EP2709756A1 - Catalyseur d'oxydation à basse température possédant des propriétés hydrophobes particulièrement prononcées pour l'oxydation de polluants organiques - Google Patents

Catalyseur d'oxydation à basse température possédant des propriétés hydrophobes particulièrement prononcées pour l'oxydation de polluants organiques

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Publication number
EP2709756A1
EP2709756A1 EP12722719.7A EP12722719A EP2709756A1 EP 2709756 A1 EP2709756 A1 EP 2709756A1 EP 12722719 A EP12722719 A EP 12722719A EP 2709756 A1 EP2709756 A1 EP 2709756A1
Authority
EP
European Patent Office
Prior art keywords
catalyst
noble metal
zeolite material
catalyst according
zeolite
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP12722719.7A
Other languages
German (de)
English (en)
Inventor
Arno Tissler
Frank Klose
Roderik Althoff
Mika ENDLER
Patrick Müller
Grigory Reznikov
Margit Schuschke
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Clariant Produkte Deutschland GmbH
Original Assignee
Clariant Produkte Deutschland GmbH
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 Clariant Produkte Deutschland GmbH filed Critical Clariant Produkte Deutschland GmbH
Publication of EP2709756A1 publication Critical patent/EP2709756A1/fr
Withdrawn legal-status Critical Current

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    • 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
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8678—Removing components of undefined structure
    • B01D53/8687—Organic components
    • 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
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B01J29/064—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof containing iron group metals, noble metals or copper
    • B01J29/068—Noble metals
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    • B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
    • B01J29/42—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing iron group metals, noble metals or copper
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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
    • B01J29/82—Phosphates
    • B01J29/84—Aluminophosphates containing other elements, e.g. metals, boron
    • B01J29/85—Silicoaluminophosphates [SAPO compounds]
    • 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
    • B01J29/87—Gallosilicates; Aluminogallosilicates; Galloborosilicates
    • 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
    • B01J29/89—Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium

