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`5/23/2016
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`WO2014161860A1 Google Patents
`
`WO2014161860A1 Google Patents
`
`Application number
`PCT/EP2014/056537
`
`Other languages
`German
`
`French
`
`Priority date
`20130405
`
`Filing date
`20140401
`
`Publication date
`20141009
`
`translated from German
`Cucha material for the SCR catalysis
`
`Description
`
`The present invention is directed to a catalyst material which is at elevated temperatures in a position to
`transform the nitrogen oxides in the exhaust gas of particular vehicles, which are driven with leanburn
`internal combustion engines in the presence of ammonia into harmless nitrogen.
`
`The exhaust gas of leanburn internal combustion engines, including diesel engines, in addition to
`resulting from incomplete combustion of fuel pollutant gases carbon monoxide (CO) and hydrocarbon
`(HC) and particulate matter (PM) and
` oxides (NOx). In addition, the exhaust gas of diesel engines
`nitrogen
`contains up to 15% by volume oxygen. It is known that the oxidizable harmful gases CO and HC by
`passing it over a suitable oxidation catalyst in carbon dioxide (CO2) and water and converted particles
`by passing the exhaust gas can be removed by a suitable tes particulate filter.
`
`A known method for removing nitrogen oxides from oxygencontaining (lean) exhaust gases (SCR drive
`supply; Selective Catalytic Reduction), the method of selective catalytic reduction with ammonia over a
`suitable catalyst, the SCR catalyst. In this method, to remove nitrogen oxides from the exhaust gas with
`ammonia are converted to nitrogen and water. The ammonia used as a reducing agent can be used as
`secondary emission in Sauerstoffbzw. Oxidantpoor (rich) operating phases are generated in the
`exhaust system desolate it is metered a precursor compound, may be formed from ammonia, such as
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`urea, ammonium carbamate or ammonium formate, made available in the exhaust line, optionally
`followed by hydrolysis.
`
`The use of zeolitebased SCR catalysts is known from numerous publications. For example, US 4,961,
`917 a method for the reduction of nitrogen oxides with ammonia using a catalyst which contains a zeolite
`having defined properties iron and / or copper as a promoter. Other SCR catalysts based on transition
`metalexchanged zeolites and processes for the selective catalytic reduction using such SCR catalysts
`are described for example in EP 1 495 804 A1, US 6,914,026 B2 and EP 1 147 801 B1.
`
`Even in the WO 9427709, catalysts based on zeolites with the Chabazitstruktur (CHA) proposed for the
`decomposition of nitrous oxide. Was also mentioned that these can be replaced with copper. The
`replacement rate is preferably 25 wt .% given as the metal based on the total weight of the catalyst. As
`a ratio of silica to alumina is demanded that this should take at least a value of 55 bar.
`
`In the US 6,709,644 B2 the preparation of zeolites of Chabazittyps is Chen discussed. It is stated that
`these zeolites in particular for the reduction of
`
`Nitrogen oxides can be used and can have silica to alumina ratios which are in excess of 10. It is further
`stated that the zeolite may contain a metal ion which enables to can perform the reduction of nitrogen
`oxides in the presence of an excess of oxygen. As typical techniques by which the ion exchange can be
`carried out in the zeolite, wet industrial processes are called, which also acetates of the corresponding
`metal ions can be used.
`
`To prepare copperexchanged zeolites, various methods are further described in the literature. These
`include ion exchange, for example in aqueous solution (US 5,171, 553, DE 10 2010 007 626 A1), and
`solidstate ion exchange method (DE 10 2006 033 451 A1, DE 10 2006 033 452 A1 and references cited
`therein).
`
`Furthermore, WO 2008132452 A2 reports on the use of copperexchanged zeolite of the Chabazittyps
`in the reduction of nitrogen oxides. The specified here NEN silica to alumina ratios of the zeolites used
`are in the range of 2300 or preferably 8150. There is presented a copperexchanged zeolite of the
`Chabazittyps containing 3 wt .% copper.
