The preparation of γ-Al 2 O 3 catalyst support by the modified hydrothermal method and synthesis of KI/γ-Al 2 O 3 catalyst, as well as the investigations of their activities in the reaction of transesterification of sunflower oil were performed in this study. The effect of various process parameters on the transesterification reaction of sunflower oil with methanol and their impacts on the reaction conversions were examined. The γ-Al 2 O 3 support and KI/γ-Al 2 O 3 catalysts were characterized by BET, XRD and SEM methods. The physico-chemical properties (surface, textural, structural and morphological) of the catalyst were correlated with its catalytic efficiency. The obtained results implicate that textural and structural properties of the catalyst and also the catalyst activity in the reaction of transesterification essentially depend on textual and structural properties of the γ-Al 2 O 3 support. From the optimization of the process parameters, it was found that the optimal conditions for transesterification reaction are: molar ratio of methanol to oil 12:1; stirring speed 600 rpm; the reflux temperature of methanol; the reaction time 5h; the amount of catalyst in the reaction 3 wt.%.