Hierarchical zeolite composite nanofibers are designed using an electrospinning technique with post‐carbonization processing to form mechanically strong pellets for biogas upgrading. A ZSM‐5 nanopowder (zeolite) and a polyvinylpyrrolidone (PVP) polymer are electrospun to form ZSM/PVP composite nanofibers, which are transformed into a ZSM and carbon composite nanofiber (ZSM/C) by a two‐step heat treatment. The ZSM/C nanofibers show a 30.4% increase in Brunauer–Emmett–Teller (BET) surface area compared with the non‐structured ZSM‐5 nanopowder. Using ideal adsorbed solution theory, CO2‐over‐CH4 selectivity of 20 and CO2 uptake of 2.15 mmolg−1 at 293 K at 1 bar for ZSM/C nanofibers are obtained. For the efficient use of adsorbents in pressure swing adsorption operation, the nanofibers are structured into ZSM/C pellets that offer a maximum tensile strength of 6.46 MPa to withstand pressure swings. In the breakthrough tests, the CO2 uptake of the pellets reach 3.18 mmolg−1 at 293 K at 4 bar after 5 breakthrough adsorption–desorption cycles, with a much higher mass transfer coefficient of 1.24 ms−1 and CO2 uptake rate of 2.4 mg of CO2 g−1s−1, as compared with other structured zeolite adsorbents.
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