WO2012156503A1 - Niedertemperatur-oxidationskatalysator mit besonders ausgeprägten hydrophoben eigenschaften für die oxidation organischer schadstoffe - Google Patents
Niedertemperatur-oxidationskatalysator mit besonders ausgeprägten hydrophoben eigenschaften für die oxidation organischer schadstoffe Download PDFInfo
- Publication number
- WO2012156503A1 WO2012156503A1 PCT/EP2012/059243 EP2012059243W WO2012156503A1 WO 2012156503 A1 WO2012156503 A1 WO 2012156503A1 EP 2012059243 W EP2012059243 W EP 2012059243W WO 2012156503 A1 WO2012156503 A1 WO 2012156503A1
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- WIPO (PCT)
- Prior art keywords
- catalyst
- noble metal
- zeolite material
- catalyst according
- zeolite
- Prior art date
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- 239000003054 catalyst Substances 0.000 title claims abstract description 81
- 230000003647 oxidation Effects 0.000 title claims abstract description 14
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 14
- 239000002957 persistent organic pollutant Substances 0.000 title description 5
- 230000002209 hydrophobic effect Effects 0.000 title description 2
- 239000010457 zeolite Substances 0.000 claims abstract description 56
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 40
- 239000011148 porous material Substances 0.000 claims abstract description 19
- 239000011230 binding agent Substances 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 22
- 229910021536 Zeolite Inorganic materials 0.000 claims description 15
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 15
- 239000010970 precious metal Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 11
- 239000002923 metal particle Substances 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 150000002736 metal compounds Chemical class 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052762 osmium Inorganic materials 0.000 claims description 2
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 241000264877 Hippospongia communis Species 0.000 description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- 239000000243 solution Substances 0.000 description 14
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 12
- 239000007789 gas Substances 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- 238000000576 coating method Methods 0.000 description 11
- 239000011248 coating agent Substances 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000005470 impregnation Methods 0.000 description 8
- 238000011068 loading method Methods 0.000 description 8
- 239000000725 suspension Substances 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000006260 foam Substances 0.000 description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 6
- 229910010271 silicon carbide Inorganic materials 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000012694 precious metal precursor Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 241000282326 Felis catus Species 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 229910001092 metal group alloy Inorganic materials 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000002459 porosimetry Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000012925 reference material Substances 0.000 description 2
- -1 structural type Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 229940082150 encore Drugs 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 150000004675 formic acid derivatives Chemical class 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000006262 metallic foam Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 150000003892 tartrate salts Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- 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
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- 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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- B01J29/068—Noble metals
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- B01J29/08—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
- B01J29/10—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y containing iron group metals, noble metals or copper
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- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