`
`WO 2008106519 A1 also describes copper exchanged zeolites for use in the reduction of nitrogen
`oxides. In the present materials are propagated, which are to have a SAR of more than 15 and a copper
`to aluminum ratio of greater than 0.25. The targeted zeolites are preferably prepared by the ion
`exchange with kupferacetathaltigen solutions. The authors of WO 20081 18434 A1 describe in this
`document copper Exchanged Chabazittypen which firstly rel. high Siliziumdioxidgehalte (SAR> 15) and,
`secondly, at least one weight percent copper based exhibit on the total weight of the catalytically active
`material. It is described that such materials available have a very good stability to hydrothermal aging.
`
`In WO 2012075400 A1 zeolitic aluminosilicates are highlighted, which are derived from Chabazittyp. The
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`assignee of this invention promote appropriate zeolites for the reduction of nitrogen oxides, in which the
`materials are to contain a relatively low content of wrestling promoters, such as copper. Likewise, the
`authors show that especially those zeolites having a large average crystal size and a relatively low silica
`to alumina ratio (SAR) are preferable. The specified contents of copper are below 0.24 (Cu: Al content)
`and the SAR is between 10 and 25. The average surface crystal size is specified μηη with greater than
`0.5.
`
`In the PhD thesis of Dustin W. Fickel, in 2010 created at the University of Delaware / USA, various
`copperexchanged zeolites are described in terms of quality and in the reduction of nitrogen oxides.
`There are highly exchanged zeolites Cucha (SAR = 12; Cu: AI = 0.35) with those with less Cu content
`(SAR = 12; Cu: AI = 0.29) compared (Figure 5.5.).
`
`CA2822788 AA describes the Cuchazeolites as catalysts for the reduction of nitrogen oxide. It SAR
`levels of 1 1 are here 14.8 proposed as being particularly preferred. The crystal sizes of the catalyst
`material are with 18 indicated μηη. The Cu: Al ratio is preferably 0,2 0,4. The zeolites described here
`are all crystallized using additions of alkali metal ions.
`
`Object of the present invention, it was nevertheless to provide an ionexchanged zeolite material based
`on the Chabazitstruktur, which is able to transform into a more advantageous manner nitrogen oxides in
`the presence of ammonia into harmless nitrogen. These and other objects which will become apparent
`to those skilled in an obvious way from the prior art are solved by the use of a material which has the
`characterizing features of the present claim. 1 From claim 1 dependent subclaims relate to preferred
`embodiments of the present invention. Furthermore, the present invention is directed to a catalyst, an
`appropriate catalyst system and a preferred use of the zeolite according to the invention.
`
`Characterized that one comprising a zeolite material Cucha:
`
`i) a molar
`
` 2: AI 03 ratio (SAR) of> 10 to <15;
`2
`
`Si0
`
`ii) Cu: AI ratios of> 0.25 to <0.35, and
`
`iii) an average crystal size from 0.75 to 2 μηη. indicates, but you get extremely beneficial for not less
`surprising for solving the problem posed above. This material is in this combination of features, even
`after hydrothermal aging at 850 ° C for 6 hours in the presence of 10% water excellent stabilities and
`activities (Fig. 1). In particular, it is surprising that the activity in the low temperature range of 200 ° C
`with just under 60% is relatively high. This was so not derivable from the available prior art without
`further ado.
`
`A parameter that further affect the stability of the inventive material, is the socalled crystal size. It has
`proven to be advantageous if the average crystal size is above 0.75 μηη. This should advantageously
`also be the case if the material has been aged at above conditions hydrothermally. According to the
`invention possess the crystals have an average size from 0.75 to 2 μηη. More preferred is an average
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`size of the crystals from 0.8 to 1, 5 μηη. Most preferably, the average size of the crystals obtained is a
`value of 0.8 1. 2 μηη. If the crystal modification obtained may be such that different lengths of axes
`forming the crystals, so the above values can be seen on the shortest of the axes of the crystals formed.
