JP5771267B2 - 排気ガス中の窒素酸化物の選択触媒還元のための新規な混合酸化物材料 - Google Patents
排気ガス中の窒素酸化物の選択触媒還元のための新規な混合酸化物材料 Download PDFInfo
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- JP5771267B2 JP5771267B2 JP2013505359A JP2013505359A JP5771267B2 JP 5771267 B2 JP5771267 B2 JP 5771267B2 JP 2013505359 A JP2013505359 A JP 2013505359A JP 2013505359 A JP2013505359 A JP 2013505359A JP 5771267 B2 JP5771267 B2 JP 5771267B2
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- oxide
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- exhaust gas
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- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims description 123
- 239000007789 gas Substances 0.000 title claims description 65
- 238000010531 catalytic reduction reaction Methods 0.000 title claims description 15
- 239000000463 material Substances 0.000 title description 3
- 239000003054 catalyst Substances 0.000 claims description 168
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 58
- 238000000576 coating method Methods 0.000 claims description 57
- 239000011248 coating agent Substances 0.000 claims description 54
- 239000000203 mixture Substances 0.000 claims description 44
- 239000010457 zeolite Substances 0.000 claims description 44
- 229910021536 Zeolite Inorganic materials 0.000 claims description 32
- 150000001875 compounds Chemical class 0.000 claims description 31
- 229910021529 ammonia Inorganic materials 0.000 claims description 29
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 27
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 25
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 20
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 20
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 20
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 20
- 150000002910 rare earth metals Chemical class 0.000 claims description 18
- -1 zeolite compound Chemical class 0.000 claims description 17
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 14
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 14
- 239000003638 chemical reducing agent Substances 0.000 claims description 12
- 238000002485 combustion reaction Methods 0.000 claims description 10
- 230000009467 reduction Effects 0.000 claims description 10
- 238000006722 reduction reaction Methods 0.000 claims description 10
- 238000000746 purification Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 8
- 150000001768 cations Chemical class 0.000 claims description 7
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 description 47
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 26
- 238000012360 testing method Methods 0.000 description 24
- 238000000034 method Methods 0.000 description 22
- 230000008569 process Effects 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 18
- 229910052760 oxygen Inorganic materials 0.000 description 17
- 239000001301 oxygen Substances 0.000 description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 15
- 239000010949 copper Substances 0.000 description 13
- 229910052757 nitrogen Inorganic materials 0.000 description 13
- 230000003197 catalytic effect Effects 0.000 description 12
