Poly(ethylene oxide)-based surfactants as templates for the synthesis of mesoporous silica materials.

Various mesoporous silica solids were prepared by using poly(ethylene oxide)-based surfactants as templates in a neutral, fluoride, or moderately acidic medium, and their properties examined by different physical techniques. Precipitation in an acid or neutral medium provided materials of pore size in between those of micropores and mesopores irrespective of the molecular size of the surfactant. On the other hand, syntheses in a fluoride-containing medium yielded mesoporous materials with pore diameters over the range 36-84 A that increased with increasing surfactant size. All materials possessed specific surface areas above 650 m(2)g(-1) and high pore volumes-particularly those obtained in a fluorinated medium. The conditions used in the syntheses and the fact that all produced highly disordered porous materials suggest that their mechanism of formation is essentially of the N(0)I(0) neutral type. The materials obtained in the presence of fluoride ion, which promote the condensation of siliceous species, retain greater amounts of surfactant and exhibit increased cross-linking and decreased particle sizes, which results in textural mesoporosity.

Synthesis and Characterization of Basic Catalysts Based on Sodium-Magnesium Mixed Phosphates and Their Use in the Conversion of 2-Hexanol.

Various catalysts consisting of sodium-magnesium mixed orthophosphates were synthesized and characterized in structural terms using X-ray diffraction, thermogravimetric analysis, differential thermal analysis, diffuse reflectance infrared spectroscopy, and solid-state (31)P NMR spectroscopy. In addition, the surface properties of the solids were determined from N(2) adsorption-desorption isotherms and their chemical properties characterized with various titrants. One of the solids obtained consists of NaMgPO(4)/Mg(2)P(2)O(7) and the rest of NaMgPO(4)/MgO. Their surface chemical properties vary depending on the particular synthetic procedure used; thus, the NaMgPO(4)/MgO systems exhibit similar populations of acid and basic sites, whereas the NaMgPO(4)/Mg(2)P(2)O(7) systems contain many more acid sites than basic sites. All the solids obtained exhibit substantial dehydrogenating activity in the conversion of gaseous 2-hexanol; in fact, some of the NaMgPO(4)/MgO systems are even more active and selective than a MgO solid tested under identical reaction conditions. Copyright 2001 Academic Press.

Activity of Basic Catalysts in the Meerwein-Ponndorf-Verley Reaction of Benzaldehyde with Ethanol.

The Meerwein-Ponndorf-Verley (MPV) reaction of benzaldehyde with ethanol in the liquid phase in the presence of basic catalysts consisting of magnesium oxide, calcium oxide, and mixed oxides obtained by calcination of layered double hydroxides, was studied. The catalysts were characterized using various techniques including X-ray diffraction and gas adsorption (viz nitrogen physisorption to determine textural properties and carbon dioxide chemisorption to elucidate surface basic properties). The catalyst consisting of calcium oxide, which was that possessing the highest density of basic sites, was found to be the most active in the process; the MPV reaction was accompanied by two other, competing reactions (viz aldol condensation and the Tishchenko cross-reaction). The MPV reaction of benzaldehyde with other alcohols was also examined, the highest conversion being obtained with secondary alcohols as hydrogen sources. Copyright 2001 Academic Press.