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Abstract: Amid growing environmental concerns and biomass waste accumulation, this study aims to valorize cassava pulp—a readily available agricultural by-product in the Philippines—by producing nanocrystalline cellulose (NCC), a high-value material with broad industrial applications and sustainability potential. This study explores the synthesis and characterization of NCC extracted from waste cassava pulp sourced in Northern Mindanao, Philippines. Extraction was performed via mixed acid hydrolysis using formic acid and sulfuric acid, following alkaline pretreatment with sodium hydroxide and bleaching with sodium hypochlorite. The effects of acid concentration, temperature (70–90°C), and hydrolysis time (1–6 hours) on extraction yield were investigated. Results showed that increasing these parameters initially improved yield, but excessive values led to a decline. Optimization yielded the most favorable conditions at 71 wt% formic acid, 77°C, and 3.6 hours, achieving an extraction yield of 67.272%± 2.295%. FTIR confirmed successful removal of lignin and hemicellulose, while SEM and dynamic light scattering (DLS) revealed nano-sized cellulose particles ranging from 15 nm to 687 nm.
Key Words: nanocrystalline cellulose; mixed acid hydrolysis; waste cassava pulp; supercapacitor; energy storage