Abstract: With titanium trichloride as oxidant, ascorbic acid as reducing agent and incendiary agent, the synthesis of titanium dioxide by combustion method was carried out rapidly and the prepared samples were characterized by FT-IR, XRD, UV-Vis and SEM. Under the optimal titanium trichloride to ascorbic acid molar ratio of 1: 0.6, the prepared cream white nano-titanium dioxide had an average particle size of 28 nm. Using this titanium dioxide as photo-catalytic catalyst, 0.01 g/L methylene blue solution as simulated wastewater, the effect of catalyst dosage, H2O2 amount, system pH value and the rotation speed of centrifuge on the degradation of methylene blue was investigated. Test results showed that the optimum treating conditions were as follows: a catalyst dosage of 3 g/L, H2O2 to methylene blue solution volume ratio of 1:20，system pH value of 9 and centrifuge rotation speed of 2 000 r/min; treating under such conditions for 240 min, the 0.01 g/L methylene blue solution was degraded to colorless.