ABSTRACT To investigate the spontaneous combustion thermal effect of the by-products oxidized powder (OP) and carbonized powder (CP) produced during the preparation of coal-based activated carbon (CBAC). First, the changes in composition and pore structure of OP and CP compared with raw coal (RC) were measured by coal quality analysis and nitrogen adsorption experiments. The ability of OP and CP to physically adsorb oxygen was determined. Then, differential scanning calorimetry (DSC) was used to study the whole process thermal effect of the spontaneous combustion of OP and CP. Finally, the thermal effect of OP and CP during low-temperature oxidation process was further explored by the C80 micro-calorimeter, and the thermodynamic characteristics were also probed. The results show that the content of fixed carbon and carbon elements in OP and CP are significantly greater than that in RC, which makes the pore structure of both complicated. In addition, the total pore volume, average pore size, and specific surface area of OP and CP are greater than that of RC, which is more conducive to the physical adsorption of oxygen by both. No transition platform is caused by the decomposition of intermediate products on the DSC curve of CP. The characteristic temperatures of CP (except T D10) are lower than that of OP, indicating that the spontaneous combustion reaction of CP started earlier than that of OP. However, part of the combustible substance of CP was consumed in the dry distillation process, leading to the thermal release and maximum thermal release rate being smaller than that of OP. The apparent activation energy (E a) of stages H2 and H3 in the low-temperature oxidation process of OP is 75.04 and 11.42 kJ mol−1, while that of CP is 83.11 and 30.91 kJ mol−1. The threshold of CP entering stages H2 and H3 is higher than that of OP. Nevertheless, from the pre-exponential factor (A), the low-temperature oxidation process of CP is more rapid.