Hierarchically porous polymers combine microporosity, mesoporosity, and macroporosity to enhance pore accessibility and transport. This work describes generating hierarchically porous polymers and carbons derived therefrom by combining emulsion-templated macroporous polymers bearing novel macromolecular structures with simultaneous Friedel−Crafts hyper-cross-linking and porogen removal. The hyper-cross-linking was based on a copolymer of vinylbenzyl chloride and divinylbenzene, while the porogen was based on poly(εcaprolactone) (PCL). The two polymer systems were combined using one-pot syntheses of either simultaneous interpenetrating polymer networks (IPNs) containing a PCL-based poly(urethane urea) (PUU) or a PCL-based semi-IPN. In the semi-IPN, the microporosity was enhanced through hyper-cross-linking and through porogen removal during carbonization. The effects of incorporating a PCL-based PUU depended upon the diisocyanate. Unexpectedly, mesoporosity was generated from hyper-cross-linking an IPN synthesized with an aliphatic diisocyanate. On the other hand, the formation of interconnected networks from hyper-cross-linking an IPN synthesized with an aromatic diisocyanate enhanced both the microporosity and thermal stability.
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