- 230000032683 aging Effects 0.000 description 11
- RCFVMJKOEJFGTM-UHFFFAOYSA-N cerium zirconium Chemical compound [Zr].[Ce] RCFVMJKOEJFGTM-UHFFFAOYSA-N 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 10
- 239000000725 suspension Substances 0.000 description 10
- 229910052742 iron Inorganic materials 0.000 description 9
- 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 8
- 239000000919 ceramic Substances 0.000 description 8
- 229910001935 vanadium oxide Inorganic materials 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 6
- 238000007598 dipping method Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910052726 zirconium Inorganic materials 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 5
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 5
- 229910052721 tungsten Inorganic materials 0.000 description 5
- 239000010937 tungsten Substances 0.000 description 5
- 229910001930 tungsten oxide Inorganic materials 0.000 description 5
- 229910052720 vanadium Inorganic materials 0.000 description 5
- 229910052684 Cerium Inorganic materials 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 210000002421 cell wall Anatomy 0.000 description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052691 Erbium Inorganic materials 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 229910001593 boehmite Inorganic materials 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
- 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 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 3
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 238000003878 thermal aging Methods 0.000 description 3
- 229910001887 tin oxide Inorganic materials 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical group 0.000 description 3
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical group [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 3
- 238000011144 upstream manufacturing Methods 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical group [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical class [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 2
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910002706 AlOOH Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-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
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052689 Holmium Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- TXONVAMTMVNDJZ-UHFFFAOYSA-N [O-2].[Zr+4].[W+4].[O-2].[O-2].[O-2] Chemical class [O-2].[Zr+4].[W+4].[O-2].[O-2].[O-2] TXONVAMTMVNDJZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052768 actinide Inorganic materials 0.000 description 1
- 150000001255 actinides Chemical class 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- DNXNYEBMOSARMM-UHFFFAOYSA-N alumane;zirconium Chemical compound [AlH3].[Zr] DNXNYEBMOSARMM-UHFFFAOYSA-N 0.000 description 1
- BVCZEBOGSOYJJT-UHFFFAOYSA-N ammonium carbamate Chemical compound [NH4+].NC([O-])=O BVCZEBOGSOYJJT-UHFFFAOYSA-N 0.000 description 1