`The determination of the crystal size by means of SEM (WO2009141324; http: //www.iza
`onIine.org/syrithesisA S_2ndEd / SEM.htm;
`
`http://portaI.tugraz.at/portaI/page/portaI/feImi/research/Scanning%20EIectron scopy / Principles% 20of%
`20SEM). As an average value, the sum of the measured crystal sizes is shown based on the number of
`crystals. The present invention shows that it is for the formation of corresponding favorable Cucha
`zeolite be vital that the ratio of silica to alumina on the one hand and its relationship to the and / or on
`the zeolite existing copper crucial for the activity and hydrothermal stability and good lowtemperature
`activity of the material according to the invention at low Is O generation is. Therefore is particularly
`advantageous, the fact that the proposed CuCHA here zeolite has a SAR value of 12, 13 and 14
`respectively. A value of 12 or 13 is highly preferred to choose. With respect to these values, the loading
`of the material with copper ions should be done in such a way that a Cucha zeolite material is formed,
`which preferably has a Cu: AI has ratio of> 0.25 to <0.31. Most preferably, the molar SiO therefore is ^ A
`Os ratio (SAR) value of 12, 13 or 14 with a Cu: Al ratio of> 0.26 to <0.31, preferably> 0.28 to <0 , 31 and
`very particularly preferably to 0.29. This material is Zugen beyond measure to preferred when an
`average crystal size of 0.75 μηη 2, preferably 0.8 1, 5 μηι, extremely preferably 0.8 1, 2 μηη has.
`
`The issues raised here Cuchazeolite materials are produced such as a rule that first the zeolite is
`obtained, which is brought into the sequence by wet process technology with copper ions into contact.
`An ion exchange can be carried out analogously to the WO2012175409. It is advantageous if the copper
`is imported exclusively by wet ion exchange technology in the finished zeolite. Such methods are well
`known to the skilled person.
`
`It has proved to be advantageous if the zeolite material is thereby synthesized in its H
`+ form.
`Advantageously, the ion exchange are connected with copper followed immediately, without in the
`meantime carried out an additional ion exchange, for example in the form NHV. The H
` contained in
`+ ions
`zeolite exchanged with copper ions their seats. Alternatively, however, only a NH4
` go from
`+ exchange
`Equip. In addition to the synthesis in
` H + form, ie without going through possibly. Crystallization with
`the
`alkali metal ions and subsequent ion exchange with NHV ions, the synthesis of zeolites has proven right
`in the NHVform favorable. In particular, therefore, is also preferred that zeolites without the addition of
`alkali metal ions, particularly sodium ions to crystallize in the presence of NHV ions, which leads directly
`to the NHVform of the zeolite, and subsequently to convert the copper exchange in the
` + form. The
`H
`content of Alkalimetallio NEN, in particular sodium ions in zeolite is present at less than 100 ppm even
`without further ion exchange.
`
`Preferably solutions of copper ions are used in water for copper exchange. It is preferred that the copper
`is present in dissolved form of a salt in water. Particularly preferred is the fact that the anion of the
`Kupfersal indices from the residue of an organic acid. As preferably used organic acids in this
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`connection are in particular acetic acid, formic acid, tartaric acid or oxalic acid is used. The use of acetic
`acid in this context is especially preferred. Al203 ratio (SAR) of 12, 13 or 14 with a Cu: therefore a Cucha
`material, which has a molar Si02 is highly preferred AI ratio> 0.26 to <0.31, preferably> 0.28 to <0.31
`and most preferably 0.29 and, where it has a crystal size of 0.75 μηι 2, preferably 0.8 1, 5 μηι,
`extremely preferably 0.8 1, 2 and by having μηη ion exchange with an aqueous solution of copper or
`copper in an initial concentration of 0.2 M to 0.8 M, preferably> 0.25M has been received to <0.6M. Most
`preferably, the concentration of copper salt in the solution is about 0.5 M.
`
`As already indicated, the product thus produced and appropriately dimensioned has an extremely good
`hydrothermal stability. These hydrothermal stability can be measured by temperaturedependent XRD
`recordings (Finkel et al., J. Chem. Phys. 2010 1 14, 1633ff.). The [100] Reflex can be used for this
`purpose. It has been shown that the present material only above a temperature of 800 ° C begins to
`lose its stability, which can be seen in the decrease in the intensity of this reflex. Accordingly, it is
`particularly preferred if the stability of the material according to the invention only above 800 ° C,
`preferably above 810 ° C and a period of more preferably above 820 ° C and most preferably above 830
`° C (as measured by the relative intensity of [100] peaks (XRD)) begins to wane (decrease [100] Reflex
`by 10% within 1 h). This is particularly preferred for the aforementioned, and particularly preferably
`employed material of the case. The present invention is also a catalyst, which the
`
`Catalyzes reduction of nitrogen oxides in the presence of ammonia and comprising material of the
`invention. The catalyst may contain in addition to the material according to the invention also other
`materials such as binders, and other excipients may be applied as a washcoat on support bodies,
`wherein the supporting bodies advantageously socalled flow monolith or wall flow monolith is.
