Carbon-based materials have been used for SO2 removal from flue gases for several decades. In this process, SO2 is captured by storing in the pores of carbons in the form of H2SO4, and regeneration of the SO2-captured materials is necessary to recover SO2 capture ability. V2O5-supported activated coke (V2O5/AC) has been reported to be highly active for SO2 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 SO2-captured sample was prepared in a fixed-bed reactor with a simulated flue gas containing 1500 ppm of SO2, 5% O-2, and 5% H2O. The kinetic equation was obtained by fitting the H2SO4 conversion (a) 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 a. At alpha = 0.1-0.4, regeneration follows first-order reaction model f(alpha) = 1 - alpha with an activation energy of about 85.7 kJ/mol. At alpha = 0.5-0.8, regeneration follows three-dimensional diffusion model f(alpha) = 1.5(1 - alpha)(2/3)[1 - (1 - alpha)(1/3)](-1), with the activation energy increasing from 88.9 kJ/mol at alpha = 0.5 to 112.1 kJ/mol at alpha = 0.8.