The photodegradation technology can improve the status quo of environmental problems seriously which hindered the development and progress of human society. In this work, the two-dimensional transition metal carbide Ti 3 C 2 was prepared by HF etching of Ti 3 AlC 2 , and subsequently TiO 2 crystals were produced by hydrothermal method to prepare TiO 2 /Ti 3 C 2 composite. The Ag nanoparticles were then doped by photoreduction to form a ternary Ag/TiO 2 /Ti 3 C 2 composite. The effect of photocatalytic degradation of the methyl orange solution by Ag/TiO 2 /Ti 3 C 2 was investigated. The degradation only with Ag/TiO 2 /Ti 3 C 2 is worser than TiO 2 /Ti 3 C 2 , so H 2 O 2 was added to improve the catalytic ability and explore the photocatalytic mechanism. In 420 min, the degradation efficiency of methyl orange (MO) solution reached 71.09% due to the active-free radicals preventing the recombination of electron hole pairs to improve the catalytic performance of photocatalytic materials.