Abstract.
After recalling a few advances made by 1H, 29Si, and 27Al on the understanding of hydro-desulfuration (HDS) molybdenum-based catalysts supported on amorphous oxides, we critically evaluate the potential of 95Mo magic-angle spinning nuclear magnetic resonance (MAS NMR) for gaining further insight into the structure of uncalcined precursors and sulfided HDS catalysts. It is shown that when performed at a very high field (19.6 T), it is indeed sensitive to the nature of the molybdenum–support interaction. In particular, a wide distribution of the molybdenum environment present on the surface was evidenced. However, the possibility to characterize sulfided catalysts by 95Mo MAS NMR appeared still an unmet challenge.
Similar content being viewed by others
References
Somorjai, G.A., McCrea, K.R., Zhu, J.: Top. Catal. 18, 157–166 (2002)
Hammer, B.: Top. Catal. 37, 3–16 (2006)
Rao, C.N.R., Kulkarni, G.U., Thomas, P.J., Edwards, P.P.: Chem. Eur. J. 8, 28–35 (2002)
Remediakis, I.N., Lopez, N., Norskov, J.K.: Appl. Catal. A 291, 13–20 (2005)
Topsoe, H., Hinnemann, B., Norskov, J.K., Lauritsen, J.V., Besenbacher, F., Hansen, P.L., Hytoft, G., Egeberg, R.G., Knudsen, K.G.: Catal. Today 107–108, 12–22 (2005)
Song, C.: Catal. Today 86, 211–263 (2003)
Harlé, V., Rouleau, L., Kressmann, S.G.D.: Patent No. EP 1364707. 2003
Bell, A.T., Pines, A. (eds.): NMR Techniques in Catalysis. Marcel Dekker, New York (1994)
d'Espinose de Lacaillerie, J.-B., Barberon, F., Romanenko, K.V., Lapina, O.B., Polles, L.L., Gautier, R., Gan, Z.: J. Phys. Chem. B 109, 14033–14042 (2005)
Isobe, T., Watanabe, T., d'Espinose de la Caillerie, J.-B., Legrand, A.P., Massiot, D.: J. Colloid Interface Sci. 261, 320–324 (2003)
Carrier, X., Lambert, J.F., Che, M.: J. Am. Chem. Soc. 119, 10137–10146 (1997)
Mertens de Wilmar, D., Clause, O., d'Espinose de la Caillerie, J.-B.: J. Phys. Chem. B 102, 7023–7027 (1998)
Fischer, L., Harle, V., Kasztelan, S., d'Espinose de la Caillerie, J.-B.: Solid State Nucl. Magn. Reson. 16, 85–91 (2000)
Sanchez, N.A., Saniger, J.M., d'Espinose de la Caillerie, J.-B., Blumenfeld, A.L., Fripiat, J.J.: J. Catal. 201, 80–88 (2001)
Fitzgerald, J.J., Piedra, G., Dec, S.F., Seger, M., Maciel, G.E.: J. Am. Chem. Soc. 119, 7832–7842 (1997)
Liu, C.C., Maciel, G.E.: J. Am. Chem. Soc. 118, 5103–5119 (1996)
Grünberg, B., Emmler, T., Gedat, E., Shenderovich, I., Findenegg, G.H., Limbach, H.-H., Buntkowsky, G.: Chem. Eur. J. 10, 5689–5696 (2004)
d'Espinose de la Caillerie, J.-B., Aimeur, M.R., Kortobi, Y.E., Legrand, A.P.: J. Colloid Interface Sci. 194, 434–439 (1997)
Trebosc, J., Wiench, J.W., Huh, S., Lin, V.S.-Y., Pruski, M.: J. Am. Chem. Soc. 127, 3057–3068 (2005)
Leonardelli, S., Facchini, L., Fretigny, C., Tougne, P., Legrand, A.P.: J. Am. Chem. Soc. 114, 6412–6418 (1992)
Crepeau, G., Montouillout, V., Vimont, A., Mariey, L., Cseri, T., Mauge, F.: J. Phys. Chem. B 110, 15172–15185 (2006)
Vega, A.J.: Solid-State Nucl. Magn. Reson. 1, 17–32 (1992)
