Acid hydrolysis was used for the synthesis of cellulose nanocrystal (CNC) from cassava peel (CP). The process was carried out at 450C for 45 min using 64% concentrated sulphuric acid, Pb2+ was removed from aqueous solution using the synthesized CNC adsorbent. Cassava peel cellulose nanocrystal (CPCNC) was characterised using FT-IR and X-Ray diffraction techniques. The different operational factors were examined to enhance the conditions for optimum adsorption of Pb2+. The equilibrium adsorption figures fitted well into both the Freundlich and Langmuir isotherm models, indicating that adsorption was due to the formation of a monolayer adsorption unto a homogenous surface and showed a good relationship between the Pb2+ and the CPCNC. The separation factor, RL, which is a dimensionless constant ranged between 0.02 and 0.248 and indicated that the adsorption was feasible and favourable. The optimum adsorption capacity was 6.4 mg Pb2+/g CNC at 25°C and pH 6. This study revealed that this novel nanomaterial has an unlimited prospect for effective removal of lead ion from aqueous solution.