Pervaporation (PV) process with the mixed matrix membrane (MMM) is a feasible and cost-effective alternative to conventional volatile organic compounds (VOC) removal methods. In this study, the mesoporous silicate MCM-41 was synthesized by a new and rapid sol-gel method and incorporated into the polyether-block-amide (PEBA-2533) polymer network. Prepared MMM and MCM-41 were characterized by XRD, FESEM, TEM, AFM, TGA, DSC, FTIR, contact angle, and mechanical analyses. Effect of MCM-41 calcination on the performance of MMM for toluene/water solution separation was studied using a PV setup. Experiments were conducted to determine the effects of MCM-41 loading, feed concentration, and feed temperature on total flux, component flux, separation factor, and pervaporation separation index (PSI). For a 300 ppm toluene aqueous solution at 30 °C, the separation factor, from 44.4 to 203.7 (358.7% increment), and toluene flux, from 3.9 to 10.5 g m−2 h−1 (163.8% increment), were improved by using 7.5% uncalcined MCM-41 loading. The PSI value of this sample was attained at 67290 g m−2 h−1, which was 412% higher than that of a neat PEBA membrane (13142 g m−2 h−1).
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