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- XFHGGMBZPXFEOU-UHFFFAOYSA-I azanium;niobium(5+);oxalate Chemical compound [NH4+].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XFHGGMBZPXFEOU-UHFFFAOYSA-I 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-N carbonic acid monoamide Natural products NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 1
- JUXLQRHSAFOZOE-UHFFFAOYSA-N cerium(3+);dioxido(dioxo)tungsten Chemical compound [Ce+3].[Ce+3].[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O JUXLQRHSAFOZOE-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 description 1
- 229910000311 lanthanide oxide Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical group [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 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- 239000006262 metallic foam Substances 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
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- QHMGFQBUOCYLDT-RNFRBKRXSA-N n-(diaminomethylidene)-2-[(2r,5r)-2,5-dimethyl-2,5-dihydropyrrol-1-yl]acetamide Chemical compound C[C@@H]1C=C[C@@H](C)N1CC(=O)N=C(N)N QHMGFQBUOCYLDT-RNFRBKRXSA-N 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 150000002822 niobium compounds Chemical class 0.000 description 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229910000487 osmium oxide Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- JIWAALDUIFCBLV-UHFFFAOYSA-N oxoosmium Chemical compound [Os]=O JIWAALDUIFCBLV-UHFFFAOYSA-N 0.000 description 1
- DYIZHKNUQPHNJY-UHFFFAOYSA-N oxorhenium Chemical compound [Re]=O DYIZHKNUQPHNJY-UHFFFAOYSA-N 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000000819 phase cycle Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 239000012041 precatalyst Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 229910003449 rhenium oxide Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- PMTRSEDNJGMXLN-UHFFFAOYSA-N titanium zirconium Chemical compound [Ti].[Zr] PMTRSEDNJGMXLN-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 150000003754 zirconium Chemical class 0.000 description 1
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Description
特許文献14には、炭化水素または酸素含有有機化合物による還元により排気ガス中の窒素酸化物の量を減少する触媒系およびプロセスが記載されている。銀含有触媒および「変性触媒」で構成された触媒系が用いられている。「変性触媒」は、鉄酸化物、セリウム酸化物、銅酸化物、マンガン酸化物、クロム酸化物、ランタニド酸化物、アクチノイド酸化物、モリブデン酸化物、錫酸化物、インジウム酸化物、レニウム酸化物、タンタル酸化物、オスミウム酸化物、バリウム酸化物、カルシウム酸化物、ストロンチウム酸化物、カリウム酸化物、カルシウム酸化物、バナジウム酸化物、ニッケル酸化物、タングステン酸化物およびこれらの混合物からなる群から選択される「変性酸化物」を含有する。この「変性酸化物」は、少なくとも1つが酸性で、チタン−ジルコニウム混合酸化物、ジルコニウム−アルミニウム混合酸化物、硫酸化ジルコニウム酸化物、リン酸化ジルコニウム酸化物、タングステン−変性ジルコニウム混合酸化物、ケイ素−アルミニウム混合酸化物、ゼオライトおよびこれらの混合物からなる群から好ましくは選択される無機担体酸化物に適用される。
後述する実施例および比較例で調製した混合酸化物組成物を、水中に懸濁し、ミリングし、壁厚0.17mmで、0.5lの体積および1平方センチメートル当たり62個のセルのセル数のセラミックハニカム体に適用した。ハニカム体を500℃で2時間空気中でか焼した後、直径25.4mmおよび長さ76.2mmのモデルガスプラントで試験するためにコートしたハニカム体からシリンダー形ドリルコアを切断した。
式中、cInlet/Outlet(NOx)=cIn/Out(NO)+cIn/Out(NO2)・・・。
CeO2:ZrO2の重量比が1:1.1およびNd2O3含量が5.3重量%の市販のセリウム−ジルコニウム混合酸化物に、アンモニウムニオブオキサレート水溶液を含浸し、500℃で2時間か焼した。本発明により得られる混合酸化物組成物は、38重量%のCeO2、14.5重量%のNb2O5、4.5重量%のNd2O3および43重量%のZrO2からなっていた。
実施例1に示したのと同様の手順を用いて、以下の組成を有する混合酸化物を得た。38重量%のCeO2、14.5重量%のNb2O5、4.5重量%のY2O3および43重量%のZrO2。
酸化バナジウムをベースとし、V2O5、WO3、TiO2およびSiO2からなる触媒活性コーティングを含有する市販のSCR触媒を、第1の比較触媒として選択した。
