In this study, a Sodium alginate-g-poly (acrylamide-clay)/TiO₂ hydrogel nanocomposite [SA-g-p(AM-Bn)/TiO₂] was synthesized using the biopolymer sodium alginate (SA), acrylamide (AM), and bentonite clay (Bn) as hybrid materials embedded with titanium dioxide nanoparticles (TiO₂NPs) for the removal of toxic Congo Red (CR) dye from an aqueous solution. The [SA-g-p(AM-Bn)/TiO₂] nanocomposite has been described on the basis of thermal stability, morphological analysis, estimation of functional group, and crystalline/amorphous character by TGA, EFSEM/EDX, TEM, FT-IR, and XRD analysis, respectively. The effects of operational parameters toward the CR dye adsorption on [SA-g-p(AM-Bn)/TiO₂], including contact time, adsorbent dosage, initial concentration, initial pH, and temperature were investigated. The maximum adsorption efficiency was found to be 185.12 mg/g for [SA-g-p(AM-Bn)/TiO₂] in 100 mg/L of solution CR at pH 6.0 within 1 h. The equilibrium isotherms, kinetics, and thermodynamics parameters of adsorption were examined, and results showed that the isotherm fitted the Freundlich model and the kinetics adsorption model of CR followed pseudo-first-order, thus indicating physisorption of anionic-CR onto the sorbent due to the development of an electrostatic attraction bond. Thermodynamic parameters for [SA-g-p(AM-Bn)/TiO₂] have values (ΔG and ΔH) reflecting the spontaneous and endothermic nature of the adsorption processes. Moreover, [SA-g-p(AM-Bn)/TiO₂] presented outstanding excellent reusability and recyclability with a relatively best removal percentage as compared to [SA-g-p(AM-Bn)] and suggested their applicability towards the textile industry and water purification purposes.