ABSTRACT In this work, two organic nonconsumable biomass municipal wastes, coconut peduncle (CP) and areca nut husk (ANH), were selected as per novelty, and the results were experimentally investigated and optimized for better suitability as per energy storage applications. Fourier transform infrared spectroscopy (FTIR) analysis of both the biomasses shows the presence of oxygen functional groups and aromatic compounds, such as lignin which are the important parameters for energy storage. CP contains more lignin content than ANH by 2.21% as investigated by the National Renewable Energy Laboratory (NREL) protocol. Proximate analysis of the two biomasses revealed that CP has more volatile matter and a lower ash content than does ANH, indicating better pore development for energy storage. Thermogravimetric/differential thermogravimetric (TG-DTG) curve reveals that both the biomasses are thermally stable nearly at 500°C above which slow pyrolysis can be performed. Two-step KOH activation improved the yield of the biochar at 1:4 (w/v) biochar to KOH ratio through direct impregnation. The adsorption−desorption isotherm shows that activated coconut peduncle biochar at 1:4 (ACPB4) has a better surface area of 494.076 m2/g and microporosity than activated areca nut husk biochar at 1:4 (AANHB4) making CP a suitable porous material for energy storage.