The rapid and scalable synthesis of hierarchical carbon monoliths with an ordered meso-structure and fully interconnected macropores has been demonstrated. Resorcinol and formaldehyde based polymers were used as the carbon precursor, triblock copolymer Plu-ronic F127 as the structural directing agent, and organic base lysine as both the polymerization catalyst and mesostructure assembly promoter. In the presence of lysine, homogeneous and crack-free polymer monoliths can be obtained through rapid gelation in 15 min at 90 °C. The polymer monoliths have a robust framework, which can be directly dried at 50 °C in air and carbonized at high temperature under a nitrogen atmosphere. The carbon monoliths are crack-free and have an ordered mesostructure with fully interconnected macropores. The surface area and the macropore volume are high with values up to 600 m~2 g~(-1) and 3.52 cm~3 g~(-1), respectively. Further steam activation of the carbon monolith can significantly improve the surface area to 2422 m~2 g~(-1) while still maintaining the ordered mesostructure.
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