JP2016195992A - 遷移金属/ゼオライトscr触媒 - Google Patents
遷移金属/ゼオライトscr触媒 Download PDFInfo
- Publication number
- JP2016195992A JP2016195992A JP2016076435A JP2016076435A JP2016195992A JP 2016195992 A JP2016195992 A JP 2016195992A JP 2016076435 A JP2016076435 A JP 2016076435A JP 2016076435 A JP2016076435 A JP 2016076435A JP 2016195992 A JP2016195992 A JP 2016195992A
- Authority
- JP
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- Prior art keywords
- zeolite
- catalyst
- nitrogen
- transition metal
- exhaust gas
- 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.)
- Granted
Links
- 239000010457 zeolite Substances 0.000 title claims abstract description 256
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 226
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 198
- 239000003054 catalyst Substances 0.000 title claims abstract description 181
- 229910052723 transition metal Inorganic materials 0.000 title claims description 73
- 150000003624 transition metals Chemical class 0.000 title claims description 73
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims abstract description 77
- 239000007789 gas Substances 0.000 claims abstract description 73
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 62
- 238000000034 method Methods 0.000 claims abstract description 62
- 239000000463 material Substances 0.000 claims abstract description 36
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 32
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 31
- 229910000323 aluminium silicate Inorganic materials 0.000 claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 24
- 239000002184 metal Substances 0.000 claims abstract description 24
- 229910052742 iron Inorganic materials 0.000 claims abstract description 18
- 229910052802 copper Inorganic materials 0.000 claims abstract description 14
- 238000002485 combustion reaction Methods 0.000 claims abstract description 13
- GHOKWGTUZJEAQD-ZETCQYMHSA-N (D)-(+)-Pantothenic acid Chemical compound OCC(C)(C)[C@@H](O)C(=O)NCCC(O)=O GHOKWGTUZJEAQD-ZETCQYMHSA-N 0.000 claims abstract 2
- 239000011148 porous material Substances 0.000 claims description 94
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 54
- 229910052676 chabazite Inorganic materials 0.000 claims description 41
- UNYSKUBLZGJSLV-UHFFFAOYSA-L calcium;1,3,5,2,4,6$l^{2}-trioxadisilaluminane 2,4-dioxide;dihydroxide;hexahydrate Chemical compound O.O.O.O.O.O.[OH-].[OH-].[Ca+2].O=[Si]1O[Al]O[Si](=O)O1.O=[Si]1O[Al]O[Si](=O)O1 UNYSKUBLZGJSLV-UHFFFAOYSA-L 0.000 claims description 39
- 230000003647 oxidation Effects 0.000 claims description 24
- 238000007254 oxidation reaction Methods 0.000 claims description 24
- 239000000758 substrate Substances 0.000 claims description 24