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- B01J29/18—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the mordenite type
- B01J29/20—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the mordenite type containing iron group metals, noble metals or copper
- B01J29/22—Noble metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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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- B01J29/50—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the erionite or offretite type, e.g. zeolite T, as exemplified by patent document US2950952
- B01J29/52—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the erionite or offretite type, e.g. zeolite T, as exemplified by patent document US2950952 containing iron group metals, noble metals or copper
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- B01J29/65—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the ferrierite type, e.g. types ZSM-21, ZSM-35 or ZSM-38, as exemplified by patent documents US4046859, US4016245 and US4046859, respectively
- B01J29/66—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the ferrierite type, e.g. types ZSM-21, ZSM-35 or ZSM-38, as exemplified by patent documents US4046859, US4016245 and US4046859, respectively containing iron group metals, noble metals or copper
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- B01J29/74—Noble metals
- B01J29/7423—MAZ-type, e.g. Mazzite, Omega, ZSM-4 or LZ-202
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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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- Exhaust Gas After Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201280024064.4A CN103534027B (zh) | 2011-05-18 | 2012-05-18 | 用于氧化有机污染物的具有特别显著的疏水性的低温氧化催化剂 |
JP2014510819A JP5789715B2 (ja) | 2011-05-18 | 2012-05-18 | 有機汚染物質の酸化のための疎水性を顕著に示す低温酸化触媒 |
US14/118,358 US20140186251A1 (en) | 2011-05-18 | 2012-05-18 | Low-temperature oxidation catalyst with particularly marked hydrophobic properties for the oxidation of organic pullutants |
EP12722719.7A EP2709756A1 (de) | 2011-05-18 | 2012-05-18 | Niedertemperatur-oxidationskatalysator mit besonders ausgeprägten hydrophoben eigenschaften für die oxidation organischer schadstoffe |
BR112013029541A BR112013029541A2 (pt) | 2011-05-18 | 2012-05-18 | catalisador de oxidação a baixa temperatura com propriedades hidrofóbicas para a oxidação dos poluentes orgânicos, método e uso |
US16/176,363 US20190060832A1 (en) | 2011-05-18 | 2018-10-31 | Low-Temperature Oxidation Catalyst With Particularly Marked Hydrophobic Properties For The Oxidation Of Organic Pollutants |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102011101877.1 | 2011-05-18 | ||
DE102011101877A DE102011101877A1 (de) | 2011-05-18 | 2011-05-18 | Niedertemperatur-Oxidationskatalysator mit besonders ausgeprägten hydrophoben Eigenschaften für die Oxidation organischer Schadstoffe |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US14/118,358 A-371-Of-International US20140186251A1 (en) | 2011-05-18 | 2012-05-18 | Low-temperature oxidation catalyst with particularly marked hydrophobic properties for the oxidation of organic pullutants |
US16/176,363 Division US20190060832A1 (en) | 2011-05-18 | 2018-10-31 | Low-Temperature Oxidation Catalyst With Particularly Marked Hydrophobic Properties For The Oxidation Of Organic Pollutants |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2012156503A1 true WO2012156503A1 (de) | 2012-11-22 |
Family
ID=46147441
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2012/059243 WO2012156503A1 (de) | 2011-05-18 | 2012-05-18 | Niedertemperatur-oxidationskatalysator mit besonders ausgeprägten hydrophoben eigenschaften für die oxidation organischer schadstoffe |
Country Status (7)
Country | Link |
---|---|
US (3) | US20140186251A1 (de) |
EP (1) | EP2709756A1 (de) |
JP (1) | JP5789715B2 (de) |
CN (1) | CN103534027B (de) |
BR (1) | BR112013029541A2 (de) |
DE (1) | DE102011101877A1 (de) |
WO (1) | WO2012156503A1 (de) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2015126732A (ja) * | 2013-12-27 | 2015-07-09 | プラスティックス インダストリー デベロップメント センター | 果物や野菜などの植物の熟成、腐敗速度を遅らせる材料及びその製造方法 |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE102014201263A1 (de) * | 2014-01-23 | 2015-07-23 | Johnson Matthey Catalysts (Germany) Gmbh | Katalysator |
