Three types of high molecular weight polyarylether adsorbents with different molar ratios of carboxyl and phenylene were designed and synthesized through direct polycondensation in mixture solvents. The as-prepared polymers were characterized by FTIR, 1 H-NMR, TGA, DSC, SEM, EDS, and GPC in order to study the regularity of polymeric adsorption/thermostability performances. Because of the highest molar ratio of carboxyl and phenylene, PAES-C-Na presented the highest adsorption capacity of Cu 21 compared to PAESK-C-Na and PAES; therefore, PAES-C-Na was opted to study the impacts of adsorbent dosage, pH, contact time, and initial concentration on the adsorption of Pb 21 and Cd 21 . Moreover, a kinetic analysis revealed that the adsorption process followed pseudo-second-order model, while the thermodynamic experimental data properly fitted with the Freundlich model. The multicomponent competitive adsorption capacity followed the order Pb 21 > Cu 21 > Cd 21 . Additionally, the regeneration tests indicated that PAES-C-Na still possessed the excellent adsorption capacity after several recycles.