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 23
- 229910021529 ammonia Inorganic materials 0.000 claims description 19
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 13
- 229910052675 erionite Inorganic materials 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052697 platinum Inorganic materials 0.000 claims description 12
- 230000009467 reduction Effects 0.000 claims description 12
- 229910052763 palladium Inorganic materials 0.000 claims description 10
- 229910052684 Cerium Inorganic materials 0.000 claims description 9
- 229910052748 manganese Inorganic materials 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 229910052804 chromium Inorganic materials 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 7
- 229910052703 rhodium Inorganic materials 0.000 claims description 7
- 238000011144 upstream manufacturing Methods 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 150000002739 metals Chemical class 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 229910052738 indium Inorganic materials 0.000 claims description 5
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- 239000000446 fuel Substances 0.000 claims description 4
- 229910052741 iridium Inorganic materials 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 229910052702 rhenium Inorganic materials 0.000 claims description 4
- 229910052707 ruthenium Inorganic materials 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 claims description 4
- MGWGWNFMUOTEHG-UHFFFAOYSA-N 4-(3,5-dimethylphenyl)-1,3-thiazol-2-amine Chemical compound CC1=CC(C)=CC(C=2N=C(N)SC=2)=C1 MGWGWNFMUOTEHG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 239000003502 gasoline Substances 0.000 claims description 3
- 239000003949 liquefied natural gas Substances 0.000 claims description 3
- 239000003915 liquefied petroleum gas Substances 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- BVCZEBOGSOYJJT-UHFFFAOYSA-N ammonium carbamate Chemical compound [NH4+].NC([O-])=O BVCZEBOGSOYJJT-UHFFFAOYSA-N 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052785 arsenic Inorganic materials 0.000 claims description 2
- 229910052790 beryllium Inorganic materials 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- KXDHJXZQYSOELW-UHFFFAOYSA-N carbonic acid monoamide Natural products NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 230000004044 response Effects 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 229910017119 AlPO Inorganic materials 0.000 claims 1
- 241000269350 Anura Species 0.000 claims 1
- 239000010949 copper Substances 0.000 abstract description 115
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 63
- -1 MER Chemical compound 0.000 abstract description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 3
