Abstract
Zirconia/surfactant composites were hydrothermally synthesized in aqueous sulfuric acid at 373 K using Zr(O-nPr)4 as oxide precursor and hexadecyl-trimethyl-ammonium bromide as template. Mesostructural features similar to those of MCM-41 were detected by X-ray diffractometry, with d=4.6 nm. A sample obtained from a starting mixture with Zr:S:CTAB = 2:2:1 was stable enough for removal of occluded organics. After calcination at 813 K, the d-value was 3.6 nm, the surface area 200 m2/g, and the mean pore diameter estimated by the BJH method 2.2 nm. Extended X-ray absorption fine structure analysis suggests Zr to be in a short-range structure (<4 Å) similar to that of Zr in monoclinic ZrO2. Scanning electron microscopy including energy dispersive X-ray analysis showed 1-5 μm sulfur-containing ZrO2 spheres. The material catalyzes the isomerization of n-butane to i-butane at 378 K with a steady activity in the order of magnitude of commercial sulfated ZrO2.
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C.T. Kresge, M.E. Leonowicz, W.J. Roth and J.C. Vartuli, Nature 359 (1992) 710.
A. Monnier, F. Schüth, Q. Huo, D. Kumar, D. Mongolese, R.S. Maxwell, G.D. Stucky, M. Krishnamurty, P. Petroff, A. Firouzi, M. Janicke and B.F. Chmelka, Science 261 (1993) 1299.
D.M. Antonelli and J.Y. Ying, Angew. Chem. 107 (1995) 2202; Angew. Chem. Int. Ed. Eng. 34 (1995) 2014.
Q. Huo, D. Magoless, T.E. Gier, P. Siege, R. Leon, P. Petroff, F. Schüth and G.D. Stucky, Nature 368 (1994) 317.
G. Wirnsberger, K. Gatterer, H.P. Fritzer, W. Grogger, B. Pillep, P. Behrens, M.F. Hansen and C. Bender Koch, Chem. Mater. 13 (2000) 1453.
T. Kimure, Y. Sugahara and K. Kuroda, Chem. Lett. (1997) 983.
K. Tanabe, Mater. Chem. Phys. 13 (1985) 347.
J.S. Reddy and A. Sayari, Catal. Lett. 38 (1996) 219.
U. Ciesla, S. Schacht, G.D. Stucky, K.K. Unger and F. Schüth, Angew. Chem. 108 (1996) 597; Angew. Chem. Int. Ed. Eng. 35 (1996) 541.
V.N. Romannikov, V.B. Fenelonov, E.A. Paukshtis, A.Yu. Derevyankin and V.I. Zaikovskii, Microporous Mesoporous Materials 21 (1998) 411.
U. Ciesla, M. Fröba, G. Stucky and F. Schüth, Chem. Mater. 11 (1999) 227.
F. Schüth, U. Ciesla, S. Schacht, M. Tieme, Q. Huo and G. Stucky, Mater. Res. Bull. 34 (1999) 483.
M. Lindén, J. Blanchard, S. Schacht, S.A. Schunk and F. Schüth, Chem. Mater. 11 (1999) 3002.
M. Mamak, N. Coombs and G. Ozin, Adv. Mater. 12 (2000) 198.
H.-R. Chen, J.-L. Shi, J. Yu, L.-Z. Wang and D.-S. Yan, Microporous Mesoporous Materials 39 (2000) 171.
V.I. Pârvulescu, V. Pârvulescu, U. Endruschat, C.W. Lehman, P. Grange, G. Poncelet and H. Bönnemann, Microporous Mesoporous Materials 44–45 (2001) 221.
M.S. Wong, D.M. Antonelli and J.Y. Ying, Nanostructured Materials 9 (1997) 165.
M.S. Wong and J.Y. Ying, Chem. Mater. 10 (1998) 2067.
D.M. Antonelli, Adv. Mater. 11 (1999) 487.
Y. Huang and W.M.H. Sachtler, Chem. Commun. (1997) 1181.
G. Pacheco, E. Zhao, P. Diaz Valdes, A. Garcia and J.J. Fripiat, Microporous Mesoporous Materials 21 (1999) 175.
G. Pacheco and J.J. Fripiat, J. Phys. Chem. 104 (2000) 11906.
Y.-Y. Huang, T.J. McCarthy and W.M.H. Sachtler, Appl. Catal. A: General 148 (1996) 135.
N.K. Simha, J. de Physique IV 5 (1995) C8-1121.
X. Song and A. Sayari, Catal. Rev., Sci. Eng. 38 (1996) 329.
J.B. Laizet, A.K. Søiland, J. Leglise and I.C. Duchet, Topics Catal. 10 (2000) 89.
K. Arata, M. Hino and N. Yamagata, Bull. Chem. Soc. Jpn. 63 (1990) 244.
T. Ressler, J. Synch. Rad. 5 (1998) 118.
T. Ressler, S.L. Brock, J. Wong and S.L. Suib, J. Phys. Chem. B 103 (1999) 6407.
J.J. Rehr, C.H. Booth, F. Bridges and S.I. Zabinsky, Phys. Rev. B 49 (1994) 12347.
J.D. McMullough, Acta Cryst. 1 (1967) 1948.
C.J. Howard, E.H. Kisi, R.B. Roberts and R.J. Hill, J. Am. Ceram. Soc. 73 (1990) 2828.
G. Katz, J. Am. Ceram. Soc. 54 (1971) 531.
S.J. Gregg and K.S.W. Sing, Adsorption, Surface Area and Porosity, 2nd edition (Academic Press, London, 1982).
E.P. Barrett, L.G. Joyner and P.P. Halenda, J. Am. Chem. Soc. 73 (1951) 373.
M. Selle and S. Ernst, Microporous Mesoporous Materials 27 (1999) 355.
B. Pauwels, G. Van Tendeloo, C. Thoelen, W. Van Rhijn and P. Jacobs, Adv. Mater. 13 (2001) 1317.
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Yang, X., Jentoft, F., Jentoft, R. et al. Sulfated Zirconia with Ordered Mesopores as an Active Catalyst for n-Butane Isomerization. Catalysis Letters 81, 25–31 (2002). https://doi.org/10.1023/A:1016095603350
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DOI: https://doi.org/10.1023/A:1016095603350