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Abstract The long‐standing challenge in fabricating advanced gas separation membranes lies in overcoming the trade‐off between precise pore size control and the formation of defect‐free layers. Herein, a high‐performance covalent organic polymer (COP) membrane is reported, fabricated via a modulated interfacial polymerization strategy. The COP structure is rationally designed using tetra‐amine and tri‐aldehyde monomers to enhance cross‐linking density and reduce effective micropore size. Analysis of CO 2 adsorption isotherms confirms a narrow pore size distribution centered around ≈0.34 nm, indicative of molecular sieving capability. The incorporation of ionic liquid combined with acetic acid at the interface enables precise regulation of amino monomer concentration, resulting in a controlled polymerization kinetic and facilitating the formation of a continuous, defect‐free membrane. The resulting membrane exhibits exceptional H 2 /CH 4 separation performance, achieving an ideal selectivity of 297.6 and H 2 permeance of 203.4 GPU. Remarkably, both permeance and selectivity remain stable under high feed pressures up to 2 MPa, attributed to the highly cross‐linked and robust polymer networks. This work demonstrates a feasible strategy for designing high‐pressure stable COP membranes with outstanding molecular sieving properties for energy‐efficient gas separations.
Liu et al. (Wed,) studied this question.