CN1320475A - 还原氮氧化物的方法及催化剂 - Google Patents
还原氮氧化物的方法及催化剂 Download PDFInfo
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- CN1320475A CN1320475A CN01109781A CN01109781A CN1320475A CN 1320475 A CN1320475 A CN 1320475A CN 01109781 A CN01109781 A CN 01109781A CN 01109781 A CN01109781 A CN 01109781A CN 1320475 A CN1320475 A CN 1320475A
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- catalyst
- zeolite
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- iron
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- 239000003054 catalyst Substances 0.000 title claims abstract description 116
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 238000000034 method Methods 0.000 title claims abstract description 28
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 52
- 230000003647 oxidation Effects 0.000 claims abstract description 32
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 32
- 239000010457 zeolite Substances 0.000 claims abstract description 32
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 31
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 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 abstract description 27
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 26
- 239000007789 gas Substances 0.000 claims abstract description 19
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 7
- 150000003624 transition metals Chemical class 0.000 claims abstract description 7
- 238000002485 combustion reaction Methods 0.000 claims abstract description 6
- 239000002912 waste gas Substances 0.000 claims description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 239000000919 ceramic Substances 0.000 claims description 12
- 229910052742 iron Inorganic materials 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 239000010949 copper Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910001868 water Inorganic materials 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 229910052720 vanadium Inorganic materials 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- 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 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 claims description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 239000011651 chromium Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 229910001657 ferrierite group Inorganic materials 0.000 claims description 2
