Abstract: Colloidal suspensions of silsesquioxanes of the general formula RSiO.sub.3/2, wherein R is a hydrocarbon or a substituted hydrocarbon radical containing from 1 to 7 carbon atoms, are prepared by the emulsion polymerization of a silane of general formula RSi(OR').sub.3 in a water surfactant mixture with a pH greater than or equal to 8 where the resulting silsesquioxanes has an average particle size of about 10 to 1000 angstroms. The surfactant is an organic carboxylic acid having greater than eight carbon atoms or a water soluble salt of the same carboxylic acids.