In this study, poly(ether sulfone) (PES)/poly(sodium acrylate) (PSA) hybrid particles for the removal of environmental toxins were prepared via in situ cross-linked polymerization coupled with a liquidliquid phase separation technique. The particles were characterized by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). Batch experiments were performed to verify the adsorption capability of the particles, and the initial concentrations and pH values of the solutions significantly affected the adsorption process. In addition, both adsorption kinetic and adsorption isotherm models were used to analyze the adsorption process of Cu2+. The modified PES particles showed high adsorption capability for Cu2+ and methylene blue (MB), and a particle column was used to further study the removal ability of environmental toxins. The results indicated that the hybrid particles had great potential to remove heavy metal ions and cationic dyes for wastewater treatment on an industrial scale.