The regeneration kinetics of coke on an industrial methanol-to-olefin (MTO) catalyst was studied via thermogravimetric analysis under the air atmosphere. To minimize the uncertainty of the kinetic parameters, four model-free methods were employed to calculate the regeneration activation energy. It was found that the activation energies obtained by all methods are quite consistent for any given coke conversion. An average activation energy of 141.1 kJ/mol was obtained for combustion of coke on the industrial MTO catalyst. The master-plot method was then employed to decide the regeneration model function. It showed that the combustion process of coke on the industrial MTO catalyst may be depicted using the Fn model. A comparison between the model prediction and additional experimental results demonstrated that the regeneration kinetics model built in this work can work very well under operation conditions of industrial interest and favor the optimization and design of a regenerator in an industrial MTO unit.