- 238000001125 extrusion Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 43
- 238000006243 chemical reaction Methods 0.000 description 32
- 229910002089 NOx Inorganic materials 0.000 description 30
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 25
- 229930195733 hydrocarbon Natural products 0.000 description 19
- 150000002430 hydrocarbons Chemical class 0.000 description 19
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 14
- 230000015572 biosynthetic process Effects 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 230000032683 aging Effects 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 239000004215 Carbon black (E152) Substances 0.000 description 10
- 238000006722 reduction reaction Methods 0.000 description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 7
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000002253 acid Substances 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 6
- 238000010531 catalytic reduction reaction Methods 0.000 description 6
- 239000000571 coke Substances 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 239000011651 chromium Substances 0.000 description 5
- 239000011572 manganese Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000002808 molecular sieve Substances 0.000 description 5
- 229910052680 mordenite Inorganic materials 0.000 description 5
- 239000010948 rhodium Substances 0.000 description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- QQONPFPTGQHPMA-UHFFFAOYSA-N Propene Chemical compound CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 229910052728 basic metal Inorganic materials 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000000875 corresponding effect Effects 0.000 description 4
- 229910001657 ferrierite group Inorganic materials 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 3
- PFEOZHBOMNWTJB-UHFFFAOYSA-N 3-methylpentane Chemical compound CCC(C)CC PFEOZHBOMNWTJB-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 230000010757 Reduction Activity Effects 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 238000012993 chemical processing Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000010944 silver (metal) Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 1
- GMVPRGQOIOIIMI-DODZYUBVSA-N 7-[(1R,2R,3R)-3-hydroxy-2-[(3S)-3-hydroxyoct-1-enyl]-5-oxocyclopentyl]heptanoic acid Chemical compound CCCCC[C@H](O)C=C[C@H]1[C@H](O)CC(=O)[C@@H]1CCCCCCC(O)=O GMVPRGQOIOIIMI-DODZYUBVSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound 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