- YOWAEZWWQFSEJD-UHFFFAOYSA-N quinoxalin-2-amine Chemical compound C1=CC=CC2=NC(N)=CN=C21 YOWAEZWWQFSEJD-UHFFFAOYSA-N 0.000 claims description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims 1
- 238000006722 reduction reaction Methods 0.000 abstract description 9
- 238000010531 catalytic reduction reaction Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 26
- 229910052757 nitrogen Inorganic materials 0.000 description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000005342 ion exchange Methods 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 6
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000003546 flue gas Substances 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 3
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 3
- -1 particulate filter Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000011144 upstream manufacturing Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- 239000012876 carrier material Substances 0.000 description 2
- 230000001413 cellular effect Effects 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 229910052878 cordierite Inorganic materials 0.000 description 2
- 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 2
- 238000007599 discharging Methods 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 208000019901 Anxiety disease Diseases 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 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
- 239000002253 acid Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000036506 anxiety Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- PPBAJDRXASKAGH-UHFFFAOYSA-N azane;urea Chemical compound N.NC(N)=O PPBAJDRXASKAGH-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000012013 faujasite Substances 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 235000013842 nitrous oxide Nutrition 0.000 description 1
- 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 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
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- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
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- F01N3/2066—Selective catalytic reduction [SCR]
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
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- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
