One‐Pot Extraction of Biodegradable Functionalized Microcrystalline Cellulose From Jute Stubble Fiber: A Sustainable Approach to Lignocellulosic Waste Utilization

ABSTRACT The valorization of agricultural wastes into high‐performance biopolymers offers a sustainable approach toward a circular bioeconomy. In this study, jute stubble fibers—a lignocellulosic waste generated after harvesting jute were used for the isolation of functionalized microcrystalline cellulose (F‐MCC) through a one‐pot oxidative technique where extraction and functionalization occur simultaneously. The process involved alkaline pretreatment followed by ammonium persulfate (APS) oxidation at different durations (10–22 h), enabling simultaneous delignification, amorphous part removal, and surface functionalization. The characterization results showed that APS oxidation introduced carboxyl groups on the cellulose surface, enhanced fibrillation, and progressively shortened fibril length while preserving the crystalline cellulose I lattice. 18 h was identified as the favorable oxidation duration among the investigated conditions based on crystallinity, surface chemistry, and morphology. The sample with 18 h of oxidation (F‐MCC 18 ) demonstrated the highest crystallinity index (88.3%), improved thermal stability with a degradation onset of above 200 °C, and biodegradability with >95% mass loss in natural soil within 38 days. These observations demonstrate that APS oxidation enhances the purity, crystallinity, and functionality of cellulose suitable for reinforcing composites and environmentally benign materials. This study highlights a strategy for converting waste into value‐added F‐MCC, advancing sustainable material development and waste‐to‐wealth initiatives.