Abstract: In order to prevent the residual coal from oxidizing and self-igniting, and overcome low inhibitory effect of single property inhibitor, we use super absorbent polymer and antioxidant as source materials to develop a physicochemical synergistic inhibitor which has both physical and chemical inhibitory effects. Furthermore, the temperature-programmed method and gas chromatograph are employed to analyze the generation of CO and C₂H₄ in the process of coal samples heating and oxidation. Meanwhile, based on the differential scanning calorimetry experiments, the activation energies of samples during temperature rising are regarded as indicators to investigate the effect of the inhibitors. The results show that physicochemical synergistic inhibitor can not only overcome low inhibitory effect of antioxidant at early stage of coal oxidation, but also eliminate the failure of inhibitory effect of super absorbent polymer at later stage of coal oxidation. And experiments prove that physicochemical synergistic inhibitor can largely reduce coal oxidation product, increase the activation energy in the process of coal oxidation and self-heating, its inhibitor efficiency is better than that of super absorbent polymer or antioxidant. Therefore, physicochemical synergistic inhibitor is a new-type inhibitor that has good comprehensive performance.