The KF/Al2O3 catalysts were prepared by an impregnation method and characterized by X-ray diffraction and thermogravimetric analysis. Their catalytic performances were evaluated in the transesterification of palm oil with methanol. The effects of the load ratio of KF to Al2O3, molar ratio of methanol/oil, amount of catalyst, reaction time, and temperature on product yields were investigated. The catalytic behavior was examined in relation to physiochemical properties of the catalysts.