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000013626 chemical specie Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012013 faujasite Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910001683 gmelinite Inorganic materials 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
- B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
- B01D53/56—Nitrogen oxides
-
- 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
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
- B01D53/56—Nitrogen oxides
- B01D53/565—Nitrogen oxides by treating the gases with solids
-
- 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
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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Abstract
Description
(i)蒸気処理及び酸または錯化剤、例えば(EDTA-エチレンジアミンテトラ酢酸)を使用する酸抽出、酸及び/または錯化剤による処理、SiCl4の気体流による処理(ゼオライト骨格中のAlをSiで置き換える)による脱アルミニウム化、
(ii)陽イオン交換−例えばLa等の多価陽イオンの使用、及び
(iii)リン含有化合物の使用(例えば米国特許第5,958,818号参照)
が挙げられる。
市販のベータゼオライト、SAPO−34またはSSZ-13、をNH4NO3溶液中でNH4+イオン交換し、次いで濾過した。得られた材料をFe(NO3) 3の水溶液に攪拌しながら加えた。このスラリーを濾過し、次いで洗浄し、乾燥させた。この手順を繰り返し、所望の金属装填量を達成することができる。最終的な生成物をか焼した。
市販のSAPO−34、SSZ-13、シグマ-1、ZSM-34、Nu-3、ZSM-5及びベータゼオライトをNH4NO3溶液中でNH4+イオン交換し、次いで濾過した。得られた材料をCu(NO3) 2の水溶液に攪拌しながら加えた。このスラリーを濾過し、次いで洗浄し、乾燥させた。この手順を繰り返し、所望の金属装填量を達成することができる。最終的な生成物をか焼した。
例1及び2で得た触媒を、750℃で24時間、4.5%H2O/空気混合物中でリーン水熱的エージングした。
例1及び2で得た触媒を、900℃で1時間、4.5%H2O/空気混合物中で過酷なリーン水熱的エージングした。
例1及び2で得た触媒を、900℃で3時間、4.5%H2O/空気混合物中で過酷なリーン水熱的エージングした。
例1により製造したFe/ベータベータ及び例2により製造したCu/ベータベータ、Cu/ZSM-5及びCu/SAPO-34の個別試料を、例3及び4によりエージングし、実験室装置で、下記のガス混合物、すなわち350 ppmNO、350 ppmNH3、14%O2、4.5%H2O、4.5%CO2、残部N2を使用して試験した。結果を図1〜図4に示す。
実験室装置に装填した触媒で、1000 ppm(C1当量として)プロペン、n−オクタンまたはトルエンを、300℃におけるSCR(350 ppmNO、350 ppmNH3、12%O2、4.5%H2O、4.5%CO2、残部N2)の際に注入した。炭化水素脱着は、12%O2、4.5%H2O、4.5%CO2、残部N2中で温度を10℃/分で上昇させることにより、測定した。
図1は、穏やかなエージング後の、Cu/SAPO−34のNOx還元効率を、一連のアルミノケイ酸塩ゼオライトが担持された遷移金属触媒(Cu/ZSM-5、Cu/ベータ及びFe/ベータ)に対して比較する。この結果は、Cu/SAPO−34が、NH3によるNOxのSCRに対して改良された低温活性を有することを明らかに立証している。
図5で、小細孔ゼオライトSAPO−34及びNu-3上に担持された新しい(すなわちエージングしていない)CuのNH3SCR活性を、大細孔ゼオライト上に担持されたCuの活性と比較した。過酷なリーン水熱条件下でエージングした同じ触媒の対応する活性を図6に示す。新しい、及びエージングした活性プロファイルの比較により、水熱安定性は、Cuが小細孔ゼオライト上に担持された場合のアルミノケイ酸塩ゼオライトでのみ達成されることが立証される。
例2により製造したCu/SSZ-13、Cu/SAPO−34、Cu/シグマ-1及びCu/ベータを、例4に記載する様式でエージングし、例6により試験した。これらの結果を図13に示すが、そこから、過酷なリーン水熱エージングしたCu/SSZ-13、Cu/SAPO−34及びCu/シグマ-1試料のそれぞれのNOx転化活性が、対応する大細孔ゼオライト、Cu/ベータの活性より著しく優れていることが分かる。さらに、図14から、Cu/ベータは、Cu/小細孔ゼオライト触媒よりも、非常に大量のN2Oを発生させることが分かる。
例2により製造したCu/ZSM-34、Cu/SAPO−34、Cu/SSZ-13及びCu/ベータを、例3に記載する様式でエージングし、例6により試験した。これらの結果を図15に示すが、そこから、リーン水熱エージングしたCu/SSZ-13、Cu/SAPO−34及びCu/ZSM-34試料のそれぞれのNOx転化活性は、対応する大細孔ゼオライト、Cu/ベータの活性より著しく優れていることが分かる。
Cu/SSZ-13及びCu/SAPO−34の新しい試料を例2により製造し、それらの試料を、例5に記載する様式でエージングした。新しい(すなわちエージングしていない)、及びエージングした試料を、例6により試験し、これらの結果を図16に示すが、そこから、Cu/SSZ-13のNOx転化活性が、長時間の過酷なリーン水熱エージングの後にも維持されることが分かる。