触媒不活性ハニカム体に15重量%のWO3、46.75重量%のZrO2、27.2重量%のCeO2、5.1重量%のY2O3および5.95重量%のNb2O3からなる触媒活性コーティングを含有する第2の比較触媒を、国際公開第2008/051752号パンフレットに記載されたとおりにして生成した。
コーティング助剤として、市販のSiO2バインダーおよび市販のベーマイトバインダーおよび硝酸鉄(III)九水和物およびモルSiO2/Al2O3比(SAR)が25の市販のβ−ゼオライトを、水に懸濁し、222g/lの量で、1平方センチメートル当たり62個のセルおよびセル壁厚0.17ミリメートルのセラミックフロースルーハニカム体に、通常のディッピングプロセスにより適用した。コートした成分をまず、350℃で15分間、その後、500℃で2時間か焼した。コーティングは、90%のβ−ゼオライトを含み、Fe2O3として計算した鉄含量は4.5重量%であった。
図2a)に示す層触媒を生成した。このために、比較例3と同様のやり方で得た触媒(適用量が222g/lの代わりに150g/l)に、実施例1によるコーティング懸濁液を、70g/lの量で、再び、通常のディッピングプロセスにより適用し、示したとおりか焼することにより追加のコーティングを与えた。
試験は、工場モデルガスプラントにおいて、担体触媒で実施した。以下の試験ガス組成物を用いた。
フェーズ1:空の容器、保持時間10分(600℃)
フェーズ2:ターゲット温度まで冷やす(10K/分)、保持時間5分
フェーズ3:NH3吸着フェーズ、保持時間20分
フェーズ4:NH3脱着フェーズ、NH3の切替、保持時間20分
フェーズ5:600℃まで加熱
フェーズ6:空の容器:NO切り替え、保持時間10分
Δc(NH3)Ph3,t=c(NH3)Ph3,end−c(NH3)Ph3,t
プロットΔc(NH3)Ph3,tの、フェーズ3についての時間tに対する積分は、濃度c(NH3)の質量m(NH3)への適切な変換後、考慮中の温度点についての合計貯蔵容量m(NH3)[触媒のmg/l)を与える。
Δm(NH3)=m(NH3)fresh-m(NH3)aged
図2b)に示す層触媒を生成した。このため、実施例2に記載したコーティングを、1平方センチメートル当たり62個のセルおよびセル壁厚0.17ミリメートルのセラミックフロースルーハニカム体に、70g/lの量で、通常のディッピングプロセスにより適用し、実施例3に記載されたとおりにしてか焼した。
図1a)に示すゾーン触媒を生成した。このため、実施例2に記載したコーティングを、第1の作業工程において、1平方センチメートル当たり62個のセルおよびセル壁厚0.17ミリメートルのセラミックフロースルーハニカム体に、200g/lの量で、通常のディッピングプロセスにより適用した。ただし、ハニカム体の入口端面から始まるその長さの僅か50%であった。
第2の作動工程において、比較例3に記載したコーティング懸濁液を、比較例4に記載したコーティング懸濁液の代わりに適用した以外は、実施例5に記載したプロセスを繰り返した。
市販のSAPO−34を水中に懸濁し、硝酸銅(II)水溶液を添加することにより、コーティング懸濁液を生成した。最終触媒が、交換ゼオライト類の化合物の総重量を基準として、2重量%のCuを含有するように、添加した硝酸銅溶液の量を計算した。懸濁液を、30分間攪拌して、イオン交換を完了し、バインダーとしてシリカゾルを添加した後、1平方センチメートル当たり62個のセルおよびセル壁厚0.165ミリメートルおよび直径92.96ミリメートルおよび長さ76.2ミリメートルのセラミックフロースルーハニカム体に直接適用した。このようにしてコートしたハニカム体を、90℃で乾燥し、350℃でか焼し、640℃で空気中2時間熱処理した。
試験は、実験室モデルガスプラントにおいて、担体触媒で実施した。以下の試験ガス組成物をセットした。
フェーズA:ガス混合物1、時間:5分
フェーズB:NH3SCRフェーズ:ガス混合物2、時間:20vpmmのNH3ブレークスルーまで、または一定の時間後
フェーズC:ガス混合物3、500℃までの昇温により、NH3貯蔵を空にする
フェーズD:ガス混合物3、混合測定温度の設定。
本発明の好ましい実施形態によれば、例えば、以下が提供される。
(項1)
酸化セリウム、酸化ニオブ、希土類金属三二酸化物および酸化ジルコニウムからなる触媒活性混合酸化物の、窒素酸化物の選択触媒還元のための、使用。
(項2)
前記混合酸化物が、
いずれの場合も主要酸化物として計算すると、
C 3 O 2 :15〜50重量%、
Nb 2 O 5 :3〜25重量%、
RE 2 O 3 :3〜10重量%
ZrO 2 :残部
からなることを特徴とする、請求項1に記載の使用。
(項3)
前記混合酸化物が、触媒活性コーティングと共に触媒を形成する触媒不活性担体に適用された、前記コーティング中に存在することを特徴とする、請求項1または2に記載の使用。
(項4)
(i)酸化セリウム、酸化ニオブ、希土類金属三二酸化物および酸化ジルコニウムからなる混合酸化物と、(ii)H + 、NH 4 + 、Fe 2+ 、Fe 3+ 、Cu + 、Cu 2+ 、Ag + およびこれらの混合物からなる群から選択される交換可能なカチオンを含有するゼオライト化合物および/またはゼオライト類の化合物とを含む、触媒活性組成物。
(項5)
(i)酸化セリウム、酸化ニオブ、希土類金属三二酸化物および酸化ジルコニウムからなる混合酸化物と、(ii)H + 、NH 4 + 、Fe 2+ 、Fe 3+ 、Cu + 、Cu 2+ 、Ag + およびこれらの混合物からなる群から選択される交換可能なカチオンを含有するゼオライト化合物および/またはゼオライト類の化合物とを含む、触媒。
(項6)
前記ゼオライト化合物および/または前記ゼオライト類の化合物が、ベータゼオライト、USY、ZSM−5、CHA、FER、ERI、SAPO−11、SAPO−17、SAPO−34、SAPO−56、ALPO−11、ALPO−17、ALPO−34およびALPO−56からなる群から選択されることを特徴とする、請求項5に記載の触媒。
(項7)
前記触媒がコートされた不活性担体として存在し、それに適用された少なくとも1つの触媒活性コーティング中に前記混合酸化物が存在し、前記ゼオライト化合物および/または前記ゼオライト類の化合物が、さらに物理的に別の触媒活性コーティング中に存在することを特徴とする、請求項5または6に記載の触媒。
(項8)
前記触媒活性コーティングが、前記担体上に、排気ガスの流れ方向において互いに水平に続くゾーンとして構成されている(「ゾーン触媒」)ことを特徴とする、請求項7に記載の触媒。
(項9)
前記触媒活性コーティングが、前記担体上に、コンポーネントの全長にわたって垂直に重なった層として構成されている(「層触媒」)ことを特徴とする、請求項7に記載の触媒。
(項10)
酸化アルミニウム、酸化ジルコニウムおよび二酸化ケイ素からなる群から選択されるバインダーが、少なくとも1つの触媒活性コーティング中に存在することを特徴とする、請求項7〜9のいずれか1項に記載の触媒。
(項11)
主に希薄条件下で操作される内燃機関の前記排気ガスを精製するための、請求項5〜10のいずれか1項に記載の触媒の、使用。
(項12)
