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In virtue of operating improperly, many exigent accidents of chemical industries are emerged frequently.1, l-Di-(tert-butylperoxy)-3,3,5-trimethylcyclohexane (TMCH), 1,1-di (tert-butylperoxy) cyclohexane (BPCH) and tert-butyl hydroperoxide (TBHP) are commonly well-known as thermal instability materials which were used as hardening and curing agents.The aim was to evaluate the safety operating parameters which play an important role in reaction system.In this study, differential scanning calorimetry (DSC) was applied to measure the heat of decomposition reactions, which can contribute to understanding the reaction characteristics of those materials.Vent sizing package 2 (VSP2) was employed to evaluate rates of increase for temperature and pressure in decomposition reactions, and then the thermokinetic parameters of three organic peroxides were estimated.At last, Semenovs model derived to criticality characteristics of various stirring rate situation were clearly identified.