The kinetics of thermal dehydration of mixed hydroxide hy- drogels in MgO-ZrO2 system was studied as a function of composition by following the isothermal heat treatment route. Kinetic parameters were calculated through the ap-plication of the Guggenheim equation. The expulsion of both loosely bound water and constitutional OH groups were not continuous processes but proceeded in steps. The applicability of Is1 order reaction kinetics for the major portion of the reaction for all compositions suggests that during the de hydroxy! at ion process the dehydration is essentially controlled by the orientation of H2O molecules and the mutual interaction of hydroxy! groups. Due to a decrease in the concentration of the reacting species the activation energy was always higher at the final stage of dehydration.