Definitions

  • the present invention relates to a catalyst comprising a microporous noble metal-containing zeolite material and a porous SiC> 2-containing binder, wherein the catalyst has a proportion of micropores of more than 70%, based on the
  • the invention also relates to a process for the preparation of the catalyst and the use of the catalyst as
  • TWC three-way catalysts
  • the exhaust gases of diesel engines are treated with catalysts.
  • Hydrocarbons to be catalytically treated include paraffins, olefins, aldehydes and aromatics.
  • Contaminants are generally sensitive to water vapor. Water vapor blocks the active sites on the catalyst surface so that their activity decreases. This is usually due to higher precious metal doping levels
  • the object of the present invention was therefore to provide a catalyst which has a high activity in the oxidation of organic pollutants at low temperatures, for example below 300 ° C., has high activity in the oxidation of organic pollutants, in particular solvent-type pollutants, even under high water vapor concentrations, which also shows a low tendency to thermal sintering and beyond manages with significantly lower Edelmetalldot michsgrade.
  • the object of the present invention was therefore to provide a catalyst which has a high activity in the oxidation of organic pollutants at low
  • the object is achieved by a catalyst comprising a microporous noble metal-containing zeolite material and a porous SiC> 2-containing binder, wherein the catalyst has a proportion of micropores of more than 70%, based on the
  • catalysts which comprise a microporous precious metal-containing zeolite material and a pure SiC> 2 binder which has little meso and macropores have significantly higher activity, in particular in the oxidation of solvent-like air pollutants.
  • the catalyst preferably has a content of micropores of more than 70%, more preferably more than 80%, most preferably more than 90%, based on the total pore volume of the catalyst.
  • Catalyst is the proportion of micropores> 72%, more preferably> 76%, based on the total pore volume of
  • the catalyst characterized by a microporous content> 70% and a meso and macroporous fraction between 20 and 30%.
  • the proportion of the micropores is preferably ⁇ 100%, more preferably ⁇ 95%.
  • the catalyst according to the invention is therefore a catalyst having a polymodal pore distribution, that is to say it contains both micropores, mesopores and macropores.
  • pores are to be understood as meaning micropores, mesopores and macropores
  • the determination of the micro and meso / macroporous fraction is carried out by means of the so-called T-plot method according to ASTM D-4365-85.
  • the integral pore volume of the catalyst is more than 100 mm 3 / g, more preferably more than 180 mm 3 / g.
  • the determination of the integral pore volume is preferably carried out in accordance with DIN ISO 9277 by means of nitrogen porosimetry or alternatively with noble gas porosimetry. It is preferred according to an embodiment of the catalyst that the zeolite material has an aluminum content of ⁇ 2 mol .-%, more preferably ⁇ 1 mol .-%, based on the
  • Binder component contains no significant amounts of aluminum.
  • the binder contains less than 0.04 wt%, more preferably less than 0.02 wt%, of aluminum, based on the amount of binder.
  • Suitable binders are, for example, Ludox AS 40 or tetraethoxysilane having an Al 2 O 3 content of ⁇ 0.04 wt .-%.
  • the zeolite material is 0.5 to 6.0 wt%, more preferably 0.6 to 5.0 wt%, even more preferably 0.7 to 4.0 wt%. % and particularly preferably 0.5 to ⁇ 3.0 wt.% Precious metal, based on the amount of zeolite material.
  • the washcoat has a noble metal loading of 0.1 to 2.0 g / l, more preferably 0.4 to 1.5 g / l, even more
  • the noble metal is preferably selected from the group
  • the precious metals can be present both in the form of noble metal particles and in the form of noble metal oxide particles.
  • the following is mainly spoken of noble metal particles, which, however, also includes Edelmetalloxidp micro, unless expressly stated otherwise.
  • the particle size of the noble metal particles preferably has an average diameter of 0.5 to 5 nanometers, more preferably a mean diameter of 0.5 to 3 nanometers, and particularly preferably a mean diameter of 0.5 to 2 nanometers.
  • the determination of the particle size can
  • the noble metal particles of the loaded zeolite material are as small as possible, since the particles then have a very high degree of dispersion.
  • the degree of dispersion the ratio of the number of metal atoms, which is the surface of the metal particles form, understood to the total number of metal atoms of the metal particles.
  • a favorable average particle diameter also depends on the application in which the catalyst is to be used and on the nature of the noble metal of the noble metal particles, the pore distribution and in particular the pore radii and channel radii of the zeolite material.
  • the noble metal particles are preferably located in the inner pore system of the zeolite. These are understood according to the invention as the micropores, meso- and macropores of the zeolite. Preferably, the noble metal particles are (im
  • Zeolite material can be both a zeolite and a
  • Zeolite materials are silicates, aluminosilicates,
  • zeolite material is used, on the one hand, depends on the nature of the precious metal, which
  • zeolite materials such as structural type, pore diameter, channel diameter, chemical composition, ion exchange capability, and activation properties to a particular application.
  • zeolite materials which are one of the
  • the zeolite materials mentioned can be present both in the sodium form and in the ammonium form or in the H form. Also preferred according to the invention are those
  • Zeolite materials prepared using amphiphilic compounds are mentioned in US 5,250,282 and are incorporated by reference into the present invention.
  • the catalyst as
  • An unsupported catalyst may be, for example
  • molded body for example, a monolith.
  • shaped bodies are, for example, spheres, rings, cylinders, perforated cylinders, trilobes or cones, particular preference being given to a monolith, for example a monolithic honeycomb body.
  • Catalyst is applied to a support body, that is present as a coating catalyst.
  • a support body that is present as a coating catalyst.
  • it may be in the support body, for example, an open-cell foam structure, for example, a metal foam, a metal alloy foam, a silicon carbide foam, an Al20 3 foam, a
  • Mullite foam an Al titanate foam, as well as a
  • monolithic support structure for example, has parallel aligned channels, which may be interconnected with each other or may contain certain installations for gas turbulence.
  • supporting bodies are formed, for example, from a metal sheet, from any desired metal or metal alloy, which comprises a metal foil or sintered metal foil or a metal foil Metal fabric and are produced for example by extrusion, winding or stacking.
  • support bodies of ceramic material can be used.
  • the ceramic material is an inert, low surface material such as cordierite, mullite, alpha-alumina, silicon carbide or aluminum titanate.
  • the inserted support body also made
  • the weight ratio is zeolite material / binder 80/20 to 60/40, more preferably 75/25 to 65/35, and most preferably about 70/30.
