A high-yield reproducible synthesis of MCM-48 starting from fumed silica

被引:60
作者
Collart, O
Van Der Voort, P
Vansant, EF
Desplantier, D
Galarneau, A
Di Renzo, F
Fajula, F
机构
[1] Univ Instelling Antwerp, Lab Adsorpt & Catalysis, B-2610 Antwerp, Belgium
[2] Ecole Natl Super Chim Montpellier, Lab Mat Catalyt & Catalyse Chim Organ, F-34296 Montpellier 5, France
关键词
Condensation - Gels - Hydrothermal synthesis - Infrared radiation - pH - Pore size - Scanning electron microscopy - Silica - Solubility - Sorption - Surface active agents - X ray diffraction analysis;
D O I
10.1021/jp013037u
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
A new synthesis pathway for MCM-48 is developed using fumed silica as the silicate source and a Gemini surfactant (GEM 16-12-16) as the surface directing agent. Different synthesis parameters have been optimized in order to obtain a highly ordered mesostructure. The determining factor in the stabilization of the final structure is proven to be a double post-synthesis hydrothermal treatment. This treatment, performed successively in a minimum of pure water at 403 K, reduces the pH of the get, allowing a better condensation of the silicate structure. Other parameters of importance are the OH-/Si ratio, the gelation time, and the synthesis temperature, influencing the solubility of the fumed silica, the condensation and the structuring of the silicate framework, and (lie pore diameter, respectively. The synthesis temperature has also a positive effect on the particle dimension, producing uniform grains of 4-5 mum. The optimized parameters (3-day gelation time followed by two consecutive post-synthesis hydrothermal treatments) give a highly reproducible synthesis, with a high silica yield (70-75%). The synthesized samples have been characterized using XRD, N-2 sorption isotherms, SEM, and infrared (DRIFT) measurements.
引用
收藏
页码:12771 / 12777
页数:7
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