2013060341A1 EP 2011005344 W EP2011005344 W EP 2011005344W WO 2013060341 A1 WO2013060341 A1 WO 2013060341A1
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- zeolite
- catalyst composition
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Classifications
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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
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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
- B01J23/72—Copper
-
- 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
- B01D53/944—Simultaneously removing carbon monoxide, hydrocarbons or carbon making use of oxidation catalysts
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
-
- 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/7007—Zeolite Beta
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- 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
- B01D2251/2062—Ammonia
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- 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
- B01D2255/2065—Cerium
-
- 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
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- 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
- B01D2255/20—Metals or compounds thereof
- B01D2255/209—Other metals
- B01D2255/2092—Aluminium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/40—Mixed oxides
- B01D2255/407—Zr-Ce mixed oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/50—Zeolites
- B01D2255/502—Beta 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, optionally promoted with copper or iron
- the problem to be solved by this invention is to provide a catalyst composition and method for the reduction of nitrogen oxides with a DeNO x activity at reaction temperatures between 150 and 550°C.
- the catalyst composition and method of this invention shall further include soot and hydrocarbon oxidation activity simultaneously with the DeNOx activity.
- the invention provides in its broadest embodiment a catalyst composition for selective reduction of nitrogen
- the catalyst composition comprises a physical mixture of one or more acidic zeolite or zeotype components and one ore more redox active metal compounds.
- catalyst compositions comprising one or more zeolite or zeotype components from the group of BEA, MFI , FAU, FER, CHA, MOR in protonic form or promoted with Fe and redox metal component (Cu/Al 2 0 3( ⁇ / ⁇ 2 0 3 , Ce0 2 -Zr0 2 , Ce- n/Al 2 0 3 ) exhibit a pronounced synergistic effect.
- DeNO x activity of such composite catalysts significantly exceeds activity of their individual components.
- the redox component can additionally provide good soot oxidation function which can be used in combined SCR/DPF systems.
- a preferred catalyst composition for selective reduction of nitrogen oxides and soot oxidation comprises one or more acidic zeolite or zeotype components and one or more redox active metal compounds wherein the one or more acidic zeolite or zeotype components are selected from the group consisting of BEA, MFI, FAU, FER, CHA, MOR or mixtures thereof.
- the acidic zeolite or zeotype component can be used in protonic form or promoted with Fe and one or more redox active metal components are selected form the group consisting of Cu/Al203, Mn/Al203, Ce02-Zr02, Ce- Mn/Al203 and mixtures thereof.
- redox active metal compounds as used herein relates 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 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 A1 2 0 3 , Ti0 2 , Si0 2 , Ce0 2 , Zr0 2 or mixtures thereof.
- the mean molar ratio Si/Al of the zeolite components according to the invention is from 5 to 100.
- Catalyst compositions prepared by mechanical mixing of the above mentioned zeolite and redox metal components exhibit a pronounced synergistic effect. DeNO x activity of such composite catalysts significantly exceeds activity of their individual components.
- the one or more redox active metal components are physically mixed with the one or more zeolite components or dispersed on surface of the zeolite components.
- the one or more redox active metal components dispersed on the surface of the one or more zeolite or zeotype components contain Ce, Mn, and Zr, Cr or mixtures thereof.
- the above described catalyst composition according to the invention can be utilised as coating material or being coated on structured bodies of metallic, ceramic, metal oxide, SiC or silica materials or fibres.
- the invention further provides 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 metallic, ceramic, metal oxide, SiC or silica fiber materials .
- 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 component in the composite catalyst can be significantly re- prised by its replacement with equivalent volume of redox component.
- overall volume of the catalyst remains 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 r eact ⁇ 250°C is observed despite decreased amount of zeolite component.
- the invention provides additionally a method for the selective 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 composition comprising a physical mixture of one or more acidic zeolite or zeotype components and one ore more redox active metal compounds .