  • the BET surface area of the catalyst of the present invention is preferably in the range of 10 to 600 m 2 / g, more preferably 50 to 500 m 2 / g, and most preferably 100 to 450 m 2 / g.
  • the BET surface area is determined by adsorption of nitrogen in accordance with DIN 66132.
  • the invention further provides a method for
  • Preparation of the catalyst according to the invention comprising the following steps: a) introducing a noble metal precursor compound into a micropore zeolite material; b) calcining the zeolite material loaded with the noble metal precursor compound; c) mixing the loaded with the noble metal compound
  • Zeolite material with a porous Si0 2 ⁇ containing binder and a solvent d) drying and calcining the mixture comprising the noble metal compound-loaded zeolite material and the binder.
  • the washcoat obtained in step c) can be applied to a carrier body before drying and calcination to form a coating catalyst.
  • the precious metal of the zeolite is either as
  • Precious metal in metallic form or as Edelmetalloxid ago If a metallic form of the noble metal is necessary, as a further method step, the conversion of the metal of the noble metal compound, with which the zeolite material is loaded, in its metallic form.
  • the conversion of the noble metal compound into the corresponding noble metal is usually carried out by thermal decomposition or by reduction by means of hydrogen, carbon monoxide or wet chemical
  • Reducing agent The reduction can also be done in situ when starting a catalytic reaction in a reactor.
  • the introduction of the noble metal compound is carried out by
  • Zeolite material with the noble metal precursor compound forms the basis for that in the following
  • Precious metal precursor compound leads, or at
  • Precious metal particles is loaded.
  • the impregnation of the zeolite material is carried out according to the incipient wetness method known to the person skilled in the art.
  • Precious metal precursor compound for example, nitrates, acetates, oxalates, tartrates, formates, amines, sulfides,
  • Precious metals are used.
  • Precious metal precursor compound is subjected to calcination, preferably at a temperature of 200 to 800 ° C, more preferably 300 to 700 ° C, most preferably 500 to 600 ° C.
  • the calcination is inventively preferred
  • Protective gas for example nitrogen or argon, preferably carried out argon.
  • the invention further relates to the use of the catalyst of the invention as an oxidation catalyst, in particular as a catalyst for the oxidation of organic
  • FIG. 1 shows the performance of the invention
  • the ratio of zeolite to binder was 70/30.
  • a BEA-150 is thus impregnated with 1.85% Pt.
  • the Pt (NO 3 ) 2 solution has to be diluted once more with 1008, 65 g of water.
  • Washcoat type Pt-BEA-150
  • Carrier material ceramic substrates, lOOcpsi
  • the particle size distribution of the zeolite powder was measured in the physical analysis.
  • the experiment was carried out according to a standard procedure.
  • Batch tank was a 5 liter beaker.
  • the zeolite powder was suspended in deionized water and the pH was measured. (pH: 2.62).
  • the Bindzil was added to the suspension and the pH was measured. (pH: 2.41).
  • the suspension was then with an Ultra-Turax stirrer for about 10 min. dispersed. From the suspension, a sample was taken and the
  • the washcoat was further stirred on a magnetic stirrer and used for coating.
  • the washcoat was diluted with 15% deionized water. The solids content after dilution was 13.62%. For the coating, the washcoat was stirred until no sediment was present and measured. For this, the carrier was completely immersed in the washcoat container and moved until no more bubbles formed (time: about 30 seconds). Subsequently, the carrier was taken out and blown with a compressed air nozzle from both sides evenly to about half of the target load. The carrier became at 150 ° C overnight
  • Washcoat type Pt-BEA-150
  • Table 1 Coating results The catalysts according to the invention were examined by means of the T-plot method for their micro- and meso / macropores content and the values were evaluated in m 2 / g (see Table 2).
  • a ceramic honeycomb was coated with 50 g / l of a washcoat consisting of 80% by weight of T1O 2 and 20% by weight of Al 2 O 3 .
  • the aqueous TiO 2 / Al 2 C> 3 suspension was initially stirred up vigorously.
  • the ceramic honeycomb was then immersed in the washcoat suspension.
  • Non-adherent washcoat was removed after dipping by blowing out the honeycomb channels.
  • the honeycomb body was dried at 120 ° C and calcined at 550 ° C for 3 h.
  • the noble metal deposition was accomplished by immersing the washcoat-coated catalyst honeycomb in a solution of Pt and Pd nitrate. After impregnation, the honeycomb was again blown out, dried at 120 ° C for 2 h and calcined at 550 ° C for 3 h.
  • a ceramic honeycomb was coated with 100 g / l of a washcoat consisting of Al 2 O 3 .
  • a washcoat consisting of Al 2 O 3 .
  • the aqueous Al 2 ⁇ 0 3 suspension was initially stirred up vigorously.
  • the ceramic honeycomb was then immersed in the washcoat suspension.
  • Non-adherent washcoat was removed after dipping by blowing out the honeycomb channels.
  • the honeycomb body was dried at 120 ° C and calcined at 550 ° C for 3 h.
  • the noble metal was applied by two impregnation steps with intermediate drying and calcination. In the first step, the washcoated honeycomb was impregnated by immersion in a solution of Pt sulphite.
  • the honeycomb was blown out, dried at 120 ° C for 2 h and calcined at 550 ° C for 3 h.
  • the honeycomb was impregnated by immersion with a solution of tetramine-Pd nitrate. It was then blown out again, dried at 120 ° C for 2 h and calcined at 550 ° C for 3 h.
  • Comparative Example 3 A dried H-BEA-35 with an acidic Pt (NC> 3) 2 _ solution by means of "Incipent wetness” method applied. To this was added 48.5 g of H-BEA-35 with 47.1 g of a 3.2 wt .-% Pt-containing Pt (NO 3 ) 2 solution impregnated
  • Impregnation the material was dried at 120 ° C overnight and then calcined under argon. The calcination was carried out at 550 ° C for 5 hours, the heating rate before was 2 K / min.
  • the final Pt-BEA-35 powder contained 3 wt% Pt.
  • the powdered Pt-BEA material was then coated with a corderite catalyst honeycomb.
  • a corderite catalyst honeycomb 33.3 g of Pt-BEA material, 57 g of H-BEA 35 and 29.4 g of binder (binder material, 34 wt .-% S1O 2 containing) dispersed in 300 g of water and then in a planetary ball mill at 350 U / min for 30 min in 5-minute intervals to a washcoat milled.
  • the suspension was transferred in each case to a plastic bottle in order to use the corderite honeycomb (200 cpsi) to coat.
  • the coating amount achieved was 100 g / 1 W / C.
  • the honeycomb was calcined for 5 hours at 550 ° C.
  • the performance of the catalyst of the invention was determined in the oxidation of 180 ppmv of ethyl acetate in air at a GHSV of 40,000 h _1 and compared to the conventional reference materials. The results are shown in FIG. 1 (data in Tables 4 to 7). In the case of Comparative Example 3, the performance data were scaled to a comparable effective honeycomb surface, the points> 90% conversion being omitted.
  • Figure 2 shows the sales comparison at a temperature of 225 ° C, plotted against the

