Sulfonated organosilica-aluminum phosphates as useful catalysts for acid-catalyzed reactions: Insights into the effect of synthesis parameters on the final catalyst

Abstract

The synthesis, by a sol-gel method, of organosilica-aluminum phosphates, (X)-AlPO(Y)-(Z), using three different silica precursors (X) 2-(4-chlorosulfonylphenyl)ethyltrimethoxysilane (C), 3-(mercaptopropyl)trimethoxysilane (MPTMS) or Bis[3-(triethoxysilyl)propyl]tetrasulfide (B), with varying Al/P molar ratio (Y = 3–10) and pH of the final gel (Z = 3–9), maintaining an Al/Si= 3 molar ratio, has been carried out. Materials were characterized by XRF, SEM-EDX, XRD, 1H–29Si CP, 27Al and 31P MAS NMR and nitrogen adsorption. The acidity of the solids was evaluated by TGA, XRF and XPS and their catalytic behavior in the etherification of glycerol with tert-butyl alcohol, under microwave irradiation. The solids with an Al/P molar ratio between 3 and 6, synthesized at a pH value over 3 with precursor C, exhibiting the highest values of acidity and predominantly a mesoporous character, showed the best catalytic behavior.