Novel Lab‐Scale System for Lyocell Fiber Manufacturing

ABSTRACT Lyocell man‐made cellulosic fibers (L‐MMCFs) are typically produced from wood sources, but sustainability efforts are driving interest in agricultural biomass feedstocks. This study presents a lab‐scale system for evaluating feedstock viability and processing conditions using a rotary evaporator, syringe pump, and microreactor vessel. Results show that lower processing temperatures (≤ 90°C for dissolution, 65°C for spinning) lead to better fiber formation, while higher spinning temperatures (95°C) result in irregular morphology. Lower processing temperatures also reduce the risk of exothermic reactions and n ‐methylmorpholine‐ n ‐oxide (NMMO) decomposition, improving process safety. This is further confirmed by scanning electron microscopy (SEM). Viscosity measurements, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and X‐ray diffraction (XRD) validate optimized processing conditions. Fourier transform infrared spectroscopy (FTIR) analysis verifies NMMO recovery efficiency, showing post‐evaporation concentrations reaching 51.4 wt.%, similar to commercial stock solutions. Even if the final proposed lab‐scale method did not apply fiber drawing to the fiber, this approach provides a repeatable, cost‐effective framework for evaluating alternative cellulose sources and refining processing conditions for sustainable L‐MMCF manufacturing. While mechanical testing is not relevant to this method due to the absence of fiber drawing, this limitation is acknowledged and highlights an area for future development in lab‐scale L‐MMCF evaluation.