Al2O3-polyethersulfone composite (APC) fiber prepared by wet-spinning method was used for deposition of CeO2 on the fiber surface, when the fibers were immersed in aqueous CeCl3 solution following by oxidation in H2O2 solution. The SEM-EDS analysis revealed that Ce was more highly deposited on the outer surface of the resultant CeO2-Al2O3 composite fibers. The adsorbent behavior for the removal of antimony (Sb) was systematically examined, resulting in superior adsorption performance obeying Langmuir isotherm with maximum adsorption capacity of 7.71 mg/g, which was approximately 2.0 times higher than that of the non-deposited APC fiber. Additionally, in the fixed-bed column experiments for aqueous Sb solution, the CeO2-deposited Al2O3 composite fibers performed their effectiveness in removing Sb from aqueous solutions in a continuous flow system.