TiO2, SiO2 and their mixt. were impregnated with H2SO4, dried, calcinated, studied for heat resistance up to 800 degrees C and used as catalysts for esterification of HO(CH2CH2O)(3)H with AcOH at 120-140 degrees C in BuOH to resp. acetates under removal of H2O by azeotropic distn. The selectivity of the diacetate formation was the highest (90.3%) when the H2SO4/TiO2/SiO2 catalyst was used at 140 degrees C.