Abstract: There have been few studies on the heat effects of coal pyrolysis in the past, and the results of heat effects research have also varied. This may be caused by different methods of measuring heat effects, measurement conditions, and methods of treating DSC baseline heat flow. In order to determine the heat effects of coal pyrolysis more universally, accurately, and standardly, based on thermogravimetric differential scanning calorimetry (TG–DSC) to study the influence of main measurement conditions on the heat effects of coal pyrolysis, in order to determine the optimal measurement conditions. Then, based on the optimal measurement conditions, the heat effects of Yankuang bituminous coal pyrolysis was explored. Thermodynamics analysis was carried out according to the TG/DSC/DTG curves, and empirical methods were used to treat the DSC baseline heat flow. The pyrolysis process was divided and the heat effects of coal pyrolysis were qualitatively and quantitatively analyzed. The results indicate that the optimal conditions for determining the heat effects of coal pyrolysis are as follows: crucible type is a 70 μL platinum crucible with a 50 μL standard capped alumina crucible, coal particle size<75 μm, coal sample weight 10 mg; coal sample loading method is not compacted, pyrolysis atmosphere is Ar, gas flow rate 80 mL/min, pyrolysis final temperature 1100 ℃, heating rate 10 ℃/min. Under the optimal measurement conditions, empirical methods were used to peak the DSC heat flow curve using spline curves as baseline. The pyrolysis process of Yankuang bituminous coal was divided into five stages, with three endothermic stages in the early stage and two exothermic stages in the late stage. The total process heat absorption was −160.13 J/g, heat release was +641.05 J/g, and the total heat effects of heat release were +480.92 J/g.