`Reference is made in this regard to the relevant mentioned in the introduction of this application
`literature.
`
`In particular, is also a subject of the present invention, a catalyst system which also includes a mate al
`next to the Cucha zeolite material according to the invention, which is capable of oxidizing ammonia in
`the presence of oxygen. It has proven to be favorable at the downstream end of the catalyst of the
`invention to provide a corresponding oxidising material to oxidize optionally unreacted ammonia to
`nitrogen as possible. Preference is therefore given to an arrangement in which the inventive material is
`present together with a catalyst for ammonia oxidation on a carrier body, wherein most preferably the
`oxidizing material is attached to the downstream end of the supporting body. Here, a system layout can
`be selected, which provides a zoned arrangement of both materials on the supporting body, the
`materials either on impact, with a gap or wholly or partially overlapping on the support body may be
`present. It is in this regard also refer to the literature described at the outset.
`
`The present invention is also the use of the material according to the invention in a catalytic converter
`for reducing nitrogen oxides with ammonia. With respect to further embodiments, as regards the use,
`reference is made to the aforementioned literature.
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`In the context of the present invention is understood to be the substance group of zeolites following
`class of compounds:
`
`M
`
` x / [(Α10
`n +
`n
`
`
`2)
`
`"χ
`
`
`
`(Si0
`
` 2)
`
`y]
`
` z H2O
`■
`
`• The factor n is the charge of the cation M and usually is 1 or 2.
`
`• M is typically an alkali or alkaline earth metal cation of a. These cations are required for electrical
`charge balance the negatively charged aluminum tetrahedron and not incorporated into the main grid of
`the crystal, but will stay in cavities of the grid and are therefore easily within the grid moveable and
`interchangeable in retrospect.
`
`• The factor z indicates how many water molecules are absorbed by the crystal. Zeolites can absorb
`water and other low molecular weight substances and release when heated again without their crystal
`structure is destroyed.
`
`• The molar ratio of S1O2 to AIO2 and y / x in the empirical formula is referred to as a module. It may be
`due to the Lowenstein rule not less than 1. The contemplated herein are zeolites of the structural class
`of Chabazite (CHA) assigned. Only the pure zeolites are the framework atoms other than aluminum,
`silicon and oxygen encompassed include without such. According to the invention therefore contain
`zeolites presented no further elements in their structure. Located on the ion exchange sites primarily
`copper ions and the
`
`Cations that have been used for the preparation of the zeolite. In particular, the content of phosphorus in
`the material according to the invention less than 100 ppm. Also, the content of residual carbon is present
`in the claimed Cucha at less than 500, preferably less than 200 and most preferably less than 100 ppm.
`This is particularly characterized become possible that the preparation of the corresponding zeolite is
`carried out without the use of a carboncontaining material.
`
`Such Cucha catalysts have little in nitrous oxide production (high selectivity) for superior nitric oxide
`reduction ability, in particular the lowtemperature activity with respect to the nitrogen oxide reduction is
`excellent. This was not to be expected in light of the known prior art.
`
`Example:
`
`The Cuchazeolite used is produced analogously to US 6,709,644, WO 2012145323 A1 or WO 201
`1073390 A2. Subsequently, the exchanged with copper material is applied on the support body, dried
`and calcined. Cores of the supporting body are hydrothermally aged at 850 ° C for 6 h and at 10% H2O.
`
`The samples thus obtained are at a space velocity of 80,000 / h in the synthesis gas (500 ppm NO, 500
`ppm NH
` H 2 0, 10% 0 7.5% C0
` 350 ppm CO, balance N2) in respect of their NOx conversion
`3, 5%
`2
`2,
`investigated (Fig. 1 and Fig. 2). It shows that average SAR ratios of> 10 to <15 coupled with Cu: AI
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`ratios of> 0.25 to <0.35 give them the best results.
`
`+ form,
`
` and then converted into the H
`
`Claims (1)
`translated from German
`1. Claims
`Cucha zeolite material comprising:
`i) a molar
` 2: AI 03 ratio (SAR) of> 10 to <15;
`2
`Si0
`ii) Cu: AI ratios of> 0.25 to <0.35, and
`iii) an average crystal size from 0.75 to 2 μηη.
