A facile solvent-free method to acetylate sago starch (Metroxylon sagu) is reported. Microwave (100 W) was used as the heating source and the heating time was varied from 2 to 10 min with the temperature of acetylation maintained at 100°C under continuous stirring. Using a 24 full factorial design of experiment, it was found that the degree of substitution (DS) of acetylated sago starch was strongly affected by the ratio of starch to acylating reagents, the ratio of acetic anhydride to acetic acid as the acylating reagents, the concentration of iodine as catalyst and reaction time. The physicochemical characteristics of the acetylated sago starch were assessed based on the FTIR spectra, the XRD spectra, the water absorption index (WAI), and the water solubility index (WSI). SEM was used to study the surface morphology of the acetylated sago starch at different DS.