Kapok fibers have been acetylated for oil spill cleanup in the aqueous environment. The structures of raw and acetylated kapok fiber were characterized using Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM). Without severe damage to the lumen structures, the kapok fibers were successfully acetylated and the resulting fibers exhibited a better oil sorption capacity than raw fibers for diesel and soybean oil. Compared with high viscosity soybean oil, low viscosity diesel shows a better affinity to the surface of acetylated fibers. Sorption kinetics is fitted well by the pseudo second-order model, and the equilibrium data can be described by the Freundlich isotherm model. The results implied that acetylated kapok fiber can be used as the substitute for non-biodegradable oil sorption materials.