Carbon-based materials have been used for SO 2 removal from flue gases for several decades. In this process, SO 2 is captured by storing in the pores of carbons in the form of H 2 SO 4 , and regeneration of the SO 2 -captured materials is necessary to recover SO 2 capture ability. V 2 O 5 -supported activated coke (V 2 O 5 /AC) has been reported to be highly active for SO 2 removal, and its regeneration has been investigated from the viewpoint of the reaction mechanism. This work studied the regeneration kinetics with the aid of a thermogravimetric analyzer coupled with a mass spectrometer. The SO 2 -captured sample was prepared in a fixed-bed reactor with a simulated flue gas containing 1500 ppm of SO 2 , 5% O 2 , and 5% H 2 O. The kinetic equation was obtained by fitting the H 2 SO 4 conversion (α) at different heating rates with nonisothermal kinetic methods called Flynn−Wall− Ozawa and Coats−Redfern. The results indicated that the regeneration kinetic behavior varies with α. At α = 0.1−0.4, regeneration follows first-order reaction model f(α) = 1 − α with an activation energy of about 85.7 kJ/mol. At α = 0.5−0.8, regeneration follows three-dimensional diffusion model f(α) = 1.5(1 − α) 2/3 [1 − (1 − α) 1/3 ] −1 , with the activation energy increasing from 88.9 kJ/mol at α = 0.5 to 112.1 kJ/mol at α = 0.8.