[en] Synthetic lamellar silica and hybrid lamellar silicas have been prepared by liquid crystal templating, template extraction and silanization. The samples have been characterized by thermogravimetric analysis (TGA), carbon analysis, spectroscopy, X-ray diffraction (XRD) and nitrogen adsorption. The XRD analyses have shown that the lamellar periodic stacking is preserved for all samples. The quantity and type of organic molecules at the silica surface have been evaluated by carbon analysis, TGA and spectroscopy. The covalent grafting of the solvent used for extraction of the initial surfactant has been highlighted by these analyses. The nitrogen
adsorption analyses have revealed three categories of pores and two types of samples. The initial lamellar silica exhibits a very low specific surface area and plate-like type of pores. The second type of samples is made up of the hybrid samples and the initial substrate from whom the surfactant has been extracted. These samples show a significantly higher specific surface area with interlamellar spaces corresponding to narrow-slit like mesopores around 4 nm. The nitrogen adsorption data analysis has highlighted the presence of micropores within the silica sheets. The difference of the specific surface is due to pore blocking by the surfactant impeding the access to nitrogen into interlamellar spaces and by the silanes covering the pores once the surface modified. The presence of micro and mesopores combined to a high BET specific surface of 612 m²/g makes these lamellar silicas interesting materials for catalysis applications.
Disciplines :
Chemistry
Author, co-author :
Toussaint, Gilles ; Université de Liège - ULiège > Chemistry Department > GreenMat
Rodriguez, Miguel Angel; Instituto de Ceramica y Vidrio, CSIC, Madrid, Spain
Cloots, Rudi ; Université de Liège - ULiège > Département de chimie (sciences) > LCIS - GreenMAT
Rubio, Juan; Instituto de Ceramica y Vidrio, CSIC, Madrid (Spain)
Rubio, Fausto; Instituto de Ceramica y Vidrio, CSIC, Madrid (Spain)
Vertruyen, Bénédicte ; Université de Liège - ULiège > Département de chimie (sciences) > Chimie inorganique structurale
Henrist, Catherine ; Université de Liège - ULiège > Département de chimie (sciences) > LCIS - GreenMAT
Language :
English
Title :
Characterization of surface and porous properties of synthetic hybrid lamellar silica
C.T. Kresge, M.E. Leonowicz, W.J. Roth, J.C. Vartuli, and J.S. Beck Ordered mesoporous molecular sieves synthesized by a liquid-crystal template mechanism Nature 359 1992 710 712
N. Nishiyama, A. Koide, Y. Egashira, and K. Ueyama Mesoporous MCM-48 membrane synthesized on a porous stainless steel support Chemical Communications 19 1998 2147
R. Burch, N. Cruise, D. Gleeson, and S.C. Tsang Surface-grafted manganese-oxo species on the walls of MCM-41 channels-a novel oxidation catalyst Chemical Communications 1996 951 952
IUPAC Reporting physisorption data for gas/solid systems with special reference to the determination of surface area and porosity Pure and Applied Chemistry 57 1985 603 619
A. Corma Studies in Surface Science and Catalysis 49 1989 49
A. Corma From microporous to mesoporous molecular sieve materials and their use in catalysis Chemical Reviews 97 1997 2373 2419
K. Lourvanij, and G. Rorrer Application of Al-pillared clay minerals as catalytic carriers for the reaction of NO with CO Applied Catalysis A: General 109 1994 147
A. Weiss Replication and evolution in inorganic systems Angewandte Chemie. International Edition 20 1981 850
Volzone C. Hydroxy-chromium smectite; influence of Cr added Clays Clay Miner. 43 1995 377
M.S. Tzou, and T.J. Pinnavaia Cromia Pillared Clay Catalysis Today 2 1988 243
McDaniel M.P., Collins K.S., Benham E.A., and Cymbaluk T.H. The activation of Phillips Cr/silica catalysts V. Stability of Cr(VI) Appl. Catal., A 335 2008 252 261
G. Toussaint, M. Brisbois, J. Grandjean, C. Henrist, and R. Cloots Hybrid lamellar silica: combined template extraction and hydrophilic silanation Journal of Colloid and Interface Science 329 2009 120 126
C. Henrist, I.G. Cano, M.A. Rodriguez, A.H. de Aza, R. Cloots, A. Rulmont, and C. Vogels Structural evolution of lamellar surfactant-silica hybrids upon calcination Composites Science and Technology 63 2003 1131
D.L. Bish, and J.E. Post Modern Powder Diffraction 1989 Mineral Society of America Washington
IUPAC Recommendations for the characterization of porous solids Pure and Applied Chemistry 66 1994 1739 1758
E.P. Barret, L.G. Joyner, and P.P. Halenda The determination of pore volume and area distributions in porous substances, I - computation from nitrogen isotherms Journal of the American Chemical Society 73 1951 373 380
S. Borsacchi, M. Geppi, L. Ricci, G. Ruggeri, and C.A. Veracini Interactions at the surface of organophilic-modified laponites: a multinuclear solid-state NMR study Langmuir 23 2007 3953 3960
K. Okuyama, Y. Soboi, K. Hirabayashi, A. Harada, A. Kumano, and M. Kaziyama Single crystals of totally synthetic amphiphiles, dialkyldimethylammonium bromides Chemistry Letters 1984 2117 2120
J.F. Lee, C.K. Lee, and L.C. Juang Size effect of exchange cation on the pore structure and surface fractility of montmorillonite Journal of Colloid and Interface Science 217 1999 172 176
Chaouri A.E., and Simonot-Grange M.H. Donnees experimentales et modelisation d'adsorption des systemes N 2 (g) / montmorillonite potassique de Camp-Berteau et N2 (g) / hydrotalcite carbonatee Thermochimica Acta 399 1999 117 123
H. Zhang, Z. Jin, and X. Wang A new synthesis of lamellar-mesostructured silica by using poly(ethylene glycol) disearate as template Materials Research Bulletin 43 2007 7
Y. Fujimoto, A. Shimojima, and K. Kuroda Surfactant-free synthesis of lamellar and wormhole-like silica mesostructures by using 1- alkynyltrimethoxysilanes Journal of Materials Chemistry 16 2006 986 994
P. Kluson, H. Luskova, O. Solcova, L. Matejova, and T. Cajthaml Lamellar micelles-mediated synthesis of nanoscale thick sheets of titania Materials Letters 61 2007 2931 2934