This paper presents an estimation of the adsorptive potential of multiwalled carbon nanotubes (MWCNTs) and modified poly (acrylonitrile-co-styrene) with activated carbon for the uptake of reactive red 35 (RR35) dye from aqueous solution by a batch system. MWCNT adsorbent was synthesized by encapsulation via in situ polymerization. The copolymer material of poly (acrylonitrile-styrene) P (AN-co-ST) was prepared in a ratio of 2:1 V/V by the precipitation polymerization process. The prepared composites’ properties were characterized by FTIR, SEM, Raman, mean particle size (PSA), and XRD analysis. The PSA of the copolymeric material was determined to be 450.5 and 994 nm for MWCNTs and P(AN-co-St)/AC, respectively. Moreover, the influences of different factors, for example pH (2–10), adsorbents dosage (0.005–0.04 g), contact time (5–120 min), initial dye concentration (10–50 mg L−1), and temperature (25–55 °C). The optimum values were determined to be 2 and 4 pH, 10 mg L−1 of RR35 dye, and 0.04 g of adsorbents at early contact time. Furthermore, the adsorption isotherm was studied using Langmuir, Freundlich, Tempkin, and Halsey models. Maximum capacity qmax for MWCNTS and P (AN-co-St)/AC was 256.41 and 30.30 mg g−1, respectively. The investigational kinetic study was appropriated well via a pseudo second-order model with a correlation coefficient around 0.99. Thermodynamic study displayed that the removal of RR35 is exothermic, a spontaneous and physisorption system. The adsorption efficiency reduced to around 54–55% of the RR35 after four cycles of reuse of the adsorbents at 120 min.