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Titanium dioxide (TiO2) film was prepared on activated carbon fibre (ACF) by hydrolysis technique, using sulphate titanium as raw material. Based on the techniques of photo catalytic degradation using TiO2/ACF, and 254nm UV-ray as the light sources, aqueous phenol solution of 40mg/L was photo catalytic decomposed over TiO2 film. The result showed that TiO2/ACF exhibited a degradation efficiency of 88.2% for phenol after 4h, while the condition of pH=7.5, the concentration of phenol is 40mg/L, power of ultraviolet light is 1.75W/L, and air quantity is 2.6mL/ (min·L). Analysis of photo degradation shows that the kinetics for photo catalytic degradation of phenol followed pseudo-first-order kinetic law, and the initial concentration of phenol, pH value, light intensity, air quantity and H2O2 concentration affected the photo catalytic degradation rates.