Abstract Pervaporation (PV) desulphurization based on membrane technology has a great perspective for sulfur removal from transportation fuels. Herein, a unique two‐dimensional structure material–graphene egg yolk‐shell nanostructure (GYSNs) with high‐specific surface area and high dispersibility was prepared. In addition, the resultant GYSNs was incorporated into polyurethane (PU) matrix to fabricate mixed matrix membranes (MMMs). The MMMs were adopted to permselectively pervaporate thiophene with a thiophene/n‐octane solution as the model gasoline system and presented an elevated overall desulfurization performance as compared to the pristine PU membrane. Effects of GYSNs loading and operational variables including feed sulfur concentration, feed temperature, and operating time on the desulfurization performance were discussed. It was found that the MMMs with 0.8 wt GYSNs loading had a permeation flux of 1411 g·m−2·h−1 and an enrichment factor of 4.32 at 303 K for PV desulfurization of a 1312 ppm thiophene/n‐octane mixture. Noteworthy was that the as‐fabricated MMMs displayed long‐term operation stability. This is a positive step forward for practical applications of MMMs in gasoline desulfurization.
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