Experimental research on the preparation of photocatalyst for the decomposition of brilliant blue FCF (C 37 H 31 O 9 N 2 S 3 Na 2 ) was performed. TiO 2 and ZnO powders were prepared from titanium (IV) sulfate and zinc acetate at low reaction temperature and atmospheric pressure by hydrothermal precipitation method without calcination. In addition, TiO 2 was prepared with cationic surfactant CTAB (Hexadecyltrimethyl ammonium bromide) at the same conditions. The physical properties of prepared TiO 2 and ZnO, such as crystallinity, average particle size and absorbance, were investigated by XRD, Zeta-potential meter and DRS. And, the photocatalytic degradation of brilliant blue FCF has been studied in the batch reactor under UV radiation. For the photocatalysts prepared without CTAB, TiO 2 has smaller particle size and larger absorbance and photocatalytic reaction rate than ZnO. And TiO 2 , prepared with CTAB whose concentration is 1/10 of that of precursor, shows 15% higher than that prepared without CTAB in final photocatalytic degradation ratio of brilliant blue FCF.