The two-step dehydroxylation of illite is studied using the differential scanning calorimetry on powder samples with heating rates from 1 to 10 °C min -1 in a dynamic argon atmosphere. The values of apparent activation energy and pre-exponential factor are calculated using the Kissinger method. The determined values of apparent activation energy and pre-exponential factor of trans-vacant layer dehydroxylation are (227 ± 6) kJ mol -1 and (2.87 ± 0.09) ×10 13 min -1 , respectively. The results also show that this process can be characterized by 1D diffusion controlled reaction with instantaneous nucleation rate. For the cis-vacant layer dehydroxylation, the values of apparent activation energy and preexponential factor are (242 ± 10) kJ mol -1 and (5.37 ± 0.23) ×10 12 min -1 , respectively. The value of Avrami peak factor for this step indicates diffusion controlled growth of the new phase with zero or decreasing nucleation rate.