NOx触媒としてのCu-ZSM-5 中のCuイオンの配位構造と反応性

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1 45 Reactivity and Coordination Structure of Cu Ion in Cu-ZSM-5 for NOx Reduction Catalysts Toshitaka Tanabe, Tomoko Iijima, Koji Yokota, Akihiko Koiwai, Jiro Mizuno NOx NOx Cu-ZSM-5 Cu Cu Cu 2+ ( ESR ) Cu NOx Cu ( MAS NMR ) ESR Cu Al Cu Al Recently, the demands for catalysts capable of reducing NOx in net oxidizing atmosphere has been increasing, which promotes the research on catalysts using hydrocarbons to reduce NOx. Cu-ZSM-5 is one of the catalysts which reduce NOx with hydrocarbons in net oxidizing atmosphere. We investigated the relationship between the states of copper in Cu-ZSM-5 and its reactivity, and also the change in the state of Cu with thermal deactivation. The results of infrared absorption spectroscopy of adsorbed NH 3 and electron spin resonance (ESR) of Cu 2+ show that the states of copper in Cu-ZSM-5 vary with Cu loading. It was clarified by comparison between the states of copper and the activity of NOx reduction of Cu-ZSM-5 that the active sites for NOx reduction were Cu ions at the ion exchange sites in zeolite and that Brønsted acid sites did not contribute to the NOx reduction directly. From solid state nuclear magnetic resonance and ESR results, the thermal deactivation was found to occur by the migration of copper ions which was induced by the dealumination of zeolite, not by the aggregation of copper ion. Ab initio molecular orbital calculation on the model of zeolites suggested that the dealumination was caused by the Brønsted acid sites. Cu-ZSM-5 NOx C 3 H 6 IR ESR NMRAl R&D Vol. 30 No. 1 ( )

2 46 NOx NOx NOx NOx NOx NOx NOx ZSM-5 Cu-ZSM-5 NOx 1988 NOx NOx NOx NOx NOx Cu-ZSM-5 Cu-ZSM-5 NH 4 -ZSM-5 ( SiO 2 /Al 2 O 3 = ) ph = 11 [ Cu(NH 3 ) 4 ] 2+ NH 4 -ZSM L/min Cu Cu Cu/2Al = ( Cu : wt% ) NH 3 H + NH + 4 Cu 2+ NH 3 IR Cu Cu NH 4 Z + Cu 2+ = Cu Z + 2NH 4 ( Z NH + 4 Cu 2+ IR IR R&D Vol. 30 No. 1 ( )

3 Torr ( 1Torr = 133.3Pa ) IR Cu-ZSM-5 IR Fig cm 1 ( H + ) NH cm 1 ( Cu 2+ ) NH 3 Cu = Cu Cu Fig. 2 Cu Cu 2+ Cu 2 Cu Cu/2Al 1 10% Cu 90 ESR Cu 2 3d 9 S = 1/2 ESRESR 10mg Bruker ESP300E X 9.5GHz ESR Cu 2+ Cu 2+ IR spectra of adsorbed NH 3 on Cu-ZSM-5. The absorption band at 1620cm 1 corresponds to the deformation band of NH 3 on the Cu ion and that at 1460cm 1 corresponds to the deformation band of NH 4 + on the Brønsted acid site. Cu loading dependence of the amount of the Brønsted acid sites in Cu-ZSM-5. The amount of acid sites is normalized to acid sites of NH 4 -ZSM-5 so that the amount of acid sites in NH 4 -ZSM-5 ( Cu/2Al = 0 ) is 100%. The broken line corresponds to the case of copper exchange with NH 4 + as Cu 2+ and the dash-dotted line corresponds to the case of copper exchange as monovalent cation like Cu(OH) +. R&D Vol. 30 No. 1 ( )

4 48 ESR Cu 2+ Cu Cu 2+ Cu 2+ Cu Cu 2+ Cu/2Al 0.75 Cu 2+ Cu/2Al 1.5 IR ESR Cu Cu Cu Cu 2+ ESR Cu Cu 2+ Cu Cu 2+ Cu/2Al Cu 2+ ESR Cu + Cu/2Al 1.5 Cu 2+ Cu SEM CuO N(B 0 ) = N(B) Cu 2+ N(Cu 2+ ) Cu + N(Cu + ) CuO N(CuO) Cu N(Cu) N(Cu) = N(Cu 2+ ) + N(Cu + ) + N(CuO) N(B 0 ) N(B) = N(Cu 2+ ) + N(Cu + ) N(Cu) N(B 0 ) N(Cu 2+ ) N(B) ESR IR 2 N(Cu + ) N(CuO) Cu Cu Fig. 4 IR ESR Cu Cu Cu Cu-ZSM-5 NOx Cu ( Cu 2+ + Cu + ) Cu No.1 Cu loading dependence of Cu 2+ concentration in Cu-ZSM-5. Cu 2+ concentration is estimated from ESR spectra. The straight line corresponds to the case in which all loaded Cu are exchanged with NH 4 + as isolated Cu 2+. The relationship between the amounts of Cu species in Cu-ZSM-5 and Cu loading. The straight line corresponds to the case in which all loaded Cu are exchanged with NH 4 + as isolated Cu 2+. R&D Vol. 30 No. 1 ( )

