Esterification of acetic acid with sec-butanol to produce sec-butyl acetate has been systematically carried out by using mesoporous (3–9 nm size) aluminosilicate (meso-AS) catalysts (surface area 327–578 m2 g−1) derived from Na-montmorillonite by controlled HCl acid activation. High catalytic activity up to 89% conversion with nearly 100% selectivity towards sec-butyl acetate is observed. The effect of reaction temperature, mole ratio of reactants and catalyst concentration on esterification reactions were studied. The catalyst could be recycled and reused several times without significant loss of their catalytic activities. The catalysts were characterized by pyridine adsorbed FT-IR, XRD, SEM-EDX, MAS-NMR, surface area (BET) and TPD analysis.