Abstract In this study, chemical modification of chitosan has been carried out using epichlorohydrin as crosslinking agent and ethyl acetoacetate as a modifier to graft acetoacetyl moiety. The said organo-functionalization on chitosan and sodium alginate not only offered a novel support for TiO₂ immobilization but also enhanced sorption performance for Ni(II) recovery from aqueous medium. So, a composite consisting of acetoacetyl moiety grafted chitosan, sodium alginate and titanium oxide (EAA-MCS/TiO₂) was prepared and characterized by fourier transform-infra red (FT-IR) spectroscopy and scanning electron microscopy (SEM). The hybrid composite (3EAA-MCS/TiO₂) which had TiO₂ to EAA-MCS mass ratio of 20.0% by weight showed maximum sorption efficiency. The formulated sorbent was conditioned in the form of hydrogel beads for operation. Isothermal sorption and kinetics studies were performed at pH = 6.0 to configure the nature of sorption. Pseudo-2nd order rate expression better explained the sorption kinetics and chemisorption is the predominant mode of uptake. Langmuir adsorption model better explained the sorption process (R ² ∼ 0.99) and maximum monolayer sorption capacity (q _m ) at sorption/desorption dynamic equilibrium was computed as 403 mg/g at optimized pH.