In general, aqueous phase reforming (APR) is used to convert glycerol into 1,3-propanediol (1,3-PDO), nonetheless, studies have shown a low selectivity of 1,3-PDO. Therefore, this study aims to optimize the selectivity of 1,3-PDO by varying the ultrasound (Us) irradiation process time between 10 and 50 �min during catalyst preparation. This is to investigate the effect on the physiochemical properties and activity of the catalyst. Ni�Mo/Al2O3 catalysts were prepared using a sonochemical method and was characterized using Brunauer-Emmett-Teller (BET), X-ray Powder Diffractometer (XRD), Field Emission Scanning Electron Microscopy (FESEM) and Hydrogen Temperature-programmed Reduction (H2-TPR). Characterization results revealed that there were significant improvements in physiochemical properties of catalysts by varying the Ultrasound (Us) irradiation time. Subsequently, all catalysts were screened using APR of glycerol for 1,3-PDO production using an Autoclave PREMEX reactor and the liquid products were analyzed to determine the selectivity of 1,3-PDO. From all the results, findings revealed that the catalyst prepared with 10 �min of Us radiation time demonstrated a high catalytic performance and physiochemical properties while producing the highest concentration of 1,3-PDO with 954 �ppm with a conversion of 38.6. The outcomes have shown that sonochemical irradiation time conversely effects on the physiochemical properties of the catalysts and 1,3-PDO production. © 2021 The Author(s)