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Abstract Over the last two decades, polymers with superior H₂/CO₂separation properties at 100–300 °C have gathered significant interest for H₂purification and CO₂capture. This timely review presents various strategies adopted to molecularly engineer polymers for this application. We first elucidate the Robeson's upper bound at elevated temperatures for H₂/CO₂separation and the advantages of high‐temperature operation (such as improved solubility selectivity and absence of CO₂plasticization), compared with conventional membrane gas separations at ~35 °C. Second, we describe commercially relevant membranes for the separation and highlight materials with free volumes tuned to discriminate H₂and CO₂, including functional polymers (such as polybenzimidazole) and engineered polymers by cross‐linking, blending, thermal treatment, thermal rearrangement, and carbonization. Third, we succinctly discuss mixed matrix materials containing size‐sieving or H₂‐sorptive nanofillers with attractive H₂/CO₂separation properties.