Heteropoly acids (molybdophosphoric acid and tungstophosphoric acid) of different wt.% (5-20 wt.%) were intercalated in Zn-Al hydrotalcite-like-compounds by indirect intercalation via terephthalate route and the materials were characterized by PXRD, FTIR, BET, acid sites, etc. PXRD reveals intercalation of MPA and TPA species, which is further corroborated by the presence of these Keggin ions by FTIR. The catalytic activity of the prepared catalysts was tested for the liquid phase esterification of acetic acid. using n-butanol under autogenous condition. The effect of various reaction parameters such as molar ratio of the reactants, temperature, time and catalyst dose, etc. on the conversion of acetic acid was studied and the findings are discussed. The 15 wt.% MPA intercalated sample shows highest conversion (84.15%) with 100% selectivity for n-butyl acetate. (c) 2006 Elsevier B.V. All rights reserved.