SARが約4であるCu/SAPO−34及びCu/天然産チャバザイト型材料を例2により製造し、これらの新しい材料を例6により試験した。これらの結果を図17に示すが、そこから、天然産Cu/チャバザイトのNOx転化活性が、Cu/SAPO−34よりも非常に低いことが分かる。図18は、例2により製造した2種類の新しいCu/天然産チャバザイト型材料のNOx転化活性を2つの温度データ点(200℃及び300℃)で比較する棒グラフであり、第一チャバザイト材料は、SARが約4であり、第二チャバザイト材料は、SARが約7である。SAR7チャバザイトのNOx転化活性は、SAR4チャバザイト材料の活性より優れており、SAR7チャバザイト材料の活性は、新しいCu/SAPO−34よりも非常に低いことが分かる。
Cu/SAPO−34及びCu/ベータを例2により製造した。Fe/ SAPO−34及びFe/SSZ-13を例1により製造した。これらの試料を例4によりエージングし、エージングした試料を例6により試験した。350℃及び450℃データ点におけるNOx活性を図19に示すが、そこから、Cu/SAPO−34、Fe/ SAPO−34及びFe/SSZ-13試料は、Cu/ベータ基準と同等か、またはそれより優れた性能を示すことが分かる。
例1により製造したFe/SSZ-13及びFe/ベータを、新しい状態で、例7に記載するようにを試験したが、その際、n-オクタン(排ガス中の未燃焼ディーゼル燃料の影響を模擬するために)を8分間で試験中に導入した。図20に示す結果は、NOx転 化活性を、n-オクタンを8分間で試験中に導入する前(HC−)と、n-オクタンを8分間で試験中に導入した後(HC+)で比較する。n-オクタン導入に 続いてFe/ベータ活性が、Fe/SSZ-13と比較して、劇的に低下することが分かる。我々は、この効果が、触媒のコークス形成によるものと考えてい る。
例1により製造したFe/SSZ-13を、新しい状態で、すなわちエージングせずに、例6に記載する様式で試験した。次いで、350 ppmNOを175 ppmNOと175 ppmNO2の混合物、すなわち合計350 ppmのNOxで置き換えた以外は、試験を同等の条件を使用して繰り返した。両方の試験から得た結果を図22に示すが、そこから、原料ガス中のNOxのNO2含有量を1:1に増加することから得られる重大な改良が分かる。実際には、NH3-SCR触媒の上流に配置した好適な酸化触媒を使用し、例えばディーゼルエンジンの排ガス中のNOを酸化することにより、NO:NO2比を調節することができる。
Claims (50)
- ガス中の窒素酸化物を窒素に転化する方法であって、
少なくとも一種の遷移金属を含むゼオライト触媒の存在下で、前記窒素酸化物を窒素系還元剤と接触させることを含んでなるものであり、
前記ゼオライトが、8個の四面体原子による最大環サイズを含む小細孔ゼオライトであり、かつ
前記少なくとも一種の遷移金属が、Cr、Mn、Fe、Co、Ce、Ni、Cu、Zn、Ga、Mo、Ru、Rh、Pd、Ag、In、Sn、Re、Ir及びPtからなる群から選択されてなる、方法。 - 前記ゼオライトが、一種以上の置換骨格金属を含む同一構造型である、請求項1に記載の方法。
- 前記置換骨格金属または各置換骨格金属が、As、B、Be、Co、Fe、Ga、Ge、Li、Mg、Mn、Zn及びZrからなる群から選択される、請求項2に記載の方法。
- 前記小細孔ゼオライトが、骨格型コードLTAを有する骨格型材料またはそれらの同一構造型ゼオライトではない、請求項1〜3のいずれか一項に記載の方法。
- 前記遷移金属含有小細孔ゼオライトが、Ce/エリオナイトではない、請求項1〜4のいずれか一項に記載の方法。
- 前記遷移金属含有小細孔ゼオライトが、Cu/チャバザイト、Mo/チャバザイト、Cu-Mo/チャバザイト、Cu/エリオナイト、Mo/エリオナイトまたはCu-Mo/エリオナイトではない、請求項1〜5のいずれか一項に記載の方法。
- 前記遷移金属含有小細孔ゼオライトが、Fe/チャバザイト、Fe/ZK-5、Fe/ZK-4、Fe-希土類元素/チャバザイト、Fe-希土類元素/ZK-5またはFe-希土類元素/ZK-4ではない、請求項1〜6のいずれか一項に記載の方法。
- 前記遷移金属含有小細孔ゼオライトが、Fe/チャバザイトではない、請求項1〜7のいずれか一項に記載の方法。
- 前記小細孔ゼオライトが、アルミノケイ酸塩ゼオライト、金属置換アルミノケイ酸塩ゼオライト及びアルミノリン酸塩ゼオライトからなる群から選択される、請求項1〜7のいずれか一項に記載の方法。
- 前記アルミノリン酸塩ゼオライトまたは各アルミノリン酸塩ゼオライトが、AlPOゼオライト、MeAlPOゼオライト、SAPOゼオライト及びMeAPSOゼオライトからなる群から選択される、請求項9に記載の方法。
- 前記小細孔ゼオライトが、ACO、AEI、AEN、AFN、AFT、AFX、ANA、APC、APD、ATT、CDO、CHA、DDR、DFT、EAB、 EDI、EPI、ERI、GIS、GOO、IHW、ITE、ITW、LEV、KFI、MER、MON、NSI、OWE、PAU、PHI、RHO、RTH、 SAT、SAV、SIV、THO、TSC、UEI、UFI、VNI、YUG及びZONからなる骨格型コードの群から選択される、請求項1〜10のいずれか 一項に記載の方法。
- 前記8個の四面体原子による最大環サイズを含む小細孔ゼオライトが、CHA、LEV、ERI及びDDRからなる骨格型コードの群から選択される、請求項11に記載の方法。
- 前記CHA骨格型コードゼオライトが、SAPO-34またはSSZ-13である、請求項12に記載の方法。
- 前記LEV骨格型コードゼオライトが、Nu-3である、請求項12に記載の方法。
- 前記ERI骨格型コードゼオライトが、ZSM-34である、請求項12に記載の方法。
- 前記DDR骨格型コードゼオライトが、シグマ-1である、請求項12に記載の方法。
- 前記ゼオライトが、水熱安定性を改良するために処理されている、請求項1〜16のいずれか一項に記載の方法。
- 前記ゼオライトの少なくとも一つの次元における細孔径が4.3Å未満である、請求項1〜17のいずれか一項に記載の方法。
- 前記ゼオライトが、三次元的構造を有する、請求項1〜18のいずれか一項に記載の方法。
- 前記ゼオライトが、二次元的構造を有する、請求項1〜18のいずれか一項に記載の方法。
