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A family of azo‐bridged covalent organic polymers (azo‐COPs) was synthesized through a catalyst‐free direct coupling of aromatic nitro and amine compounds under basic conditions. The azo‐COPs formed 3D nanoporous networks and exhibited surface areas up to 729.6 m2 g−1, with a CO2‐uptake capacity as high as 2.55 mmol g−1 at 273 K and 1 bar. Azo‐COPs showed remarkable CO2/N2 selectivities (95.6–165...
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