A novel Ti/MCM-22/MCM-41 composite material was prepared by Nano self-assembly method. The synthesized material was characterized by XRD, N2 adsorption, SEM, and subsequently applied in the Acid Red B degradation. Several parameters such as dosage of catalyst, reaction time, pH of wastewater, and initial concentration of dye were systematically investigated. The oxidation products were analysed by ultraviolet spectrum. The results showed the highest removal efficiency up to 98% could be achieved when initial concentration of acid red B, pH of wastewater, amount of catalyst and reaction time were as 50mg/L, 6,0.1g/L and 120min respectively. The process of the catalyst reaction was accordant with first order kinetics equation. The ultraviolet spectrogram indicated two characteristic absorption bands of acid red B disappeared after degradation, structure of conjugated system was broken, and color of wastewater disappeared. It demonstrated the degradation of acid red B was mainly through photocatalysis of the composite material.