(NH4)6[NiMo9O32]·6H2O was synthesized by(NH4)6Mo7O24·4H2O,NiSO4and(NH4)2S2O8.It was used as the photocatalyst for the degradation of methyl orange solution under sun irradiation.The results indicated that when the dosage of catalyst was 0.2g/L,the initial concentration of methyl orange was 10mg/L and the illumination time was 100 min,the decolorization rate of methyl orange solution could beup to 98.67%.