This study focuses on the increasing global demand for Monoethylene Glycol (MEG) and its production from corncob through Catalytic Hydrogenation. The process was optimized using Design of Experiment (DOE) and Response Surface Methodology (RSM). Physiochemical properties of the produced MEG were found to align with ASTM standards. Physiochemical properties of the produced Monoethylene glycol (MEG) was determined to have the following; density 2.19g/cm3, specific gravity 1.077 at 20 oC, flash point 116.20 oC and viscosity 12.32mm2/s at 40 oC, this values is in agreement with the ASTM standard values for monoethylene glycol. The study utilized a central composite design (CCD) with 21 runs to assess the impact of key parameters on biomass hydrogenation, revealing a quadratic model, also Analysis of variance (ANOVA) shows a high coefficient of determination (R2) of >0.9932. Four parameters (mass ratio of binary catalyst, hydrogen pressure, temperature and mass ratio of catalyst to feedstock) were varied with two center points to determine the effects of process parameters and eventually to get optimum monoethylene glycol (MEG) yield. The optimized conditions yielded a MEG yield of 70.2wt.%, demonstrating the potential of corncob as a viable source for MEG production. This finding proved that corncob can be utilized to produce monoethylene glycol (MEG) which could be potentially used in many way.