A novel flexible PAN fiber adsorbent was developed using an electrospinning technique with UTSA-16 (Co) and UTSA-16 (Zn) metal organic frameworks (MOFs). MOF powders with different ratios were dispersed within PAN fiber networks and processed to produce MOF crystalline layers under microwave irradiation for the seeded growth of MOFs. The PAN/UTSA-16 (Co) and (Zn) fiber mats exhibit 75% and 78% of the CO 2 adsorption capacities of pristine UTSA-16 (Co) and UTSA-16 (Zn), respectively, while a high CO 2 /N 2 selectivity of 113–128 is preserved. Stability experiments show that PAN/UTSA-16 (Zn) fibers are more robust under humid air, NO 2 , and SO 2 environments compared to PAN/UTSA-16 (Co). Additionally, the PAN/UTSA-16 fibers show excellent recyclability during ten adsorption-desorption cycles at 298 and 393 K. Morphology, porous properties, and crystallinity of the PAN/UTSA-16 fibers were examined using SEM, BET, and XRD. ● Flexible fiber mats with UTSA-16 (Co) and (Zn) were produced by using an electrospinning and microwave irradiation. ● PAN/UTSA-16 fiber mats show even better CO2 adsorption capacity and selectivity than powder adsorbents. ● Excellent recyclability was proven by a repeated adsorption-desorption at 298 and 393 K. ● Stability of PAN/UTSA-16 fiber mats under humid air, SO 2 , and NO 2 was evaluated for a practical application.
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