精製する前記排気ガスへの還元剤として、任意選択により分解するとアンモニアを形成することのできる化合物の形態でのアンモニアの添加後の、主に希薄条件下で操作される内燃機関の前記排気ガス中の窒素酸化物を選択触媒還元するための、請求項5〜10のいずれか1項に記載の触媒の、使用。
Claims (13)
- 酸化セリウム、酸化ニオブ、希土類金属三二酸化物および酸化ジルコニウムからなる触媒活性混合酸化物の、窒素酸化物の選択触媒還元のための、使用。
- 前記混合酸化物が、
いずれの場合も主要酸化物として計算すると、
CeO2:15〜50重量%、
Nb2O5:3〜25重量%、
RE2O3:3〜10重量%
ZrO2:残部
からなることを特徴とする、請求項1に記載の使用。 - 前記混合酸化物が、触媒活性コーティングと共に触媒を形成する触媒不活性担体に適用された、前記コーティング中に存在することを特徴とする、請求項1または2に記載の使用。
- (i)酸化セリウム、酸化ニオブ、希土類金属三二酸化物および酸化ジルコニウムからなる混合酸化物と、(ii)H+、NH4 +、Fe2+、Fe3+、Cu+、Cu2+、Ag+およびこれらの混合物からなる群から選択される交換可能なカチオンを含有するゼオライト化合物および/またはゼオライト類の化合物とを含む、排気ガス中の窒素酸化物の選択的還元触媒として使用するための触媒活性組成物。
- (i)酸化セリウム、酸化ニオブ、希土類金属三二酸化物および酸化ジルコニウムからなる混合酸化物と、(ii)H+、NH4 +、Fe2+、Fe3+、Cu+、Cu2+、Ag+およびこれらの混合物からなる群から選択される交換可能なカチオンを含有するゼオライト化合物および/またはゼオライト類の化合物とを含む、排気ガス中の窒素酸化物の選択的還元触媒として使用するための触媒。
- 前記ゼオライト化合物および/または前記ゼオライト類の化合物が、ベータゼオライト、USY、ZSM−5、CHA、FER、ERI、SAPO−11、SAPO−17、SAPO−34、SAPO−56、ALPO−11、ALPO−17、ALPO−34およびALPO−56からなる群から選択されることを特徴とする、請求項5に記載の触媒。
- 前記触媒がコートされた不活性担体として存在し、それに適用された少なくとも1つの触媒活性コーティング中に前記混合酸化物が存在し、前記ゼオライト化合物および/または前記ゼオライト類の化合物が、さらに物理的に別の触媒活性コーティング中に存在することを特徴とする、請求項5または6に記載の触媒。
- 前記触媒活性コーティングが、前記担体上に、排気ガスの流れ方向において互いに水平に続くゾーンとして構成されている(「ゾーン触媒」)ことを特徴とする、請求項7に記載の触媒。
- 前記触媒活性コーティングが、前記担体上に、コンポーネントの全長にわたって垂直に重なった層として構成されている(「層触媒」)ことを特徴とする、請求項7に記載の触媒。
- 酸化アルミニウム、酸化ジルコニウムおよび二酸化ケイ素からなる群から選択されるバインダーが、少なくとも1つの触媒活性コーティング中に存在することを特徴とする、請求項7〜9のいずれか1項に記載の触媒。
- 希薄条件下で操作される内燃機関の前記排気ガスを精製するための、請求項5〜10のいずれか1項に記載の触媒の、使用。
- 精製する前記排気ガスへの還元剤として、アンモニアの添加後の希薄条件下で操作される内燃機関の前記排気ガス中の窒素酸化物を選択触媒還元するための、請求項5〜10のいずれか1項に記載の触媒の、使用。
- 前記アンモニアの添加が、分解するとアンモニアを形成することのできる化合物の形態における、請求項12に記載の使用。
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EP2116293B1 (de) | 2008-04-11 | 2010-03-17 | Umicore AG & Co. KG | Abgasreinigungssystem zur Behandlung von Motorenabgasen mittels SCR-Katalysator |
WO2010064497A1 (ja) * | 2008-12-03 | 2010-06-10 | 第一稀元素化学工業株式会社 | 排気ガス浄化触媒、それを用いた排気ガス浄化装置、及び排気ガス浄化方法 |
US8017097B1 (en) * | 2010-03-26 | 2011-09-13 | Umicore Ag & Co. Kg | ZrOx, Ce-ZrOx, Ce-Zr-REOx as host matrices for redox active cations for low temperature, hydrothermally durable and poison resistant SCR catalysts |
FR2962431B1 (fr) * | 2010-07-07 | 2018-01-19 | Rhodia Operations | Composition a base d'oxydes de cerium, de niobium et, eventuellement, de zirconium et son utilisation en catlyse. |
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- 2011-04-16 EP EP11716376A patent/EP2560755A1/de not_active Withdrawn
- 2011-04-16 KR KR1020127030255A patent/KR20130097076A/ko not_active Application Discontinuation
- 2011-04-16 WO PCT/EP2011/001944 patent/WO2011131324A1/de active Application Filing
- 2011-04-16 JP JP2013505359A patent/JP5771267B2/ja active Active
- 2011-04-16 US US13/642,048 patent/US8617497B2/en active Active
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US8617497B2 (en) | 2013-12-31 |
CN102844112B (zh) | 2015-05-13 |
EP2560755A1 (de) | 2013-02-27 |
WO2011131324A1 (de) | 2011-10-27 |
CN102844112A (zh) | 2012-12-26 |
BR112012027087A2 (pt) | 2016-07-26 |
JP2013527799A (ja) | 2013-07-04 |
KR20130097076A (ko) | 2013-09-02 |
US20130121902A1 (en) | 2013-05-16 |
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