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- 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
- B01D53/9459—Removing one or more of nitrogen oxides, carbon monoxide, or hydrocarbons by multiple successive catalytic functions; systems with more than one different function, e.g. zone coated catalysts
- B01D53/9477—Removing one or more of nitrogen oxides, carbon monoxide, or hydrocarbons by multiple successive catalytic functions; systems with more than one different function, e.g. zone coated catalysts with catalysts positioned on separate bricks, e.g. exhaust systems
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/064—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof containing iron group metals, noble metals or copper
- B01J29/072—Iron group metals or copper
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- 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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Abstract
本发明涉及一种还原内燃机所产生的稀薄废气中的氮氧化物的方法,其是在还原催化剂上使用氨来进行选择性催化还原,其中废气中所含的一部分一氧化氮在废气与氨一起从还原催化剂上通过之前被氧化为二氧化氮。该方法的特征在于,还原催化剂包含已与过渡金属交换的沸石,而且一氧化氮的氧化使得废气在与还原催化剂接触前包含30-70vol%的二氧化氮。
Description
本发明涉及还原内燃机所产生的稀薄废气中的氮氧化物的方法,其是在还原催化剂上使用氨来进行选择性催化还原,其中废气中所含的一部分一氧化氮在废气与氨一起在还原催化剂上通过之前被氧化成二氧化氮。
选择性催化(SCR)的方法长时间以来都是在发电厂中使用,以还原发电站所产生的烟道气中的氮氧化物。发电站所产生的烟道气因为含有高比例的氧气而具有净氧化作用。其中存在的氮氧化物因此可被还原成氮,仅略有困难。该困难可用所谓的选择性催化还原来解决,其中烟道气与氨混合,然后于300-550℃的温度下从合适的还原剂上通过。除包含钒氧化物和钨氧化物的二氧化钛催化剂外,所用的还原催化剂也可以是经离子交换的沸石,如ZSM-5、丝光沸石和八面沸石。适合于选择性催化还原的还原催化剂在以下也称为SCR催化剂。
在最近几年中已进行了许多努力来使用选择性催化还原,以便从柴油发动机和稀薄汽油发动机所产生的废气中除去氮氧化物。这些废气也包含高比例的氧,最高可达15vol%。其中所包含的约60-95vol%的氮氧化物由一氧化氮组成,这取决于发动机的运行状态。
已知的SCR催化剂的缺陷是,在轿车废气处理时主要是处于高空间速度,此时催化剂的催化活性不够高,而且易于快速老化。对于包含氧化钒的催化剂,在超过700℃的温度下将大大失去活性。
DE19820682A1公开了为提高对内燃机所产生的稀薄废气的还原,可初始将废气中的二氧化氮的浓度提高至50vol%。根据所公开的应用,这可通过在气体放电(electrical gas discharge)中将一氧化氮氧化为二氧化氮来进行。以此方式处理的废气然后从SCR催化剂上通过,并同时提供还原剂、优选氨。合适的SCR催化剂可以是发电站脱氮领域中的催化剂以及已经与铜离子进行交换的ZSM-5沸石。
US5,891,409披露了许多还原催化剂对于还原二氧化氮比还原一氧化氮具有更高的活性。因此,US5,891,409建议首先在氧化催化剂上将内燃机所产生的稀薄废气中存在的一氧化氮氧化为二氧化氮,然后在SCR催化剂上将所形成的二氧化氮转化为氮、二氧化碳和水,同时添加烃作为还原剂。其提到由γ-氧化铝组成的催化剂是优选的还原催化剂。
WO99/39809描述了用于减少内燃机废气、特别是柴油发动机废气中的氮氧化物的体系,其由氧化催化剂、颗粒过滤器、还原剂如氨源和SCR催化剂组成,所述氧化催化剂将至少一部分一氧化氮转化为二氧化氮。在使用该体系时,氮氧化物的转化可大大提高。优选使用基于V2O5/WO3/TiO2催化剂的SCR催化剂。
与通常用于发电站中的V2O5/WO3/TiO2催化剂相关的一个问题是在高的废气温度下有可能排放出挥发性的有毒的钒化合物。用无钒的催化剂替换这些含钒的催化剂,例如基于已与过渡金属如铁或铜交换过的沸石的催化剂,由于已知这些催化剂具有低的老化稳定性,它们似乎并不合适。
