A series of supported photocatalyst with different calcination temperature and coated times were prepared by coated TiO2 sol-gel on floating sphere with hollow structure to find photocatalyst having high photocatalytic activity so as to enhance the efficiency of degradated wastewater from dyestuff industrial processes.Methyl orange solution was selected as an example to study the effects of calcinate temperature,coated times and initial concentrations on photocatalytic activity.Experimental results show that TiO2/floating sphere supported photocatalyst,which is calcined at 500 ℃ and coated four times,has the best catalytic property and nearly 69% methyl orange solution(5 mg/L) is degradated within 120 min.The photocatalytic activity enhances when the initial concentration of methyl orange solution decreases.