Efficient purification of ethylene (C₂H₄) from ethane (C₂H₆) is a crucial but daunting task for the chemical industry given their similar physical natures and molecular dimensions. Reversed capture of C₂H₆ from C₂H₆/C₂H₄ dual-mixtures can be expected to directly yield high-purity C₂H₄ through a one-step separation unit, but it remains a daunting challenge. Here, we skillfully target an unusual "electrostatic-driven linker microrotation" (EDLM) in a Zr-MOF through coupling dual-ligands having electron-withdrawing/donating groups (e.g., F and CH₃ motifs). EDLM triggered microrotation of linker geometry and screening sites not only enhanced structural rigidity and hydrophobic nature, etc., but also effectively purified C₂H₄ through reversely trapping C₂H₆. Under ambient conditions, 1 kg of activated 2 adsorbents directly produces 7.2 L of C₂H₄ with over 99.9%+ purity in a single breakthrough operation starting from the equimolar C₂H₆/C₂H₄ cracked mixtures. Geometrical models and simulations have revealed that EDLM-derived H-bonding interaction and microrotation of linker geometry, synergistically customized C₂H₆-selective screening sites and pore inert for reversed C₂H₆ capture and improved surface hydrophobicity. Adsorption isotherms, modeling simulations, and breakthrough tests based on pressure swing adsorption (PSA) conditions have jointly elucidated the underlying separation properties for C₂H₄ purification. The enhanced hydrophobic nature, cycling durability, and separation property awarded 2 a new benchmark adsorbent to purify the olefin/paraffin mixtures.

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