A series of novel adsorption resins were synthesized via the chloromethylation of polyphenylene sulfide (PPS) resin and subsequent functional group conversion reaction. Their chemical structure, thermal stability, and morphology were systematically characterized by the Fourier transform infrared spectroscopy, elemental analysis, Raman spectroscopy, thermogravimetric analysis, scanning electron microscope, and energy dispersive spectrometer, respectively. The experimental results showed that the thioureido, mercapto, aminopyridine, and quaternary ammonium groups had been respectively introduced into PPS matrix, the functional group content of PPSâbased mercapto resin (HSâPPS), aminopyridine resin (APâPPS), and quaternary ammonium resin (QAâPPS) were about 2.20, 1.71, and 2.61 mmol gâ1, respectively. The adsorptive performance for Hg (II) and As (V) were studied by batch adsorptive method; the adsorption capacities of the HSâPPS and APâPPS resin for Hg (II) were 210.65 and 169.06 mg gâ1. The adsorption capacity of the QAâPPS resin was 88 mg gâ1 for As (V). Copyright © 2017 John Wiley & Sons, Ltd.