`2 Cuchazeolite according to claim 1,
`characterized in that
`the molar SiC ^ A Os ratio (SAR) 12, 13 or 14 is.
`3 Cucha zeolite material according to one or more of claims 1 2,
`characterized in that
`the Cu: AI ratio> 0.25 to <0.31.
`4. Cucha zeolite material according to one or more of claims 1 3,
`characterized in that
`the molar SiC ^ A Os ratio (SAR) 12, 13 and 14, and the Cu: AI ratio
`> 0.26 is up <0.31.
`5. Cucha zeolite material according to one or more of claims 1 4,
`characterized in that
`Cu that has been used in the form of a salt with the anion of an organic acid to the ion exchange. 6.
`Cucha zeolite material according to one or more of claims 1 5,
`characterized in that
`its stability only above 800 ° C (as measured by the relative intensity of the [100] peaks (XRD))
`begins to wane.
`7. catalyst for catalytic reduction of nitrogen oxides in the presence of ammonia comprising the
`material according to claim 1 to 6.
`8. A catalyst system comprising the catalyst according to claim 7,
`characterized in that
`it is present together with a catalyst for ammonia oxidation on a carrier body.
`9. Use of a material according to one or more of the preceding claims 1 7 in a catalyst for reducing
`nitrogen oxides with ammonia.
`10. A process for the preparation of the zeolite material Cucha according to one or more of claims 1
`6,
`characterized in that
`synthesizing the CHA zeolite material in the NH4
`copper is exchanged.
`
`+ form,
`
` before the
`
`Patent Citations (5)
`
`https://patents.google.com/patent/WO2014161860A1/en
`
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`
`Publication
`number
`
`Priority
`date
`
`WO2014161860A1 Google Patents
`Publication
`date
`
`Assignee
`
`Title
`
`WO2008106519A1
`*
`
`2007
`0227
`
`20080904
`
`Basf
`Catalysts
`Llc
`
`Copper cha zeolite catalysts
`
`WO2011073398A2
`*
`
`2009
`1218
`
`20110623
`
`Basf
`Corporation
`
`WO2012086753A1
`*
`
`2010
`1222
`
`20120628
`
`Tosoh
`Corporation
`
`Process of direct copper exchange into
`na+form of chabazite molecular sieve,
`and catalysts, systems and methods
`
`Chabazite type zeolite and process for
`production thereof, coppercarrying low
`silica zeolite, nox reductive elimination
`catalyst including said zeolite, and
`method for reductive elimination of nox
`employing said catalyst
`
`WO2012145323A1
`*
`
`2011
`0418
`
`20121026
`
`Pq
`Corporation
`
`Large crystal, organicfree chabazite,
`methods of making and using the same
`
`WO2013064887A2
`*
`
`2011
`1102
`
`20130510
`
`Johnson
`Matthey
`Public
`Limited
`Company
`
`Catalyzed filter for treating exhaust gas
`
`* Cited by examiner, † Cited by third party
`NonPatent Citations (1)
`Title DUSTIN W FICKEL ET AL: "The ammonia selective catalytic reduction activity of copperexchanged
`smallpore zeolites", APPLIED CATALYSIS B: ENVIRONMENTAL, ELSEVIER, AMSTERDAM, NL, Bd.
`102, Nr. 3, 9. Dezember 2010 (20101209), Seiten 441448, XP028139896, ISSN: 09263373, DOI:
`10.1016/J.APCATB.2010.12.022 [gefunden am 20101216] *
`* Cited by examiner, † Cited by third party
`Also Published As
`
`Publication number Publication date
`
`Type
`
`US20160038875A1
`
`20160211
`
`Application
`
`DE102013005749A1
`
`20141009
`
`Application
`
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`Nitrogenoxidestorage catalytic converter and process for its
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`https://patents.google.com/patent/WO2014161860A1/en
`
`9/10
`
`Exhibit 1121
`IPR2015-1125
`UMICORE AG & CO. KG
`Page 28 of 29
`
`
`
`5/23/2016
`
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`WO2014161860A1 Google Patents
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`20061207 Catalyst for catalytic reduction of nitrogen oxide
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`10/10
`
`Exhibit 1121
`IPR2015-1125
`UMICORE AG & CO. KG
`Page 29 of 29