CN107847865A (zh) | 2015-07-02 | 2018-03-27 | 庄信万丰股份有限公司 | 被动nox吸附剂 |
US11179707B2 (en) * | 2017-03-31 | 2021-11-23 | Johnson Matthey Catalysts (Germany) Gmbh | Composite material |
CN114206489A (zh) * | 2019-09-05 | 2022-03-18 | 三井金属矿业株式会社 | 废气净化用组合物及其制造方法 |
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US5250282A (en) | 1990-01-25 | 1993-10-05 | Mobil Oil Corp. | Use of amphiphilic compounds to produce novel classes of crystalline oxide materials |
JPH07136461A (ja) * | 1993-11-24 | 1995-05-30 | Agency Of Ind Science & Technol | 含酸素化合物、芳香族化合物及び酸素を含む混合ガスからの含酸素化合物の選択的除去方法 |
WO2000047309A1 (en) * | 1999-02-10 | 2000-08-17 | General Electric Company | Method of removing methanol from off gases |
DE102009015592A1 (de) * | 2009-03-30 | 2010-10-07 | Süd-Chemie AG | Alterungsstabiler Katalysator zur Oxidation von NO zu NO2 in Abgasströmen |
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US4560820A (en) * | 1981-04-13 | 1985-12-24 | Chevron Research Company | Alkylaromatic dealkylation |
US4906353A (en) * | 1987-11-27 | 1990-03-06 | Mobil Oil Corp. | Dual mode hydrocarbon conversion process |
DE19623609A1 (de) * | 1996-06-13 | 1997-12-18 | Basf Ag | Oxidationskatalysator und Verfahren zur Herstellung von Epoxiden aus Olefinen, Wasserstoff und Sauerstoff unter Verwendung des Oxidationskatalysators |
JP2000516248A (ja) * | 1996-08-20 | 2000-12-05 | ザ ダウ ケミカル カンパニー | アルキル化ベンゼンの製造方法 |
US6756029B2 (en) * | 1999-08-11 | 2004-06-29 | Petroleo Brasileiro S.A.-Petrobras | Molecular sieves of faujasite structure |
US7361797B2 (en) * | 2002-02-05 | 2008-04-22 | Abb Lummus Global Inc. | Hydrocarbon conversion using nanocrystalline zeolite Y |
US20080249340A1 (en) * | 2004-04-01 | 2008-10-09 | Siler Susan J | Hydro-Oxidation of Hydrocarbons Using a Catalyst Prepared by Microwave Heating |
ES2761656T3 (es) * | 2007-03-08 | 2020-05-20 | Praxair Technology Inc | Adsorbentes de alta velocidad y alta resistencia al aplastamiento |
US8969232B2 (en) * | 2007-05-24 | 2015-03-03 | Saudi Basic Industries Corporation | Catalyst for conversion of hydrocarbons, process of making and process of using thereof—incorporation 2 |
US8450232B2 (en) * | 2009-01-14 | 2013-05-28 | Lummus Technology Inc. | Catalysts useful for the alkylation of aromatic hydrocarbons |
-
2011
- 2011-05-18 DE DE102011101877A patent/DE102011101877A1/de not_active Withdrawn
-
2012
- 2012-05-18 BR BR112013029541A patent/BR112013029541A2/pt not_active IP Right Cessation
- 2012-05-18 WO PCT/EP2012/059243 patent/WO2012156503A1/de active Application Filing
- 2012-05-18 CN CN201280024064.4A patent/CN103534027B/zh not_active Expired - Fee Related
- 2012-05-18 JP JP2014510819A patent/JP5789715B2/ja not_active Expired - Fee Related
- 2012-05-18 US US14/118,358 patent/US20140186251A1/en not_active Abandoned
- 2012-05-18 EP EP12722719.7A patent/EP2709756A1/de not_active Withdrawn
-
2018
- 2018-10-31 US US16/176,363 patent/US20190060832A1/en not_active Abandoned
-
2019
- 2019-05-09 US US16/407,538 patent/US20190262771A1/en not_active Abandoned
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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US5250282A (en) | 1990-01-25 | 1993-10-05 | Mobil Oil Corp. | Use of amphiphilic compounds to produce novel classes of crystalline oxide materials |
JPH07136461A (ja) * | 1993-11-24 | 1995-05-30 | Agency Of Ind Science & Technol | 含酸素化合物、芳香族化合物及び酸素を含む混合ガスからの含酸素化合物の選択的除去方法 |
WO2000047309A1 (en) * | 1999-02-10 | 2000-08-17 | General Electric Company | Method of removing methanol from off gases |
DE102009015592A1 (de) * | 2009-03-30 | 2010-10-07 | Süd-Chemie AG | Alterungsstabiler Katalysator zur Oxidation von NO zu NO2 in Abgasströmen |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2015126732A (ja) * | 2013-12-27 | 2015-07-09 | プラスティックス インダストリー デベロップメント センター | 果物や野菜などの植物の熟成、腐敗速度を遅らせる材料及びその製造方法 |
Also Published As
Publication number | Publication date |
---|---|
JP5789715B2 (ja) | 2015-10-07 |
EP2709756A1 (de) | 2014-03-26 |
US20190060832A1 (en) | 2019-02-28 |
JP2014519970A (ja) | 2014-08-21 |
CN103534027B (zh) | 2017-03-15 |
DE102011101877A8 (de) | 2015-05-28 |
BR112013029541A2 (pt) | 2017-01-24 |
US20140186251A1 (en) | 2014-07-03 |
US20190262771A1 (en) | 2019-08-29 |
CN103534027A (zh) | 2014-01-22 |
DE102011101877A1 (de) | 2012-11-22 |
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