A composite compound of [CTMA]6SiW11NiO39 with Keggin type was synthesized by the simple method.The sample was characterized by means of element analysis,IR and TG-DTA measurement.The potocatalytic activities of the polyoxometalates for the degradation of methy orange solution under UV light irradiation were studied.The results indicated that the compound had high photocatlysis performances and could be reused.