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We report a facile in‐situ etching method for the synthesis of defective CuBTC (H‐CuBTC) with hierarchical pore structure. The fabricated mixed matrix membranes (MMMs) containing H‐CuBTC was prepared for the separation of CO2/CH4, showing superior separation performance due to the defective structure with larger pore size and more open Cu sites, which enhance the interactions between H‐CuBTC and the...