A convenient synthesis of silylated silica xerogels

Treated silica xerogels with controlled porosity and surface area were prepared by the in situ treatment of hydrogels with hexamethyldisiloxane or alkylchlorosilanes in the presence of isopropyl alcohol. The resulting hydrogels were hydrophobic and readily transferred to nonpolar organic solvents upon contact. The surface area and porosity of the xerogel were controlled by varying the pH, time, and temperature used to polymerize the hydrogel prior to treatment. In general, the surface area decreased with increases in aging time or temperature, whereas the total pore volume and pore size increased. Silylation of the hydrogel in the aqueous phase retains the structure of the hydrogel and permits isolation with minimum structure collapse. By using this technique, silylated xerogels with surface areas ranging from 200 to >700 m(2)/g and pore volumes of 1.5 to 3.8 cm(3)/g were obtained.