- the acidic zeolite or zeotype components are selected from the group consisting of BEA, MFI, FAU, FER, CHA, MOR or mix- tures thereof and the one or more redox active metal components are selected form 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.
- 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 Al 2 0 3/ Ti0 2 , Si0 2/ Zr0 2 or mixtures thereof.
- the one or more redox active metal components are physically mixed with the one or more zeolite components or dispersed on surface of the zeolite components.
- the one ore more redox active metal components are dispersed on the surface of the one or more zeolite components contain Ce, Mn, and Zr, Cr or mixtures thereof.
- the catalyst composition is contacted with the off-gas at a tem- perature below 250°C.
- the powders 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. Similarly 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 -DeN0x in the temperature 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.
- ⁇ 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.
- Fe-Beta Fe-Beta zeolite
- 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 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 temperature range of 150-550 °C. The test was performed under following 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.
- a first sample was prepared by mixing 74wt%Ce0 2 -26wt%ZrC>2 and Fe-Beta powders at a weight ratio of 3.3. In this case volume ratio of 74wt% Ce0 2 - 26wt% Zr0 2 /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%Ce0 2 -26wt%Zr0 2 and Fe-Beta zeolite components equals 5/1.
- a third sample was prepared by was prepared by mixing 74wt%Ce0 2 -26wt%Zr0 2 and Fe-Beta zeolite powders at a weight ratio of 30.
- For the second sample volume ratio of 74wt%Ce0 2 -26wt%Zr0 2 and Fe-Beta zeolite components equals 10/1. After grinding in agate mortar for 10-15 min, the resulted mixtures were pelletized. The pellets were crushed and sieved collecting 0.2 - 0.4 mm fraction for catalytic test. Similarly pelletized Fe-Beta zeolite was used as reference. Activities of the prepared samples were tested using the following catalyst loading which kept constant volume of the catalyst in the reactor. In all experiments described below overall volume on the catalyst loaded was 0.067 ml, which results in GHSW ⁇ 270 000 h "1 :
- Second sample [0.109g 74wt%Ce0 2 - 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 temperature range of 150-550 °C . The test was performed under following 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.
- Catalyst load 0.04g Fe-Beta and
- Three samples of [10wt%Cu/Al 2 O 3 + H-zeolite] composite catalyst were prepared by thorough grinding of 10wt%Cu/Al 2 O 3 and H-Beta, H-ZSM-5, or H-ferrierite powder.
- 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 catalysts were tested in NH 3 -DeNO x within the temperature range of 150-550 °C. The test was performed under following 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.
- Profiles of soot oxidation over [Ce0 2 -Zr0 2 + Fe-Beta] and Fe-Beta are displayed in Figure 7.
- [Ce0 2 -Zr0 2 + Fe-Beta] significantly higher activity in soot oxidation then individual Fe-Beta, as evidenced by a shift of soot oxidation maximum from ⁇ 600°C for (Fe- Beta + soot) to ⁇ 420°C for ( [Ce0 2 -Zr0 2 + Fe-Beta] + soot)
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Abstract
L'invention concerne une composition de catalyseur et un procédé de réduction sélective d'oxydes d'azote et d'oxydation de la suie. On fait passer un gaz d'échappement à épurer, avec de l'ammoniac ou un composé décomposable en ammoniac, sur un catalyseur qui comprend un mélange de zéolithe acide et d'un composant d'oxydo-réduction.
