Copoly(amide-thioamide)s synthesized by polycondensation of bis(thioamide-amine)s and terephthaloyl dichloride in N-methyl pyrrolidone with moderate yields, possess inherent viscosity around 0.70 dL/g, and could be easily dissolved in amide-type polar aprotic solvent. The corresponding polythioamide was amorphous and showed a good thermal stability with glass transition temperature of 177°C in nitrogen atmosphere. The synthesized polymers were characterized by 1H and 13C NMR and X-ray diffraction and were used as sorbents for the treatment of waste water containing heavy metals. Various factors affecting the uptake behavior such as concentration and pH were investigated.