本发明的目的是提供一种还原稀薄废气中所含的氮氧化物的方法,其是在还原催化剂上使用氨进行选择性催化还原,与现有技术相比,该方法在高的废气温度下没有任何或者大大减少了钒化合物的排放,而且其特征在于SCR催化剂具有显著的活性和长期的稳定性。
该目的是通过使用氨的选择性催化还原方法来实现的,其中废气中所含的一部分一氧化氮在废气与氨一起从还原催化剂上通过之前被氧化为二氧化氮。该方法的特征在于,还原催化剂包含已与过渡金属交换的沸石,而且一氧化氮的氧化使得废气在与还原催化剂接触前包含30-70vol%的二氧化氮。
根据本发明,不使用V2O5/WO3/TiO2催化剂,而是使用已与特定的过渡金属交换的沸石催化剂。优选的过渡金属是铬、铁、镍、铜、铈、镨、Tb或它们的混合物。在此也可使用钒作为交换组分,这是因为与V2O5/WO3/TiO2催化剂相比钒基本上更为牢固地键合在沸石催化剂的晶格中。但优选的是仍避免使用钒作为交换元素。
已证实增加废气中的二氧化氮含量可大大提高所述还原催化剂的活性,而且还可减少催化剂的老化。另外,二氧化氮还特别增加催化剂在低温时的活性。猜测二氧化氮的此等正面作用是基于以下事实,例如催化剂中的二价铜离子由于选择性催化还原而被还原为一价铜,这意味着它们的催化活性被降低。由于废气中存在的氧化性组分,如氧气和二氧化氮,铜离子被重新氧化成二价铜离子,并由此恢复它们的原始活性。二氧化氮在此以特别有利的方式发挥作用,这是由于其相对较高的氧化能力。该反应原理适用于所有的SCR-活性过渡金属离子,其允许该类型的价键变化。这包括钒、铬、铁、镍、铜、铈、镨和Tb的离子。铁、铜和铈的离子是特别合适的。
适合用于本发明中的沸石例如是选自于以下组中的沸石:ZSM-5、A、β、X、Y、Ferrierite、Linde型L和八面体型沸石。这些沸石可以混合物的形式使用。
与铁和/或铜交换的ZXM-5沸石特别优选用作催化剂。其对于产生氮具有高的选择性。当使用Fe-ZSM-5催化剂时,仅有少量的SCR反应副产物例如笑气(N2O)。
为形成二氧化氮或者增加发动机所产生的废气中的二氧化氮的量,在实际SCR催化剂的上游设置氧化催化剂。特别是当使用Fe-ZSM-5时,即使老化后,仍可在SCR反应中实现高的转化率。除氧化催化剂外,也可使用其他产生二氧化氮的装置如气体放电装置。
一氧化氮在氧化催化剂上完全转化为二氧化氮并不是令人希望的,而且可通过与还原催化剂相比适当地负载和/或施加氧化催化剂来避免。可使用在由活性且任选经稳定的氧化铝组成的载体材料上的铂催化剂作为氧化催化剂。相对于催化剂的总重量,在载体材料上的铂浓度可为0.1-5wt%。以涂层的形式将催化剂涂敷在常规蜂窝体上。涂层浓度可在50-200g/l蜂窝体之间选择,以确保氧化催化剂下游的废气包含约30-70vol%的二氧化氮。还可通过所用蜂窝体的体积来调节二氧化氮的产生。
另外,氧化催化剂的目的是尽可能完全地将废气中所包含的一氧化碳、特别是烃转化为二氧化碳和水,因为否则这些烃将会被随后的沸石催化剂储存。这有使沸石催化剂阻塞及失活之虞。
适用于本发明方法中的氧化催化剂是那些在高表面积载体氧化物、优选γ-氧化铝上包含铂作为催化活性成分的催化剂。用约5wt%二氧化硅稳定的氧化铝是特别有益的。
选择性催化还原所需要的氨可直接在与还原催化剂接触前添加至废气中。但优选的是,氨是在车辆上由可水解产生氨的化合物得到的。为此目的,可水解的化合物在一氧化氮的部分氧化之后但在与还原催化剂接触之前添加在废气中,然后使废气从水解催化剂上通过。脲或氨基甲酸铵适合用作可水解的化合物。
本发明方法所需要的SCR催化剂是与上述金属离子交换的沸石催化剂。可使用各种离子交换法来制备该催化剂(固体交换、水溶液中的交换、极性或非极性有机溶液中的交换)。但是,已证实制备Fe-ZSM-5是特别困难的。常规在水溶液中的交换法已证明都是无用的,这是因为铁(Ⅲ)化合物由于具有大的水合外层而几乎不能渗透入沸石的孔中,而且使得在酸溶液中的交换非常困难。在氨溶液中的交换也被证明是不合适的,因为可形成氢氧化铁并沉淀出来。
使用铁(Ⅱ)的水溶液的交换通常首先使铁(Ⅱ)被氧化为铁(Ⅲ),但可通过用惰性气体如氮气或氩气对溶剂进行适当的预处理来解决。但除硫酸铁(Ⅱ)和氯化铁(Ⅱ)外,可使用略微溶解性的铁盐。当使用溶解度低的盐时,离子交换仅缓慢进行。
已证明最简单而且最好的方法是沸石与氯化铁(Ⅱ)和氯化铁(Ⅲ)的固体离子交换。完全交换所需要的铁盐量与沸石混合,形成均匀的粉末。然后在氮气流中加热该混合物至发生离子交换的温度。所形成的氯化氢随氮气流排出。从经验上来看,离子交换在300℃下约2小时后完成。经交换的沸石然后用水洗涤,并在120℃下干燥。混合物在氮气中于恒定的300℃下再保持2小时。
最终的沸石催化剂优选以涂层的形式涂敷在由陶瓷或金属制成的蜂窝体上。为此目的,催化剂粉末与作为粘合剂的硝酸氧锆一起悬浮在水中。根据已知的方法用所得的涂敷悬浮液涂敷所希望的蜂窝体。优选在每升蜂窝体中用最多200克的催化剂粉末进行涂敷。涂敷完成后,煅烧蜂窝体,例如在约300℃下进行4小时,以将催化剂粉末固定在蜂窝体上,并将硝酸氧锆转化为氧化锆。以涂层的总重量计,优选的催化剂包含1-10wt%的氧化锆。
以下将用图1-9和实施例来更为详细地说明本发明。在附图中:
图1是在废气中直接添加氨的废气净化体系的示意图。
图2是通过水解氨释放化合物而产生氨的废气净化体系的示意图。
图3是在空间速度为30000h-1、NO/NO2体积比为1∶1时,新制的Fe-ZSM5催化剂的氮氧化物转化程度X随废气温度的变化。
图4是在空间速度为30000h-1、NO/NO2体积比为3∶1时,已老化的Fe-ZSM5催化剂的氮氧化物转化程度X随废气温度的变化。
