In this work, nanochitosan (NC) was prepared through ionic gelation using low-molecular-weight chitosan and maleic acid (MA). The synthesized NC was charac¬terized by means of Fourier Transform Infrared Spectroscopy (FTIR), Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM). In the course of preparation, the particle size of the material was strongly depended on the parameters such as chitosan concentration and pH of the solution. By controlling the above parameters, NC with the size of smaller than 100 nm was prepared. The chitosan and prepared NC were used for the adsorption of Pb (II) from aqueous solutions in a batch system. Among the sorption parameters, pH showed the strongest effect on the sorption process and maximum Pb (II) removal was obtained at pH value of 6. The pseudo-first-order and pseudo-second-order were used to track the kinetics of adsorption process. Langmuir and Freundlich isotherms were subjected to sorption data to estimate the sorption capacity. NC proved to be an excellent adsorbent with remarkable capacity to remove Pb (II) ions from the aqueous solutions at various concentrations. The NC also showed incredible performance with a comparatively easier preparation process than other reported work.