Azo compounds (azos) are vital basic initiators used in chemical plants that also possess thermally active properties. Azos may trigger serious accidents because of their intense exothermicity. We applied a specific method to characterize the reaction kinetics of azos using data from differential scanning calorimetry (DSC). Specifically, this method was used to analyse the thermal decomposition of 2,2-azobis(2-methylbutyronitrile) (AMEN). The exothermic peak temperature, exothermic final temperature, and heat of decomposition were determined. The data obtained from the experiments were utilized to predict the self-accelerating decomposition temperature, control temperature, and emergency temperature. Experiments conducted to explore the runaway phenomenon of AMEN during the overall decomposition process interfered with the thermal analysis studies. We utilized a process simulation model to mimic the decomposition of AMEN, ensuring that the simulation results were realistic and practical. The results are worthy of being applied to thermal analysis, for example, for application in proactive loss prevention.