Abstract: By adjusting the pH of the H₂SO₄ leaching liquor of fly ash,Ti⁴⁺ and Fe³⁺ were extract-separated with trioctylphosphineoxide(TOPO)-kerosene and di(2-ethylhexyl) phosphoric acid(P204)-kerosene,respectively.Effects of the extractants,the concentration of the cations,pH of the aqueous solution,extracting temperature,and extracting time on the extracting efficiency were investigated.Effect of the recycle conditions of the loaded extractants on the recovery yield and the purity of recovered products were discussed as well.The phase of the precursor and its calcined products were characterized by X-ray diffraction(XRD).The purity of the TiO₂ and Fe₂O₃ were determined by X-ray fluorescence(XRF).The analysis results show that the extracting-titanium efficiency and the extracting-iron efficiency were as high as 97%.The extraction yields of ferric oxide and titanium dioxide are 96% and greater than 92%,respectively.The purities of TiO₂ and Fe₂O₃ are 98% and 97%,respectively,which can be used as a white pigment or iron oxide red pigment in the production of paints,respectively.