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The construction of high‐performance MOF‐based hollow fiber composite membrane (HFCM) modules is a significant, yet challenging task for the biofuel production industry. In this study, a novel approach was taken to fabricate PDMS@ZIF‐8/PVDF HFCMs in modules through a facile ZIF‐8 self‐crystallization synthesis followed by pressure‐assisted PDMS infusion for pervaporation ethanol‐water separation. The as‐prepared HFCMs exhibited an ultrathin separation layer (thickness, 370 ± 35 nm), which was achieved through precise regulation of the ZIF‐8 membrane and defect repair by PDMS infusion. Moreover, the strategy utilized in this study resolved the defect issues arising from MOF agglomeration in conventional composite membranes. Impressively, at the optimal packing density, the prepared membrane demonstrated a remarkable ethanol flux (1.11 kg m−2 h−1) with an PSI value (26.59 kg m−2 h−1) and showed promising long‐term stability for the pervaporation of 5 wt% ethanol aqueous solution at 40°C. [ABSTRACT FROM AUTHOR]

1,3‐Butadiene (BD) is a petrochemical‐based volatile organic compound, extensively used for the manufacture of synthetic rubber. There is no method reported for its recovery from nitrogen mixture. Herein, for the first time, BD is efficiently recovered by gas separation through facile and novel mixed‐metal ZIF‐8 based mixed matrix membranes (MMMs). Addition of Ni‐ZIF‐8 nanoparticles in PDMS matrix, significantly improved the penetrant‐membrane interactions and the solution‐diffusion properties of BD. Positron annihilation lifetime spectroscopy analysis showed that the well dispersion of Ni‐ZIF‐8 in PDMS enhanced the free volume of membrane and created efficient continuous paths for BD diffusion. Then, 15 wt% Ni‐ZIF‐8 MMM exhibited the BD permeance of 323 GPU and the BD/N2 ideal selectivity of 19.5, which were 60 and 81% higher than pure PDMS membrane, respectively. The simultaneous enhancement of BD permeance and BD/N2 ideal selectivity indicated that Ni‐ZIF‐8 was an effective filler applied in MMMs for efficient BD recovery. [ABSTRACT FROM AUTHOR]