Abstract. Preparation of Fe2O3/TiO2 composite from Bengkulu iron sand via roasting, leaching and co-precipitation treatment has been carried out. Roasting was performed at 800 °C by addition of sodium disulfide (Na2S) in a various weight ratio of iron sand : Na2S were 1:1; 1:1.5 and 1:2 (w/w), respectively. X-Ray Fluorescence (XRF) analysis result showed that Bengkulu iron sand contained hematite (Fe2O3) about 79.96% and titanium dioxide (TiO2) about 10.53%. While the X-Ray Diffraction (XRD) analysis result of roasted iron sand compositions were rutile TiO2, Fe2O3, (hematite), NaFeO2, NaFeS2, FeO, and Na2TiO3. Leaching process using H2SO4 solution indicated that the H2SO4 concentration had influenced the leaching process of roasted iron sand. The optimum iron sand dissolution reached maximum value about 95.10% using H2SO4 7 N solution treatment. Inductive Coupled Plasma-Optical Emission Spectrometry (ICP-OES) analysis demonstrated the Fe content = 10.8338 g/L and Ti content = 1.5372 g/L. Therefore, the content of Fe2O3:TiO2 in leaching filtrate was 3.125:1 (mol/mol) estimated in pH range of 8-10. Photocatalytic activities of Fe2O3/TiO2 composites exhibited that Rhodamine B could be decomposed up to 57.73% at 60 minutes contact times under visible irradiation using 300 Watt xenon lamp.