In this work, proper operation and improved control of a heterogeneous azeotropic distillation of isopropyl alcohol (IPA) + water (H2O) with cyclohexane (CyH) as an entrainer were investigated. A simple operating procedure under inverse double loop control strategy is proposed to automatically adjust the manipulated variables to be at optimum operating point. A simple one-way decoupling control scheme is also proposed to account for the high interactions between two temperature control loops. Both feed rate and composition load disturbances will be introduced to test the proposed decoupling control scheme.