AbstractMesoporous alumina catalyst supports with high surface area (upto458m2/g) and pore volume (upto1.55cm3/g) have been synthesized through Sol-gel process using non-ionic block copolymers as a template. Nitrogen gas adsorption, FT-IR and transmission electron microscopy were performed to determine the structure of these synthesized materials. Hydroprocessing of vacuum residue with prepared NiMo catalysts supported on mesoporous alumina was conducted in a batch reactor. The hydroprocessing reactions were performed at 400-420˚C with hydrogen pressure of 100bar. High conversions with low coke formation and high quality of liquid products (12.46wt% of naphtha, 31 wt% of middle distillates, 21wt% of VGO and 36wt% of residue) is obtained with the catalyst having large pore diameter and high pore volume.