图5是在空间速度为30000h-1、NO/NO2体积比为1∶1时,已老化的Fe-ZSM5催化剂的氮氧化物转化程度X随废气温度的变化。
图6是在空间速度为30000h-1、NO/NO2体积比为1∶3时,已老化的Fe-ZSM5催化剂的氮氧化物转化程度X随废气温度的变化。
图7是在空间速度为60000h-1和不同的废气温度下,氧化催化后在废气中的NO2浓度。
图8是在空间速度为120000h-1和不同的废气温度下,氧化催化后在废气中的NO2浓度。
图9是在空间速度为180000h-1和不同的废气温度下,氧化催化后在废气中的NO2浓度。
图1显示了适合用于本发明方法中的废气净化体系的示意图。其由氧化催化剂(1)和下游的还原催化剂(2)组成。从内燃机中产生的废气包括一氧化氮和氧气,其进入氧化催化剂。一部分一氧化氮在氧化催化剂中被氧化为二氧化氮,使得从氧化催化剂中产生一氧化氮和二氧化氮的混合物。在进入还原催化剂之前,将还原剂氨添加在该气体混合物中,NH3/NOx的摩尔比为0.6-1.6。该气体混合物在还原催化剂中转化为氮和水。NH3/NOx的摩尔比以下也称为α值(α)。
图2显示了图1中废气处理体系的一个变化例。替代氨将能够分解产生氨的化合物如脲添加在氧化催化剂下游的废气中。为释放氨,在还原催化剂上游的废气流中设置脲水解催化剂(3),其可将脲分解为氨、二氧化碳和水。制备还原催化剂
如下制备用于本发明方法中的Fe-ZSM5催化剂:模量为40(沸石的模量是SiO2/Al2O3的摩尔比)的沸石H-ZSM5小心地与FeCl3混合,然后在氮气流中于恒定的300℃下保持2小时。测量FeCl3的量,根据其交换容量使沸石的交换进行完全。经交换的沸石然后用水洗涤,在120℃下干燥,接着在氮气中于300℃下再处理2小时。
以粉末的总重量计,以此方式得到的催化剂粉末具有1.7wt%的铁含量。将该粉末与作为粘合剂的硝酸氧锆一起分散在水中,并用于涂敷常规的堇青石蜂窝体,其蜂窝密度为62cm-2。在空气中于300℃下煅烧涂层4小时。最终的涂层包含196g/l的催化剂粉末和6g/l的氧化锆。
实施例
这些催化剂的钻孔芯直径为2.54cm,长度为7.62cm,放置在以下的合成气体混合物中,该气体混合物的空间速度为30000h-1,以便根据本发明的方法对它们进行测试。
500volppm氮氧化物,NO∶NO2的比例为1∶1、3∶1和1∶3
450volppm氨
5vol%氧气
1.3vol%水蒸气
其余为氮
合成气体的温度逐步由150℃增加至525℃。对于每次温度增加,都在还原催化剂的下游分析气体组成。
图3给出了新制催化剂的结果。NO/NO2的体积比此时为1∶1。
图4-6显示了已老化催化剂的实验结果。为老化该催化剂,将它们在650℃的温度下在湿热条件中储存48小时。
图4显示了NO/NO2的体积比为3∶1时的结果,图5显示了NO/NO2的体积比为1∶1时的结果,而图6显示了NO/NO2的体积比为3∶1时的结果。从这些测量的结果可以看出,已老化的催化剂比新制的催化剂具有更好的低温活性(在150-250℃之间),其中NO/NO2的体积比为1∶1。对于向氮转化的催化活性以及选择性的变化,约1∶1的值代表最佳的NO/NO2体积比。
需要的体积比可通过设置在还原催化剂上游的废气流中的氧化催化剂来调节(图1和2)。
图7-9显示了当与以下组成的合成气体混合物接触时在铂氧化催化剂下游的二氧化氮浓度的测量值:
500volppm一氧化氮NO
5vol%氧气
1.3vol%水蒸气
其余的是氮
铂催化剂以120g/l的浓度涂敷在堇青石蜂窝体上,该蜂窝体的蜂窝密度为62cm-2。催化剂的铂含量为每升蜂窝体3.2g。
这些图显示了在60000-180000h-1之间的宽范围空间速度SV中可维持所需要的NO/NO2体积比。应考虑的是,发动机所产生的废气的温度随着空间速度的增加而增加,这也随着发动机负载的增加而增加。
Claims (12)
1、一种还原内燃机所产生的稀薄废气中的氮氧化物的方法,其是在还原催化剂上使用氨来进行选择性催化还原,其中废气中所含的一部分一氧化氮在废气与氨一起从还原催化剂上通过之前被氧化为二氧化氮,
该方法的特征在于,还原催化剂包含已与过渡金属交换的沸石,而且一氧化氮的氧化使得废气在与还原催化剂接触前包含30-70vol%的二氧化氮。
2、如权利要求1所述的方法,其特征在于
所述过渡金属选自于钒、铬、铁、镍、铜、铈、镨、Tb或它们的混合物。
3、如权利要求2所述的方法,其特征在于
所述还原催化剂包含与铁、铜、铈或它们的混合物交换的沸石。
4、如权利要求3所述的方法,其特征在于
所述还原催化剂包含至少一种选自于以下组中的沸石:ZSM-5、A、β、X、Y、Ferrierite、Linde型L和八面体型沸石。
5、如权利要求4所述的方法,其特征在于
所述还原催化剂包含与铁和/或铜交换的ZSM-5沸石。
6、如权利要求1所述的方法,其特征在于
废气中一氧化氮的氧化是借助于氧化催化剂进行的。
7、如权利要求1所述的方法,其特征在于
废气中一氧化氮的氧化是借助于气体放电来进行的。
8、如前述任一权利要求所述的方法,其特征在于
选择性催化还原所需要的氨是由可水解产生氨的化合物得到的,其中所述可水解的化合物在一氧化氮的部分氧化之后但在与还原催化剂接触之前添加在废气中,然后使废气从水解催化剂上通过。
9、如权利要求8所述的方法,其特征在于
所述可水解产生氨的化合物是脲或氨基甲酸铵。
10、一种用于如权利要求9所述的方法中的还原催化剂,
其特征在于该催化剂以在蜂窝体上的涂层形式存在,该涂层包含与铁交换的沸石以及作为粘合剂的氧化锆成分。
