In this experiment, Sm (NO 3 ) 3 6H 2 O, hexamethylene tetramine (HMT) and glucose as the main raw material, nanosized Sm 2 O 3 was prepared by hydrothermal method. Sm 2 O 3 samples were characterized by XRD, SEM, FT-IR, TG-DTA and DRS respectively. It found that plus C elements could increase the crystallinity of the sample by exothermic reaction, but carbon dioxide lead to the destruction of Sm 2 O 3 nanospheres. In photocatalytic test, nano Sm 2 O 3 was applied in degradation of methyl orange by adjusting catalyst quality and illumination time to optimize parameters. The catalytic time and mass of the catalyst can increase the degradation rate of methyl orange, but excessive catalyst will discourage the degradation of methyl orange.