Al-Cu composite metal oxides were supported on MCM-41 to simultaneous adsorption/oxidation of NO and SO2 from Coal-fired flue gas in this work. The material was prepared by hydrothermal synthesis method and the synthetic conditions such as aluminum content, the second metal selection, the second metal content and calcination temperature were investigated. The experiment results showed that the adsorption/oxidation effect achieved the best when the ratio was Si: 02 Al: 0.02 Cu at 90 degrees C. The synthesized materials were characterized by N-2 adsorption-desorption measurements, transmission electron microscope (TEM) and energy dispersive spectrometer (EDS). Compared with other adsorbents, Al-Cu-MCM-41 had larger specific surface area and total pore volume by N-2 adsorption-desorption measurements. Meanwhile, the additions of aluminum and copper did not change mesoporous structure of MCM-41 and the active components could be dispersed uniformly within the framework of Al-Cu-MCM-41 by TEM. In addition, the results of EDS explained that the presence of active components was convinced and sulfur element was detected on inactivated Al-Cu-MCM-41adsorbent. The analysis results illustrated that the presence of aluminum and copper could enhance the adsorption/oxidation capacity of NO and SO2. Therefore, it could infer that chemical adsorption probably had a better removal effect than physical adsorption.