A series of porous polymers based upon polyacrylic acid crosslinked with Zn/Mn (Zn/Mn/PAA) were prepared by sol-gel method using polyacrylic acid as raw material, Zn2+ and Mn2+ as crosslinkers, and propylene oxide as coagulant. The adsorption performance of Zn/Mn/PAA for uranyl ions (UO22+) were then investigated by adjusting adsorbent dosage, pH, adsorption time, coexisting ions and ionic concentration. The results showed that the prepared Zn/Mn/PAA-2 with a molar ratio of Zn2+ to Mn2+ 1:1, the molar ratio of the total amount of crosskinkers to the polyacrylic acid 10:1, exhibited best adsorption performance for UO22+. Under optimal conditions of pH 4.3, initial UO22+ mass concentration 10 mg/L, adsorption time 30 min, adsorbent dosage 1 g/L and adsorption temperature 25 oC, removal rate of UO22 by Zn/Mn/PAA-2 reached maximum of 82.3% with the adsorption kinetics fitting the pseudo-second kinetic model. In presence of other metal ions, Zn/Mn/PAA-2 displayed selective adsorption for UO22+. The maximum removal rate of UO22+ in different water samples could reach 82.8%. After five times of recycling, the removal rate and desorption rate of UO22+ by Zn/Mn/PAA-2 still remained 65% and 72%, respectively.