MCM-48 is an important mesoporous silica material for current large-scale applications in key fields of the chemical industry including CO2 separation. Despite conventional hydrothermal synthesis used to produce mesoporous silica materials, but there is still research efforts needed to seek for the alternative for the production of mesoporous silica materials. In the current project, reflux synthesis method was studied and compared with conventional hydrothermal synthesis for the synthesis of MCM-48 samples. The synthesis temperature was varied (60 - 100 °C) at constant 2 days for both methods. The synthesized samples were characterized for its property using different analytical techniques including scanning electron microscope (SEM), x-ray powder diffraction (XRD), Fourier transform infrared microscope (FTIR), Thermogravimetric Analysis (TGA) and Brunauer-Emmett-Teller (BET). In current project, spherical particles of MCM-48 were successfully synthesized by reflux synthesis method at 100 °C for 2 days as well as conventional hydrothermal synthesis at 100 °C for 2 days, as observed from SEM and XRD analysis. From the BET analysis, the MCM-48 samples produced by reflux synthesis and conventional hydrothermal synthesis at 100 °C for 2 days displayed comparable pore characteristic with the commercial MCM-48 and MCM-48 reported by other researchers. © 2018 Penerbit Akademia Baru.