A Two-Component, Non-Aqueous Route to Silica Gel

A new means for generating silica gel has been developed. Simple two component systems comprising tetraalkoxysilanes and strong carboxylic acids such as formic acid can react rapidly to give transparent monolithic gels. The acid serves as solvent, water source, and catalyst for both hydrolysis and condensation. Water need not be present as an initial reactant; it is generated in situ during the reaction. The gelation reaction is at least two orders of magnitude faster than those conducted in conventional acid-catalyzed aqueous systems at comparable pH*. Kinetic evidence indicates a lowering of the activation energy of condensation reactions, believed to be associated with reaction of silyl carboxytates and silanol groups. Physical properties of the dry gels such as bulk density more closely resemble conventional acid-catalyzed gels than those associated with other rapidly gelling systems. Dry gels often exhibit porosity so fine that nitrogen (at 77 degrees K) is not absorbed at significant rates. Independent evidence of porosity arises from comparison of skeletal and bulk densities, sample immersion in water and adsorption isotherms of CQ.