Rotating Packed Bed (RPB) provides enhanced flexibility and the opportunity for significant size reductions in distillation processes by intensifying mass transfer. Rotating packed beds have a distinct advantage over conventional columns, mainly due to the intense micro-mixing within the fluid channels. Thinner liquid films will be formed in RPB’s which greatly enhances mass transfer between phases. In current study, distillation of methanol water system at total reflux condition was experimental investigated. The mass transfer performance was studied by varying the rotational speed and gas flow rate in the rotating packed bed. It was found that rotational speed has a significant impact on mass transfer effectiveness. The Height Equivalent to a Theoretical Plate (HETP) in the rotating packed bed used in this study was 3 to 4 times lower than that of conventional packed columns, indicating superior efficiency. Additionally, Response Surface Methodology (RSM) was employed, along with analysis of variance (ANOVA), to optimize the process parameters. The design of experiments was carried out using Minitab, with the mass transfer coefficient selected as the response variable in RSM, dependent on other independent variables. The optimized mass transfer coefficient was achieved at a rotational speed of 800 rpm and a gas flow rate of 0.23 kg/m²s. According to the ANOVA analysis, the gas flow rate was determined to be insignificant, whereas the rotational speed was found to be significant at a 95% confidence interval.