AbstractThis work discusses the preparation and characterization of hollow nanospheres based on kraft lignin (KL). Kraft lignin is a by-product of the papermaking industry and an abundant renewable resource. It was determined that adding water to a KL/THF solution induced KL to form hollow nanospheres via self-assembly. Scanning electron microscopy and transmission electron microscopy confirmed the hollow nanosphere morphology. The shell thickness of the hollow nanospheres was tunable by adjusting the initial KL concentration in THF, making the nanospheres a potential material for the encapsulation and controlled release of guest molecules. Ultraviolet (UV) and Fourier transform infrared (FTIR) spectroscopy confirmed the π-π stacking of aromatic rings as an important and distinctive mechanism for the formation of hollow KL nanospheres. The nanospheres were obtained simply and inexpensively, and they exhibited the characteristics of biocompatibility, biodegradability, and low toxicity. These advantages make hollow KL nanospheres attractive for applications in nanoscience and nanotechnology. This study developed an economically feasible and facile strategy for the effective use of biomass waste in sustainable chemistry.