Priority Applications (14)
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 |
MX2014004494A MX2014004494A (es) | 2011-10-24 | 2011-10-24 | Composicion de catalizador y metodo para el uso en la reduccion catalitica selectiva de oxidos de nitrogeno. |
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 |
RU2014120917A RU2608616C2 (ru) | 2011-10-24 | 2012-05-02 | Каталитическая композиция и способ применения в селективном каталитическом восстановлении оксидов азота |
IN2950CHN2014 IN2014CN02950A (fr) | 2011-10-24 | 2012-05-02 | |
AU2012327482A AU2012327482A1 (en) | 2011-10-24 | 2012-05-02 | Catalyst composition and method for use in selective catalytic reduction of nitrogen oxides |
BR112014008669-9A BR112014008669B1 (pt) | 2011-10-24 | 2012-05-02 | Composição de catalisador e método para utilização em reduções catalíticas de óxidos de nitrogênio |
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 |
KR1020147013999A KR101789114B1 (ko) | 2011-10-24 | 2012-05-02 | 질소 산화물의 선택적 촉매 환원에서 사용하기 위한 촉매 조성물 및 방법 |
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 |
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 |
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 |
US14/353,620 US9168517B2 (en) | 2011-10-24 | 2012-05-02 | Catalyst composition and method for use in selective catalytic reduction of nitrogen oxides |
CL2014000993A CL2014000993A1 (es) | 2011-10-24 | 2014-04-17 | Composicion de catalizador para la reduccion selectiva de oxidos de nitrogeno y la oxidacion de hollin, que comrpende uno o mas compuestos de zeolita o zeotipo acidos, mezclados fisicamente con uno o mas compuestos de metales con actividad de redox; cuerpo estructurado monolitico; y metodo para la reduccion selectiva |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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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 |
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WO2013060341A1 true WO2013060341A1 (fr) | 2013-05-02 |
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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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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 |
Country Status (11)
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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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US11427693B2 (en) | 2016-06-08 | 2022-08-30 | Blueshft Materials, Inc. | Polymer aerogel with improved mechanical and thermal properties |
WO2018029329A1 (fr) | 2016-08-11 | 2018-02-15 | Umicore Ag & Co. Kg | Matériau actif scr présentant une stabilité thermique élevée |
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US10799831B2 (en) | 2016-08-11 | 2020-10-13 | Umicore Ag & Co. Kg | SCR-active material |
EP3281698A1 (fr) | 2016-08-11 | 2018-02-14 | Umicore AG & Co. KG | Materiau scr actif |
US11873379B2 (en) | 2017-12-05 | 2024-01-16 | Blueshift Materials, Inc. | Thermally treated polyamic amide aerogel |
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WO2019141718A1 (fr) | 2018-01-16 | 2019-07-25 | Umicore Ag & Co. Kg | Procédé de fabrication d'un catalyseur scr par préséchage |
US11230955B2 (en) | 2018-01-16 | 2022-01-25 | Umicore Ag & Co. Kg | Method for producing an SCR catalytic converter by way of pre-drying |
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EP3791955A1 (fr) | 2019-09-10 | 2021-03-17 | Umicore Ag & Co. Kg | Matériau catalytique scr contenant une zéolite au cuivre et cuivre/alumine, procédé de traitement de gaz d'échappement avec ce matériau et procédé de fabrication de ce matériau |
CN110586176B (zh) * | 2019-09-27 | 2020-11-17 | 中国环境科学研究院 | 一种电解锰渣基微介孔zsm-5催化剂及制备方法 |
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Also Published As
Publication number | Publication date |
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CA2853154A1 (fr) | 2013-05-02 |
RU2014120917A (ru) | 2015-12-10 |
JP6112734B2 (ja) | 2017-04-12 |
CN103889569A (zh) | 2014-06-25 |
KR20140095512A (ko) | 2014-08-01 |
BR112014008669A2 (pt) | 2017-04-18 |
KR101789114B1 (ko) | 2017-10-23 |
CL2014000993A1 (es) | 2014-08-22 |
AU2012327482A1 (en) | 2014-05-15 |
BR112014008669B1 (pt) | 2019-07-02 |
WO2013060487A1 (fr) | 2013-05-02 |
IN2014CN02950A (fr) | 2015-07-03 |
MX2014004494A (es) | 2014-07-11 |
CA2853154C (fr) | 2018-04-03 |
RU2608616C2 (ru) | 2017-01-23 |
JP2015501210A (ja) | 2015-01-15 |
CN103889569B (zh) | 2017-02-15 |
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