Catalyst-free soft-template synthesis of ordered mesoporous carbon tailored using phloroglucinol/glyoxylic acid environmentally friendly precursors

Abstract

Carbon porous materials with a periodically ordered pore structure, controlled pore size and geometry and high thermal stability are synthesized using self-assembly of environmentally friendly phloroglucinol/glyoxylic acid precursors with an amphiphilic triblock copolymer template. Glyoxylic acid, a plant-derived compound, is used for the first time as a substituent of carcinogen formaldehyde usually employed in such a synthesis. Thanks to the double functionality, i.e., aldehyde and carboxylic acid, glyoxylic acid plays not only the role of a cross-linker for the formation of the resin but also the role of a catalyst by creation of H-bonding or specific reactions between the precursors. Hence, no extra catalyst such as strong acids (HCl) or bases (NaOH) is any longer required. Carbon films and powders were successfully prepared with high surface areas (up to 800 m² g⁻¹), high porous volume (up to 1 cm³ g⁻¹), tunable pore size (0.6 nm to 7 nm) and various pore architectures (hexagonal, cubic, and ink-bottle) by tuning the precursor ratio and by applying different manufacturing engineering strategies. Insights on the synthesis mechanism of the phenolic resin and carbon mesostructures were obtained using several analysis techniques, i.e., nuclear magnetic resonance (¹³C NMR) and FTIR spectroscopy, temperature programmed desorption coupled with mass spectrometry (TPD-MS) and thermo-gravimetric analysis (TGA).