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Triazine-based materials with porous structure have recently received numerous attentions as af ascinating new class because of their superior potential for various applications.H owever,i ti ss till af ormidable challenge to obtain triazine-based materials with precise adjustable meso-scaled pore sizes and controllable pore structures by reported synthesis approaches.H erein, we develop as olvent polarity induced interface self-assembly strategy to construct mesoporous triazine-based carbon materials.I nt his method, we employamixed solvent system within as uitable range of polarity (0.223 Lippert-Mataga parameter (Df) 0.295) to induce valid self-assembly of skeleton precursor and surfactant. The as-prepared mesoporous triazine-based carbon materials possess uniform tunable pore sizes (8.2-14.0 nm), high surface areas and ultrahigh nitrogen content (up to 18 %). Owing to these intriguing advantages,t he fabricated mesoporous triazine-based carbon materials as functionalizedporous solid absorbents exhibit predominant CO 2 adsorption performance and exceptional selectivity for the capture of CO 2 over N 2 .

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The functional groups in porous carbon generally suffer a severe loss during the high‐temperature carbonization. Instead, the low‐temperature synthesis of carbon featuring porous structures and abundant functional groups is not only a solution that evades the pitfalls of pyrolysis but also is of significance for the development of synthetic methodology. Herein, a liquid metal interfacial engineering strategy is reported for the synthesis of porous carbon using CCl4 as the carbon precursor and sodium‐potassium alloy (NaK) as the reducing agent, which is superior to traditional synthetic methods because it enables the engineering of a highly active liquid metal alloy microemulsion to directly generate porous carbon at ambient temperature. As synthesized porous carbon featured abundant carbon‐chlorine bonds can be tandem‐grafted with imidazole and 1,2‐dibromoethane to achieve a CO2 cycloaddition catalyst, which exhibits excellent catalytic activity, in addition to exceptional stability.