5 h NOx Cu ( Cu 2+ + Cu + ) Cu-ZSM-5 NOx Cu ( Cu 2+ + Cu + ) Cu NOx 2 ( Cu 2+ + Cu + ) NOx NOx Cu 2+ Cu + Cu-ZSM-5 Table 1 No.2 5 Cu-ZSM-5 NOx Table 1 No h Cu Cu/2Al = NOx MAS NMR ESR Cu 29 Si 27 Al MAS NMR 29 Si MAS NMR The relationship between NOx conversion and total copper ion concentration ( Cu + + Cu 2+ ). Total copper ion concentration was estimated from ESR and IR results as shown in Fig. 4. Composition of simulated exhaust gas. Gas concentration/% No.1 No.2 CO H C 3 H NO O CO H 2 O 3 3 N 2 Balance Balance Temperature dependence of NOx conversions in the reaction of simulated exhaust gas ( Table 1 : No.1 ) with Cu-ZSM-5 ; a) unheated, b) heated at 600, c) 700 and d) 800, for 5 hours in simulated exhaust gas ( Table 1 : No.2 ). R&D Vol. 30 No. 1 ( )

6 50 27 Al and 29 Si MAS NMR spectra of Cu-ZSM-5 heated for 5 hours in simulated exhaust gas ( Table 1 : No.2 ) ; a) unheated, b) heated at 600, c) 700 and d) 800. Concentration of Cu 2+ in Cu-ZSM-5 estimated from ESR spectrum. Heating temperature / Cu 2+ concentration / g 1 Unheated ppm 107ppm Si Al Si Si Al Si 107ppm 27 Al 70ppm Al tetrahedral Al ESR Cu 2+ Cu 2+ Cu Cu 2+ Cu Cu ESR ESR spectra of Cu 2+ in Cu-ZSM-5 heated for 5 hours in simulated exhaust gas ( Table 1 : No.2 ) ; a) unheated, b) heated at 600, c) 700 and d) 800. Each sample was dehydrated by evacuation at 500 for 2 hours before measurement and ESR spectra were measured at room temperature. Cu 2+ Cu Cu-ZSM-5 Cu 2+ ESR R&D Vol. 30 No. 1 ( )

7 Torr 800 Bruker Simfonia Cu 2+ Cu 2+ Cu NO C 3 H 6 ESR 10Torr NO ESR Torr NO The ESR spectra of the unheated Cu-ZSM-5 measured at room temperature after the dehydration by evacuation at 500 for 1 hour ; (a) experimental, (b) simulated. The ESR spectra of the Cu-ZSM-5 heated at 800 for 5 hours in the simulated exhaust gas ( Table 1 : No.2 ) measured at room temperature after the dehydration by evacuation at 500 for 1 hour ; (a) experimental, (b) simulated. ESR parameters used in spectrum simulation. g g A /mt A /mt Species a ( unheated and heated at 600 ) Species b ( unheated and heated at 600 ) Species c ( heated at 800 ) R&D Vol. 30 No. 1 ( )

8 52 ESR spectra of Cu-ZSM-5 after the introduction of 10 Torr of NO at room temperature. For the dehydration the sample was evacuated at 500 for 2 hours ; (A) spectra of the unheated sample, (a) after the dehydration, (b) just after the introduction of NO, (c) 1 min. after the introduction and (d) 5 min. after the introduction, (B) spectra of the sample heated at 800 for 5 hours in the simulated exhaust gas ( Table 1 : No.2 ), (e) after the dehydration, (f) just after the introduction of NO, (g) 1 min. after the introduction and (h) after evacuation at room temperature. NO Cu 2+ Cu 2+ Cu 2+ NO Cu 2+ NO NO NO Cu Cu 2+ Cu + Cu R&D Vol. 30 No. 1 ( )

