AbstractSeparation of acetylene (C2H2) and carbon dioxide (CO2) is of prime importance in the petrochemical industry, but their similarities in molecular size and volatility make it particularly difficult. A desired adsorbent for highly efficient C2H2/CO2 separation should have high selectivity and C2H2 uptake simultaneously, and the introduction of functional groups into MOFs is an effective strategy to achieve this purpose. Herein, we report a titanium‐based MOF material (MIL‐125‐NH2), featuring the suitable pore sizes and amino‐functionalized pore surfaces to show the preferential adsorption of C2H2 over CO2 with both high C2H2 uptake and C2H2/CO2 selectivity. Theoretical simulation results indicate that the preferential C2H2 adsorption is mainly attributed to multiple hydrogen bonding interactions between C2H2 molecule and amino functional groups.

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