11、如权利要求10所述的还原催化剂,其特征在于
涂层包含与铁交换的ZSM-5沸石。
12、一种制备如权利要求10或11所述的还原催化剂的方法,
其特征在于通过与铁(Ⅱ)或铁(Ⅲ)盐的固体离子交换得到已与铁交换的沸石,然后与硝酸氧锆一起悬浮在水中,以涂层形式涂敷在蜂窝体上,接着在空气中煅烧该涂层。
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CN101607209B (zh) * | 2002-11-18 | 2014-07-02 | 优美科触媒日本有限公司 | 废气净化用催化剂的制备方法与废气净化方法 |
CN101065321B (zh) * | 2004-11-29 | 2010-07-28 | 切夫里昂美国公司 | 高硅石分子筛cha |
CN101175906B (zh) * | 2005-05-17 | 2010-08-25 | 日产柴油机车工业株式会社 | 发动机的废气净化装置 |
CN101175907B (zh) * | 2005-05-17 | 2010-06-09 | 五十铃自动车株式会社 | 废气净化方法及废气净化系统 |
CN101443116B (zh) * | 2007-01-09 | 2015-07-22 | 田中贵金属工业株式会社 | 氨scr催化剂及使用该催化剂的方法 |
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CN101932803B (zh) * | 2008-01-31 | 2013-01-16 | 卡特彼勒公司 | 执行scr和egr的排气系统 |
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CN103402634A (zh) * | 2011-03-03 | 2013-11-20 | 尤米科尔股份公司及两合公司 | 用于氮氧化物的选择性催化还原的催化活性材料和催化转化器 |
CN112371164A (zh) * | 2013-03-14 | 2021-02-19 | 巴斯夫公司 | 选择性催化还原催化剂系统 |
CN107427821A (zh) * | 2015-02-20 | 2017-12-01 | 庄信万丰股份有限公司 | 双金属分子筛催化剂 |
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CN104741000A (zh) * | 2015-03-24 | 2015-07-01 | 上海华明高技术(集团)有限公司 | 一种复合床层低温scr脱硝催化剂的应用 |
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CN110461469B (zh) * | 2017-03-31 | 2022-09-13 | 庄信万丰催化剂(德国)有限公司 | 选择性催化还原催化剂 |
CN114452972A (zh) * | 2020-11-09 | 2022-05-10 | 财团法人工业技术研究院 | 触媒与其形成方法以及转换no成no2的方法 |
Also Published As
Publication number | Publication date |
---|---|
US7005116B2 (en) | 2006-02-28 |
RU2001110723A (ru) | 2003-04-10 |
US20020039550A1 (en) | 2002-04-04 |
CZ20011396A3 (cs) | 2002-04-17 |
BR0101550A (pt) | 2001-11-20 |
EP1147801B2 (de) | 2014-12-17 |
JP2002001067A (ja) | 2002-01-08 |
MXPA01003937A (es) | 2003-08-20 |
KR20010098787A (ko) | 2001-11-08 |
US6843971B2 (en) | 2005-01-18 |
AU3877501A (en) | 2001-10-25 |
JP4913953B2 (ja) | 2012-04-11 |
EP1147801B1 (de) | 2004-09-15 |
PL347148A1 (en) | 2001-11-05 |
CA2344735A1 (en) | 2001-10-22 |
EP1147801A1 (de) | 2001-10-24 |
DE10020100A1 (de) | 2001-10-31 |
ATE276035T1 (de) | 2004-10-15 |
US20050196333A1 (en) | 2005-09-08 |
DE50103588D1 (de) | 2004-10-21 |
JP5683448B2 (ja) | 2015-03-11 |
ZA200103245B (en) | 2001-10-23 |
KR100838500B1 (ko) | 2008-06-17 |
AR028350A1 (es) | 2003-05-07 |
JP2012061470A (ja) | 2012-03-29 |
BR0101550B1 (pt) | 2010-07-13 |
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