Aminated polyethersulfone (PES-NH 2 ) has been synthesized and used with carboxylated activated carbon (AC-COOH) as an adsorbent using two different methods: in situ and ex situ techniques. The chemical modification of polyethersulfone (PES) to introduce -NH 2 functions was used to overcome the hydrophobicity of PES which maximizes its use in water treatment applications whereas applying AC-COOH to this polymer provides a promising effective method as an adsorbent-separation technique to remove dye pollutants from wastewater. The structure and characterization of aminated polyethersulfone with carboxylated activated carbon (PES-NH 2 -AC-COOH) were identified using proton nuclear magnetic resonance ( 1 H-NMR), Fourier transform infrared (FT-IR spectroscopy), X-ray diffraction (XRD), thermal analysis (TA), and a scanning electron microscopy (SEM). The performance of PES-NH 2 in situ and ex situ with AC-COOH was tested for the adsorption of cationic (methylene blue) and anionic (acid red 1) dyes from an aquatic environment. The results of the study showed a better thermal stability for the PES-NH 2 with 20% AC-COOH with both in situ and ex situ techniques as well as an excellent adsorption performance in comparison with the bare PES-NH 2 . The resultant polymers displayed significantly high adsorption rates for the acid red dye (60% and 68%) and methylene blue dye (61% and 88%) by PES-NH 2 with AC-COOH using in situ and ex situ techniques, respectively, in comparison with the control (PES-NH 2 ) which showed lower adsorption rates for both dyes (21% for acid red and 33% for methylene blue). Lastly, the study experimental measurements found the most suitable model to describe the kinetic behavior of the acid red dye adsorption by our developed polymer (by PES-NH 2 with AC-COOH) to be the pseudo-second-order kinetic model.