A ternary Nano-composite using kaolin clay- activated carbon (bagasse) – chitosan was prepared via sol-gel method. The raw kaolin clay was modified by using aluminium nitrate and it was characterized using Fourier Transform Infrared Spectroscopy (FT-IR). Activated carbon was synthesized from bagasse by KOH activation. The synthesized activated carbon was characterized by Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscope (SEM). The particle size, surface area and porosity of the activated carbon were also measured. The Nano-composite prepared was characterized by using Fourier transform infrared analyzer (FT-IR) and Scanning electron microscope (SEM). The particle size, surface area and porosity of the Nano-composite were measured. The surface area of the ternary nanocomposite from Brunauer-Emmett-Teller analyzer (BET) was found to be 1957m2/g. Batch wise adsorption tests were conducted for different concentrations of the nickel effluent, for different residence time with constant amount of the prepared Nano-composite. The nanocomposite exhibited excellent performance of nickel removal from the aqueous solution. The Atomic Absorption Spectroscopy results revealed that upto 99% adsorption efficiency was achieved in 200ppm of nickel effluent for 0.5g of adsorbent. The Atomic Absorption Spectroscopy analysis was conducted for 200,400,600,800 and 1080 ppm of nickel effluent with 0.5g of the adsorbent for a contact time of three days and seven days. After three days the concentration of the nickel effluent was found to be reduced and at the seventh day the concentration of nickel effluent was increased when compared to the concentration of the nickel at the end of three days. This explains the phenomenon of desorption. The cause of desorption is due to the increase in temperature. Hence the optimum contact time for this adsorption process was found to be three days.