The construction of functionalized covalent organic frameworks (COFs) is of great significance for broadening their potential applications, but is yet challenging to achieve, especially for three-dimensional (3D) COFs, because the connection of the building organic skeleton must strictly follow the pre-designed topology. Here we present the synthesis of two diamondyne-like 3D COFs (CPOF-2 and CPOF-3) functionalized with acetylene (-CC-) and diacetylene (-CC-CC-), respectively. The obtained COFs show a high crystallinity, permanent porosity, and chemical stability. Furthermore, CPOF-3 exhibited an extremely high volatile iodine uptake (as high as 5.87 g g), much higher than that of most reported COF-based adsorbents for iodine capture. Therefore, this study provides a new design principle to obtain high-performance iodine loading porous materials to solve the environmental pollution problem caused by radioactive iodine in the waste of the nuclear industry.
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