Carbon emission reduction is an important measure to mitigate the greenhouse effect, which has become a hotspot in global climate change research. To contribute to this, here, we fabricated two Co-based metal-organic frameworks (Co-MOFs), namely, {[Co(NTB)(bib)]·(DMA)·(HO)} (DZU-211) and {[Co(NTB)(bmip)]·(DMA)} (DZU-212) (HNTB = 4,4',4″-nitrilotribenzoic acid, bib = 1,4-bis(imidazol-1-yl)-butane, bmip = 1,3-bis(2-methyl-1-imidazol-1-yl)propane) to realize efficient CO/N separation by dividing coordination spaces into suitable pores with narrow windows. DZU-211 reveals a 3D open porous framework, while DZU-212 exhibits a 3D double-fold interpenetrated structure. The two MOFs both possess large coordination spaces and small open pore sizes, via the bib ligand insertion and framework interpenetration, respectively. Comparatively, DZU-211 reveals superior selective CO uptake properties due to its more suitable pore characteristics. Gas sorption experiments show that DZU-211 has a CO uptake of 52.6 cm g with a high simulated CO/N selectivity of 101.7 (298 K, 1 atm) and a moderate initial adsorption heat of 38.1 kJ mol. Moreover, dynamic breakthrough experiments confirm the potential application of DZU-211 as a CO separation material from postcombustion flue gases.
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