The removal of carbon dioxide (CO2) from acetylene (C2H2) represents a pivotal industrial process for the production of high-purity C2H2. Nevertheless, the separation of C2H2 and CO2 is challenging due to their highly similar molecular sizes and physical properties. In this work, we report a fine regulation of a sql layered coordination polymer (termed NTU-107) into a rare fsc open framework (termed NTU-108) with naphthalenedisulphonic acid pillar for selective C2H2 capture from CO2-contained mixtures. NTU-107 was prepared by the reaction of 4-(1H-imidazol-1-yl)benzoic acid (L1) ligand and Cu2+ ion, showing a layered framework with a pore size of 4.2 Å. After inserting 1,5-naphthalenedisulphonic acid between the layers, a new pillar-layered open framework (5.8 Å) with sulphonic acid functional sites was prepared. Single-component gas adsorption experiments and breakthrough experiments demonstrated that NTU-108 with accessible sulphonic acid sites exhibits a high C2H2 absorption capacity and dynamic C2H2/CO2 separation performance at room temperature.
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