- 前記少なくとも一種の遷移金属が、Cr、Ce、Mn、Fe、Co、Ni及びCuからなる群から選択される、請求項1〜20のいずれか一項に記載の方法。
- 前記少なくとも一種の遷移金属が、Fe、Ce及びCuからなる群から選択される、請求項1〜21のいずれか一項に記載の方法。
- 前記少なくとも一種の遷移金属が、Fe及び/またはCuである、請求項1〜22のいずれか一項に記載の方法。
- 前記触媒中に存在する前記少なくとも一種の遷移金属の合計が、前記ゼオライト触媒の総重量に対して0.01〜20重量%である、請求項1〜23のいずれか一項に記載の方法。
- 前記触媒中に存在する前記少なくとも一種の遷移金属の合計が、前記ゼオライト触媒の総重量に対して0.1〜10重量%である、請求項1〜24のいずれか一項に記載の方法。
- 前記触媒中に存在する前記少なくとも一種の遷移金属の合計が、前記ゼオライト触媒の総重量に対して0.5〜5重量%である、請求項25に記載の方法。
- 前記ゼオライト触媒が、Fe/CHA、特にFe/SAPO-34またはFe/SSZ-13からなる、請求項1〜26のいずれか一項に記載の方法。
- 前記ゼオライト触媒が、Cu/CHA、特にCu/SAPO-34またはCu/SSZ-13からなる、請求項1〜26のいずれか一項に記載の方法。
- 前記窒素酸化物が、還元剤で、少なくとも100℃の温度で還元される、請求項1〜28のいずれか一項に記載の方法。
- 前記温度が約150℃〜750℃である、請求項29に記載の方法。
- 前記窒素酸化物の還元が、酸素の存在下で行われる、請求項1〜30のいずれか一項に記載の方法。
- 前記窒素系還元体の添加を制御し、前記ゼオライト触媒入口において、NH3が、1:1NH3/NO及び4:3NH3/NO2で計算して、理論的アンモニアの60%〜200%になるように制御されてなる、請求項1〜31のいずれか一項に記載の方法。
- 前記ゼオライト触媒の上流に配置された酸化触媒を使用し、前記ガス中の一酸化窒素を二酸化窒素に酸化し、次いで、
得られたガスを窒素系還元体と混合し、前記混合物を前記ゼオライト触媒に供給し、
前記酸化触媒を適用し、約4:1〜約1:3であるNOとNO2の体積比を有してなる前記ゼオライト触媒に流入するガス流を付与してなる、請求項1〜32のいずれか一項に記載の方法。 - 前記ゼオライトが合成ゼオライトである、請求項1〜33のいずれか一項に記載の方法。
- 前記窒素系還元体が、アンモニア自体、ヒドラジン、または尿素((NH2) 2CO)、炭酸アンモニウム、カルバミン酸アンモニウム、炭酸水素アンモニウム及びギ酸アンモニウムからなる群から選択されたアンモニア前駆物質である、請求項1〜34のいずれか一項に記載の方法。
- 前記窒素酸化物含有ガスが、燃焼過程から得られる、請求項1〜35のいずれか一項に記載の方法。
- 前記燃焼過程が、車両リーンバーン内燃機関における燃料の燃焼である、請求項1〜36のいずれか一項に記載の方法。
- 車両リーンバーン内燃機関用の排気システムであって、
流出する排ガスを通過させる導管と、
窒素系還元体の供給源と、
前記排ガスの流路中に配置された、少なくとも一種の遷移金属を含むゼオライト触媒と、
前記ゼオライト触媒の上流で前記排ガス中に窒素系還元体を計量供給するための手段とを備えてなり、
前記ゼオライト触媒が、8個の四面体原子による最大環サイズを含む小細孔ゼオライトであり、
前記少なくとも一種の遷移金属が、Cr、Mn、Fe、Co、Ce、Ni、Cu、Zn、Ga、Mo、Ru、Rh、Pd、Ag、In、Sn、Re、Ir及びPtからなる群から選択される、排気システム。 - 前記ゼオライト触媒が、フロースルー基材上に被覆されている、請求項38に記載の排気システム。
- 使用の際に、前記計量供給手段を制御し、
前記ゼオライト触媒が、要求される効率以上で、NOx還元を触媒作用可能であると決定された時にのみ、前記流出する排ガス中に窒素系還元体を計量供給する手段を備えてなる、請求項38または39に記載の排気システム。 - 使用の際に、前記制御手段が、
排ガス温度、触媒床温度、加速器の位置、前記システム中を流れる排ガスの量、マニホルド真空、点火時期、エンジン速度、排ガスのラムダ値、前記エンジン中 に注入される燃料の量、及び排ガス再循環(EGR)バルブの位置、並びにEGRの量及びブースト圧からなる群から選択された、前記エンジンの状態を示す入 力に応答するように配置されてなる、請求項40に記載の排気システム。 - 使用の際に、前記制御手段が、決定された前記排ガス中の窒素酸化物の量に応答して窒素系還元体の計量供給を制御してなる、請求項41に記載の排気システム。
- 使用の際に、前記制御手段が、窒素系還元体を前記排ガス中に計量供給するように適応され、1:1NH3/NO及び4:3NH3/NO2で計算して、理論的アンモニアの60%〜200%が、前記ゼオライト触媒に入る前記排ガス中に存在してなる、請求項40〜42のいずれか一項に記載の排ガス。
- 前記制御手段が、予めプログラム化されたプロセッサーを備えてなる、請求項40〜43のいずれか一項に記載の排気システム。
- 一酸化窒素を二酸化窒素に酸化するための酸化触媒が、流出する排ガス中に窒素系還元体を計量供給するための前記手段の上流に配置されてなる、請求項38〜44のいずれか一項に記載の排気システム。
- 前記酸化触媒が、少なくとも一種の白金族金属、例えば白金、を含んでなる、請求項45に記載の排気システム。
- 使用の際に、前記酸化触媒を適用し、前記酸化触媒入口における排ガス温度150℃〜750℃において、NOとNO2の体積比を約4:1〜約1:3としてなる、請求項45または46に記載の排気システム。
- フィルター基材が、前記酸化触媒と前記ゼオライト触媒の間に配置されてなる、請求項38〜47のいずれか一項に記載の排気システム。
- 車両リーンバーンエンジン及び請求項38〜48のいずれか一項に記載の排気システムを含んでなる、装置。
- 前記エンジンが、ディーゼルエンジン、リーンバーンガソリンエンジン、または液化石油ガスもしくは天然ガスで作動するエンジンである、請求項49に記載の装置。
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