In order to improve the experimental teaching level, based on the concept of serving air pollution control with material chemistry, a comprehensive experiment of catalytic ozonation of toluene using hydrotalcite-derived catalysts was designed. The experimental plans were designed by students independently, and different preparation methods combined with the high-temperature calcination technology could be selected according to different plans. Modern instrumental analysis methods such as X-ray diffraction (XRD), scanning electron microscopy (SEM), BET, H₂-temperature programmed reduction (H₂-TPR), NH₃-temperature programmed desorption (NH₃-TPD), and electron paramagnetic resonance (EPR), were used to characterize physicochemical characterization from the microscopic point of view. This experiment helps students understand the application of materials chemistry in the field of environmental engineering, which is helpful to improve students’ macro-micro combination ability to think innovatively and stimulating students’ interest in scientific research.