A massive amount of coal gangue (an accompanying solid waste) is annually produced during coal mining and washing prcesses , leading to the wastage of land resources and causing environmental impacts. Due to the abundant presence of metal oxides such as Fe2O3, and Al2O3 in coal gangue, the extraetion of iron and aluminum from it serves as a crucial pathway for the resource utilization of coal gangue. ln this study , a thermal activation-acid leaching method was used to extraet Fe3+ and Al3+ from coal gangue. Through single-factor experiments, with varables including liquid-to-solid ratio, aeid coneentration, acid leaching time, and acid leaching temperature , the influenee of these factors onthe leaching rates of Fe’* and Al’* was investigated. Subsequently, response surface optimization experiments were conducted using Design-Expert 13 and Box-Behnken methods, and a regression model with a high degree of fit was established. The results of the regression model indicated that the optimal conditions for the leaching of Fe3+ and Al3+ were as follows: An aeid leaching temperature of 101.71 ℃, aeid coneentration of 2.67 mol/L, a liquid-to-solid ratio of 5.90 : 1 mL·g-1, and an acid leaching time of 3.04 hours. Under these conditions, the leaching rate of Fe3+ and Al3+ was 66.04% and 35 .84%, respectively. These findings provide valuable references for the resouree utilization of coal gangue.