Sustainable Production of Microcrystalline and Nanocrystalline Cellulose from Textile Waste Using HCl and NaOH/Urea Treatment

Bio-nanomaterials are gaining increasing attention due to their renewable and eco-friendly characteristics. Among these, nanocrystalline cellulose (NCC) stands out as one of the most advanced materials for applications in food, healthcare, composite production, and beyond. In this study, NCC was successfully extracted from cotton-based textile waste using a combination of chemical and mechanical methods. The cellulose fibers were first hydrolyzed using a dilute HCl solution, neutralized, and then dried, resulting in microcrystalline cellulose (MCC) with diameters ranging from 7 to 15 µm and lengths up to 300 µm (as observed via optical microscopy and scanning electron microscopy, SEM). To achieve nanoscale dimensions, NaOH/urea solution with mechanical treatment was applied, resulting in the successful extraction of NCC in the supernatant, particularly under room-temperature conditions. Dynamic light scattering (DLS) analysis confirmed the presence of nanostructures (average sizes ranging from 120 nm to 750 nm), and atomic force microscopy (AFM) analysis verified the nanoscale range (diameters between 2 and 4 nm and lengths from 200 nm to 1 µm). Fourier transform infrared (FTIR) spectroscopy revealed the conversion of cellulose I to cellulose II, confirming the successful transformation into NCC. For the first time, NCC was obtained from undyed cotton textile wastes using NaOH/urea treatment after HCl hydrolysis, eliminating the need for pre-treatment and intermediate steps.