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MAS NMR Strategies for the Characterization of Supported Molybdenum Catalysts

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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.

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References

  • Somorjai, G.A., McCrea, K.R., Zhu, J.: Top. Catal. 18, 157–166 (2002)

    Article  Google Scholar 

  • Hammer, B.: Top. Catal. 37, 3–16 (2006)

    Article  Google Scholar 

  • Rao, C.N.R., Kulkarni, G.U., Thomas, P.J., Edwards, P.P.: Chem. Eur. J. 8, 28–35 (2002)

    Article  Google Scholar 

  • Remediakis, I.N., Lopez, N., Norskov, J.K.: Appl. Catal. A 291, 13–20 (2005)

    Article  Google Scholar 

  • 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)

    Article  Google Scholar 

  • Song, C.: Catal. Today 86, 211–263 (2003)

    Article  Google Scholar 

  • 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)

    Google Scholar 

  • 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)

    Article  Google Scholar 

  • Isobe, T., Watanabe, T., d'Espinose de la Caillerie, J.-B., Legrand, A.P., Massiot, D.: J. Colloid Interface Sci. 261, 320–324 (2003)

    Article  Google Scholar 

  • Carrier, X., Lambert, J.F., Che, M.: J. Am. Chem. Soc. 119, 10137–10146 (1997)

    Article  Google Scholar 

  • Mertens de Wilmar, D., Clause, O., d'Espinose de la Caillerie, J.-B.: J. Phys. Chem. B 102, 7023–7027 (1998)

    Article  Google Scholar 

  • Fischer, L., Harle, V., Kasztelan, S., d'Espinose de la Caillerie, J.-B.: Solid State Nucl. Magn. Reson. 16, 85–91 (2000)

    Article  Google Scholar 

  • 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)

    Article  Google Scholar 

  • Fitzgerald, J.J., Piedra, G., Dec, S.F., Seger, M., Maciel, G.E.: J. Am. Chem. Soc. 119, 7832–7842 (1997)

    Article  Google Scholar 

  • Liu, C.C., Maciel, G.E.: J. Am. Chem. Soc. 118, 5103–5119 (1996)

    Article  Google Scholar 

  • Grünberg, B., Emmler, T., Gedat, E., Shenderovich, I., Findenegg, G.H., Limbach, H.-H., Buntkowsky, G.: Chem. Eur. J. 10, 5689–5696 (2004)

    Article  Google Scholar 

  • d'Espinose de la Caillerie, J.-B., Aimeur, M.R., Kortobi, Y.E., Legrand, A.P.: J. Colloid Interface Sci. 194, 434–439 (1997)

    Article  Google Scholar 

  • Trebosc, J., Wiench, J.W., Huh, S., Lin, V.S.-Y., Pruski, M.: J. Am. Chem. Soc. 127, 3057–3068 (2005)

    Article  Google Scholar 

  • Leonardelli, S., Facchini, L., Fretigny, C., Tougne, P., Legrand, A.P.: J. Am. Chem. Soc. 114, 6412–6418 (1992)

    Article  Google Scholar 

  • Crepeau, G., Montouillout, V., Vimont, A., Mariey, L., Cseri, T., Mauge, F.: J. Phys. Chem. B 110, 15172–15185 (2006)

    Article  Google Scholar 

  • Vega, A.J.: Solid-State Nucl. Magn. Reson. 1, 17–32 (1992)

    Article  Google Scholar 

  • Kautt, W.D., Kruger, H., Lutz, O., Maier, H., Nolle, A.: Z. Naturforsch. A: Phys. Sci. 31, 351–356 (1976)

    ADS  Google Scholar 

  • Lynch, G.F., Segel, S.L.: Can. J. Phys. 50, 567–572 (1972)

    ADS  Google Scholar 

  • Nolle, A.: Z. Phys. A 280, 231–234 (1977)

    Article  Google Scholar 

  • Edwards, J.C., Zubieta, J., Shaikh, S.N., Chen, Q., Bank, S., Ellis, P.D.: Inorg. Chem. 29, 3381–3393 (1990)

    Article  Google Scholar 

  • Eichele, K., Wasylishen, R.E., Nelson, J.H.: J. Phys. Chem. A 101, 5463–5468 (1997)

    Article  Google Scholar 

  • Proust, A., Thouvenot, R., Roh, S.G., Yoo, J.K., Gouzerh, P.: Inorg. Chem. 34, 4106–4112 (1995)

    Article  Google Scholar 

  • Bastow, T.J.: Solid State Nucl. Magn. Reson. 12, 191–199 (1998)

    Article  Google Scholar 

  • Bastow, T.J.: Solid State Nucl. Magn. Reson. 23, 116–118 (2003)

    Article  Google Scholar 

  • Machida, N., Eckert, H.: Solid-State Ionics 107, 255–268 (1998)

    Article  Google Scholar 

  • Mastikhin, V.M., Lapina, O.B., Maximovskaya, R.I.: Chem. Phys. Lett. 148, 413–416 (1988)

    Article  ADS  Google Scholar 

  • Edwards, J.C., Adams, R.D., Ellis, P.D.: J. Am. Chem. Soc. 112, 8349–8364 (1990)

    Article  Google Scholar 

  • Edwards, J.C., Ellis, P.D.: Langmuir 7, 2117–2134 (1991)

    Article  Google Scholar 

  • Han, O.H., Lin, C.Y., Haller, G.L.: Catal. Lett. 14, 1–9 (1992)

    Article  ADS  Google Scholar 

  • 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)

    Article  Google Scholar 

  • Harris, R.K., Becker, E.D., De Menezes, S.M.C., Goodfellow, R., Granger, P.: Pure Appl. Chem. 73, 1795–1818 (2001)

    Article  Google Scholar 

  • Smith, M.E.: Annu. Rep. NMR Spectrosc. 43, 121–175 (2001)

    Article  Google Scholar 

  • Bryce, D.L., Wasylishen, R.E.: Phys. Chem. Chem. Phys. 4, 3591–3600 (2002)

    Article  Google Scholar 

  • Forgeron, M.A.M., Wasylishen, R.E.: J. Am. Chem. Soc. 128, 7817–7827 (2006)

    Article  Google Scholar 

  • Vosegaard, T., Skibsted, J., Jakobsen, H.J.: J. Phys. Chem. A 103, 9144–9149 (1999)

    Article  Google Scholar 

  • Hove, A.R., Bildsoe, H., Skibsted, J., Brorson, M., Jakobsen, H.J.: Inorg. Chem. 45, 10873–10881 (2006)

    Article  Google Scholar 

  • 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)

    Google Scholar 

  • 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)

    Article  Google Scholar 

  • Reichelt, W., Weber, T., Sohnel, T., Dabritz, C.: Z. Anorg. Allg. Chem. 626, 2020–2027 (2000)

    Article  Google Scholar 

  • Plazenet, G., Payen, E., Lynch, J., Rebours, B.: J. Phys. Chem. B 106, 7013–7028 (2002)

    Article  Google Scholar 

  • d'Espinose de la Caillerie, J.-B., Kermarec, M., Clause, O.: J. Phys. Chem. 99, 17273–17281 (1995)

    Article  Google Scholar 

  • Carrier, X., Lambert, J.-F., Kuba, S., Knozinger, H., Che, M.: J. Mol. Struct. 656, 231–238 (2003)

    Article  ADS  Google Scholar 

Download references

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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

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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

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  • DOI: https://doi.org/10.1007/s00723-007-0033-0

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