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A new class of core–shell adsorbents has been created by electrospun metal–organic framework (MOF) particles embedded in polymer nanofibers, which have provided many unique properties compared to the existing MOF coating technologies. For the first time, we demonstrate the improved adsorption selectivity of CO₂over N₂using electrospun polymer/ZIF‐8 adsorbents in experiments. Furthermore, an analytical model based on the assumption that the diffusivity in core is 10 times higher than that in shell is developed to describe the theory of improved selectivity for core–shell adsorbents that is validated against a more accurate finite element model developed in COMSOL. Our model shows three regimes including exclusive shell uptake, linear core uptake, and asymptotic core uptake. These regimes are related to material properties and uptake times, which could be used as design criteria to balance core stability, maximum selectivity, and maximum uptake. An advanced HAADF STEM tomography (MovieS1) shows that the shell thickness in the case of polymer/ZIF‐8 is on the order of 10 nm, allowing the regime of maximum selectivity to be realized. Kinetically limited adsorption tests at 45°C demonstrate that these composite fibers can perform in a regime of selectivity and uptake for the separation of CO₂and N₂that is unobtainablemore »by either the MOF or fiber independently, showing a great potential for postcombustion CO₂capture.

Direct air capture (DAC) of CO₂is an emerging technology in the battle against climate change. Many sorbent materials and different technologies such as moisture swing sorption have been explored for this application. However, developing efficient scaffolds to adopt promising sorbents with fast kinetics is challenging, and very limited effort has been reported to address this critical issue. In this work, the availability and kinetic uptake of CO₂in sorbents embedded in various matrices are studied. Three scaffolds including a commercially available industrial film containing ion‐exchange resin (IER), IER particles embedded in dense electrospun fibers, and IER particles embedded in porous electrospun fibers are compared, in which a solvothermal polymer additive removal technique is used to create porosity in porous fibers. A frequency response technique is developed to measure the uptake capacity, sorbent availability, and kinetic uptake rate. The porous fiber has 90% IER availability, while the dense fibers have 50% particle accessibility. The sorption half time for both electrospun fiber samples is 10 ± 3 min. Our experimental results demonstrate that electrospinning polymer/sorbent composites is a promising technology to facilitate the handleability of sorbent particles and to improve the sorption kinetics, in which the IER embedded in porous electrospun fibers shows the highestmore »cycle capacity with an uptake rate of 1.4 mol CO₂per gram‐hour. © 2018 American Institute of Chemical EngineersAIChE J, 65: 214–220, 2019