This study aims to optimize, scale-up and assess the economic feasibility of mechanical nanofibrillation strategies (high-pressure homogenization and ball milling) to generate high-quality cellulose nanofibers (CNFs) from delignified sweet potato vines biomass, utilizing γ-valerolactone/water (GVL/H2O), while comprehensively analyzing the physicochemical, structural characteristics and appearance morphology of CNFs. Sequential parametric optimization allowed to determine optimum high-pressure homogenization (40 MPa, 4 cycles) and ball milling (60 Hz, 100 min) processing conditions. CNF by high-pressure homogenization achieved yields of 22.60 %, zeta potential of −27.23 mV, and average diameter of 23.66 nm; while ball milling yielded 19.74 % of CNF with zeta potential of −25.83 mV, and average diameter of 22.25 nm. The scale-up of high-pressure homogenization conditions at pilot scale generated yields of 21.90 % CNFs with consistent nanofibril morphology (19.81 nm average diameter). Moreover, comprehensive characterization revealed all CNFs exhibited superior thermal stability (>314 °C), enhanced crystallinity, and improved hydrophilicity compared to commercial CNFs. Techno-economic analysis of the pilot scale method under 2 different scenarios, recovering lignin and solvent or not. This analysis confirmed higher long-term profitability of the scenario recovering the compounds, despite the relatively higher initial investment, with a higher net present value ($485.82 million) and return on investment (57.24 %). Through the implementation of recyclable solvent-based biomass pretreatment, optimization of biorefining processes, pilot-scale validation, and techno-economic analysis, this study establishes a comprehensive green and sustainable biorefinery model for effectively converting agricultural waste into high-value nanomaterials, providing an economically feasible model for large-scale production of CNFs.
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