9 53 ESR spectra of Cu-ZSM-5 after the introduction of 10Torr of C 3 H 6. For the dehydration the sample was evacuated at 500 for 2 hours ; (A) spectra for the unheated sample, (a) after the dehydration, (b) just after the introduction of C 3 H 6, (c) 1 min. after the introduction and (d) 13 min. after the introduction, (B) spectra for the sample heated at 800 for 5 hours in simulated exhaust gas ( Table 1 : No.2 ), (e) after the dehydration, (f) just after the introduction of C 3 H 6, (g) after evacuation at room temperature and (h) just after the introduction of C 3 H 6. Cu Cu 2+ 10Torr C 3 H 6 ESR NO Torr 2 C 3 H 6 Cu 2+ g = 2.00 Cu 2+ C 3 H 6 C 3 H 6 Cu 2+ Cu 2+ Cu + g = 2.00 C 3 H C 3 H 6 ESR C 3 H 6 C 3 H 6 ESR Cu 2+ NO C 3 H ESR ( g c A c Table 3 ) L. KevanCu-ZSM-5 Cu 2+ ESR 5 Cu Cu 2+ 5 R&D Vol. 30 No. 1 ( )

10 54 Cu-ZSM-5 Cu MAS NMR Al Cu Cu Cu-ZSM 5 Al Al H + S. Beran IBM3090 Gaussian86 S. Beran STO-3G 3-21G Li Na Al-O Al-O Al The model of zeolite used in the ab-initio molecular orbital calculation. Schematic representation of the (100) face of ZSM-5 showing the 10-membered ring accessible to adsorbates and smaller 5-membered rings inaccessible to adsorbates. The relationship between electronegativity and bond order or bond length of Al-O. R&D Vol. 30 No. 1 ( )

11 55 Cu-ZSM-5 NOx Cu-ZSM-5 Cu Cu NOx Cu CuCu Cu Al 1),, : No.10,, (1990), 181, 2) Iwamoto, M., et al. : J. Chem. Soc., Faraday Trans. 1, (1981), ), : ) Held, W., König, A., Richter, T. and Puppe, L. : SAE Tech. Pap. Ser., No , (1990), 8p. 5),,,, :, (1990), 430 6) Misono, M. and Kondo, K. : Chem. Lett., (1991), ) Yogo, K., Tanaka, S., Ihara, M., Hishiki, T. and Kikuchi, K. : Chem. Lett., (1992), ) Sato, S., Hirabayashi, H., Yahiro, H., Mizuno, N. and Iwamoto, M. : Catal. Lett., (1992), 193 9) Kintaichi, Y., Hamada, H., Tabata, M., Sasaki, M. and Ito, T. : Catal. Lett., (1990), ) Hamada, H., Kintaichi, Y., Sasaki, M., Ito, T. and Tabata, M. : Appl. Catal., (1991), L15 11) Zhang, G., Yamazaki, T., Kawakami, H. and Suzuki, T. : Appl. Catal. B, (1992), L15 12) Hirabayashi, H., Yahiro, H., Mizuno, N. and Iwamoto, M. : Chem. Lett., (1992), ) Obuchi, A., Ohi, A., Nakamura, M., Ogata, A., Mizuno, K. and Obuchi, H. : Appl. Catal. B, (1993), 71 14) Ansell, G. P., Diwell, A. F., Golunski, A. F., Hayes, J. W., Rajaram, R. R., Truex, T. J. and Walker, A. P. : Appl. Catal. B, (1993), 81 15) Tanaka, T., Okuhara, T. and Misono, M. : Appl. Catal. B, (1994), L1 16) Burch, R., Millington, P. J. and Walker, A. P. : Appl. Catal. B, (1994), 65 17),,, : 70, (1992), ),,,, : 65 (I), (1993), ) Howard, J. and Nicol, J. M. : J. Chem. Soc., Faraday Trans. 1, -6(1989), ),,, : 70, (1992), ),,,,,, : 70, (1992), ) Engerhaldt, G. and Michel, D. : High-Resolution Solid-State NMR of Silicates and Zeolites, (1987), 301, John Wiley & Sons 23) Engerhaldt, G. and Michel, D. : High-Resolution Solid-State NMR of Silicates and Zeolites, (1987), 261, John Wiley & Sons 24) Michel, W. and Kevan, L. : J. Phys. Chem., -15(1987), ),,,,, :, No.11 (1989), ) Beran, S. : J. Phys. Chem., -3(1988), 766 R&D Vol. 30 No. 1 ( )

12 56 R&D Vol. 30 No. 1 ( )

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