AbstractThe purpose of this study is to investigate the effective chemical treatment of fly Ash (FA) that affects the mechanical, thermal, and water absorption capabilities of polystyrene/styrene‐butadiene‐copolymer (PS/SBC) nanocomposites. NaOH, H2SO4 and distilled water have been employed to conduct the chemical treatment. Specimens have been prepared using injection molding technique. In order to evaluate the mechanical properties of the material, tensile, flexural, impact, and hardness tests were carried out. thermo‐gravimetric analysis (TGA) and differential thermal analysis (DTA) were employed to gain an understanding of the thermal behavior of the material. Furthermore, to determine the moisture resistance, water absorption experiments were conducted. Experimental results show that, alkali‐treated FA (AL‐FA) demonstrated the maximum values with an ultimate tensile strength of 26.68 MPa, acid‐treated FA (AC‐FA) composite exhibiting the highest flexural strength at 5 MPa whereas water‐treated FA (WA‐FA) composite led to better impact strength of 17.6 kJ/m2. TGA revealed that WA‐FA and AL‐FA composites experienced an 80% reduction in weight at 500°C, while AC‐FA composites exhibited weight reductions of 90%. The significance of treatment methods in interfacial interactions between the polymer and FA has been studied through morphological analysis. These findings provide valuable insights that can be applied to future research and industrial applications in the field of sustainable materials engineering.Highlights Polystyrene/Styrene‐Butadiene‐Copolymer composites were prepared with Fly ash (FA) filler. FA pre‐treated by NaOH (AL‐FA), H2SO4 (AC‐FA) and distilled water (WA‐FA). Injection molding technique was employed to prepare the ASTM standard samples. WA‐FA composite exhibited the highest ductility but lower tensile strength. TGA revealed that AC‐FA composites exhibited weight reductions of 90%.