Kautt, W.D., Kruger, H., Lutz, O., Maier, H., Nolle, A.: Z. Naturforsch. A: Phys. Sci. 31, 351–356 (1976)
Lynch, G.F., Segel, S.L.: Can. J. Phys. 50, 567–572 (1972)
Nolle, A.: Z. Phys. A 280, 231–234 (1977)
Edwards, J.C., Zubieta, J., Shaikh, S.N., Chen, Q., Bank, S., Ellis, P.D.: Inorg. Chem. 29, 3381–3393 (1990)
Eichele, K., Wasylishen, R.E., Nelson, J.H.: J. Phys. Chem. A 101, 5463–5468 (1997)
Proust, A., Thouvenot, R., Roh, S.G., Yoo, J.K., Gouzerh, P.: Inorg. Chem. 34, 4106–4112 (1995)
Bastow, T.J.: Solid State Nucl. Magn. Reson. 12, 191–199 (1998)
Bastow, T.J.: Solid State Nucl. Magn. Reson. 23, 116–118 (2003)
Machida, N., Eckert, H.: Solid-State Ionics 107, 255–268 (1998)
Mastikhin, V.M., Lapina, O.B., Maximovskaya, R.I.: Chem. Phys. Lett. 148, 413–416 (1988)
Edwards, J.C., Adams, R.D., Ellis, P.D.: J. Am. Chem. Soc. 112, 8349–8364 (1990)
Edwards, J.C., Ellis, P.D.: Langmuir 7, 2117–2134 (1991)
Han, O.H., Lin, C.Y., Haller, G.L.: Catal. Lett. 14, 1–9 (1992)
Han, O.H., Lin, C.Y., Sustache, N., McMillan, M., Carruthers, J.D., Zilm, K.W., Haller, G.L.: Appl. Catal. A 98, 195–210 (1993)
Harris, R.K., Becker, E.D., De Menezes, S.M.C., Goodfellow, R., Granger, P.: Pure Appl. Chem. 73, 1795–1818 (2001)
Smith, M.E.: Annu. Rep. NMR Spectrosc. 43, 121–175 (2001)
Bryce, D.L., Wasylishen, R.E.: Phys. Chem. Chem. Phys. 4, 3591–3600 (2002)
Forgeron, M.A.M., Wasylishen, R.E.: J. Am. Chem. Soc. 128, 7817–7827 (2006)
Vosegaard, T., Skibsted, J., Jakobsen, H.J.: J. Phys. Chem. A 103, 9144–9149 (1999)
Hove, A.R., Bildsoe, H., Skibsted, J., Brorson, M., Jakobsen, H.J.: Inorg. Chem. 45, 10873–10881 (2006)
Blaha, P., Schwarz, K., Madsen, G.K.H., Kvasnicka, D., Luitz, J.: WIEN2k, An Augmented Plane Wave plus Local Orbitals Program for Calculating Crystal Properties. Technische Universität Wien, Wien, Austria (2001)
Massiot, D., Fayon, F., Capron, M., King, I., Le Calve, S., Alonso, B., Durand, J.O., Bujoli, B., Gan, Z.H., Hoatson, G.: Magn. Reson. Chem. 40, 70–76 (2002)
Reichelt, W., Weber, T., Sohnel, T., Dabritz, C.: Z. Anorg. Allg. Chem. 626, 2020–2027 (2000)
Plazenet, G., Payen, E., Lynch, J., Rebours, B.: J. Phys. Chem. B 106, 7013–7028 (2002)
d'Espinose de la Caillerie, J.-B., Kermarec, M., Clause, O.: J. Phys. Chem. 99, 17273–17281 (1995)
Carrier, X., Lambert, J.-F., Kuba, S., Knozinger, H., Che, M.: J. Mol. Struct. 656, 231–238 (2003)
Author information
Authors and Affiliations
Additional information
Authors' address: Jean-Baptiste d'Espinose de Lacaillerie, PPMD, Ecole Supérieure de Physique et de Chimie Industrielles, 10 rue Vauquelin, Paris 75231, Cedex 05, France
Rights and permissions
About this article
Cite this article
d'Espinose de Lacaillerie, JB., Gan, Z. MAS NMR Strategies for the Characterization of Supported Molybdenum Catalysts. Appl Magn Reson 32, 499–511 (2007). https://doi.org/10.1007/s00723-007-0033-0
Received:
Issue Date:
DOI: https://doi.org/10.1007/s00723-007-0033-0