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  • Chemical & Material Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
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  • General Chemical & Material Sciences (AREA)
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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Exhaust Gas After Treatment (AREA)

Abstract

L'invention concerne un catalyseur comprenant un matériau de zéolite microporeux contenant un métal précieux et un liant poreux contenant du SiO2, le catalyseur comprenant une proportion de micropores supérieure à 70 %, rapporté au volume total des pores du catalyseur. L'invention concerne en outre un procédé pour la préparation du catalyseur ainsi que l'utilisation du catalyseur en tant que catalyseur d'oxydation.
EP12722719.7A 2011-05-18 2012-05-18 Catalyseur d'oxydation à basse température possédant des propriétés hydrophobes particulièrement prononcées pour l'oxydation de polluants organiques Withdrawn EP2709756A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102011101877A DE102011101877A1 (de) 2011-05-18 2011-05-18 Niedertemperatur-Oxidationskatalysator mit besonders ausgeprägten hydrophoben Eigenschaften für die Oxidation organischer Schadstoffe
PCT/EP2012/059243 WO2012156503A1 (fr) 2011-05-18 2012-05-18 Catalyseur d'oxydation à basse température possédant des propriétés hydrophobes particulièrement prononcées pour l'oxydation de polluants organiques

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US (3) US20140186251A1 (fr)
EP (1) EP2709756A1 (fr)
JP (1) JP5789715B2 (fr)
CN (1) CN103534027B (fr)
BR (1) BR112013029541A2 (fr)
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WO (1) WO2012156503A1 (fr)

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TWI481498B (zh) * 2013-12-27 2015-04-21 Plastics Industry Dev Ct 蔬果保鮮材料及其製造方法
DE102014201263A1 (de) * 2014-01-23 2015-07-23 Johnson Matthey Catalysts (Germany) Gmbh Katalysator
GB2544839B (en) * 2015-07-02 2019-01-16 Johnson Matthey Plc Passive NOx Adsorber
US11179707B2 (en) * 2017-03-31 2021-11-23 Johnson Matthey Catalysts (Germany) Gmbh Composite material
US20220258123A1 (en) * 2019-09-05 2022-08-18 Mitsui Mining & Smelting Co., Ltd. Exhaust gas purifying composition and production method therefor

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DE102011101877A1 (de) 2012-11-22
JP5789715B2 (ja) 2015-10-07
CN103534027B (zh) 2017-03-15
DE102011101877A8 (de) 2015-05-28
JP2014519970A (ja) 2014-08-21
WO2012156503A1 (fr) 2012-11-22
US20140186251A1 (en) 2014-07-03
CN103534027A (zh) 2014-01-22
BR112013029541A2 (pt) 2017-01-24
US20190060832A1 (en) 2019-02-28
US20190262771A1 (en) 2019-08-29

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