The facile and environmentally friendly synthesis of porous organic polymers with designed polar functionalities decorating the interior frameworks as an excellent adsorbent for selective carbon dioxide capture and metal ion removal is a target worth pursuing for environmental applications. In this regard, two azo-linked porous organic polymers denoted man-Azo-P1 and man-Azo-P2 were synthesized in water by the azo-linking of 4,4′-diaminobiphenyl (benzidine) and 4,4′-methylenedianiline, respectively, with 1,3,5-trihydroxybenzene. The resulting polymers showed good BET surface areas of 290 and 78 m 2 g –1 for man-Azo-P1 and man-Azo-P2, respectively. Due to the enriched core functionality of the azo (−N=N−) and hydroxyl groups along with the porous frameworks, man-Azo-P1 exhibited a good CO 2 uptake capacity of 32 cm 3 g –1 at 273 K and 1 bar, in addition to the remarkable removal of lead (Pd), chromium (Cr), arsenic (As), nickel (Ni), copper (Cu), and mercury (Hg) ions. This performance of the synthesized man-Azo-P1 and man-Azo-P2 in the dual application of CO 2 capture and heavy metal ion removal highlights the unique properties of azo-linked POPs as excellent and stable sorbent materials for the current challenging environmental applications.

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