Condensation and structure of silicic acid in tetrahydrofuran

Silicic acid (SA) was extracted with THF from aqueous sodium metasilicate (SMS) solutions neutralized with hydrochloric acid, followed by silylation to give silylated SA from which the condensation and structure of SA in tetrahydrofuran (THF) were investigated. The degree of extraction markedly depends on SA and HCl concentrations. The condensation of 0.86 and 3.5 mol/L SA-THF solutions was followed by measuring the viscosity of the solutions at 0 and 20°C. The silylated SA was isolated as a distillate (LS) and a residue (HS) with low and high Mns (ca. 1300 and 3800) by vacuum distillation. The ratio of LS against HS decreased as a SA concentration in THF increased. In an aqueous solution, SA exists as lower molecular weight SAs compared with those in THF. SAs such as monomer, dimer, cyclic tri- and tetramer were the main components in a 0.1 mol/L aqueous solution. On the extraction with THF from an aqueous solution, SA was found to undergo condensations to form more polymerized SAs. From the THF solutions of SA concentration above 0.5 mol/L, the HS was obtained as a main component (73%) which was expected to have ladder-like structures. © 1992 John Wiley & Sons, Inc.