Tert‐butyl peroxypivalate is a typical free radical polymerization initiator due to the active O−O peroxide group, and it is a thermal instability material. To evaluate the thermal safety of tert‐butyl peroxypivalate, Dewar test, Differential Scanning Calorimetry (DSC) and Accelerating Rate Calorimeter (ARC) were used to study the self‐accelerating decomposition temperature (SADT), thermal performance parameters and kinetic parameters. The results of DSC reveal that the onset decomposition temperature of the initiator was 76.30 °C. The apparent activation energy (Ea) was 91.86 kJ mol−1 by Kissinger method. In ARC test, the onset decomposition temperature was 40.64 °C. The adiabatic temperature of the reaction was 86.68 °C, and the apparent activation energy was 120.14 kJ mol−1. The results of Dewar test show that the SADT of the initiator was 38 °C. The simulated SADT value by thermal analysis software (AKTS) was about 35 °C which was basically consistent with the results of Dewar test.
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