High-siliceous MCM-41 was calcined at 800 degrees C in dry air and at 600 degrees C in water-saturated air for different time respectively. Their XRD patterns and adsorption isotherms of cyclohexane were determined. The results show that the structure of MCM-41 is more stable after calcining at high temperature in dry air. The structures of the samples were damaged by the hydrothermal treatment precalcined at high temperature in dry air for different time with different degrees. The parent MCM-41 was damaged more, but the precalcined samples less. The influence of thermal and hydrothermal treatment on the pore size is not too remarkable.