Terephthalaldehyde (T)-phloroglucinol (POL) aerogels (TPOL) were synthesized via a novel acid-catalyzed (HCl) gelation process, which is completed in less than 2 h at room temperature. Based on the stoichiometry of the reaction (Scheme 1), the T:POL mol ratios were set at 1:2 and 3:4 and all starting materials were incorporated into the framework with no side products, as expected from a condensation polymerization. In analogy to resorcinol-formaldehyde aerogels, the mechanism may involve o-quinomethine intermediates, which are responsible for the red color dominant throughout the process. The bulk densities of TPOL aerogels could be as low as 0.2 g cm-3, the porosity as high as 80% v/v of empty space, and the surface areas can reach 500 m2 g-1, of which 19% (93 m2 g-1) is attributed to micropores. TPOL aerogels were carbonized via pyrolysis first at 240 0C in air followed by treatment at 800 0C under argon. Etching with CO2 at 1000 °C increases the BET surface area of TPOL to 1600 m2 g-1 .The structural, physical, and chemical composition at various stages along processing were studied with DSC, TGA, SEM, SAXS, FTIR, N2-sorption porosimetry, elemental analysis, and solid-state 13C NMR. Their high carbonization yield (~80% w/w), together with high BET surface areas (&gt; 620 m2 g-1), high porosity (88% v/v), and microporosity renders TPOL-derived C-aerogels viable candidates as electrodes for fuel cells, batteries and solar energy collectors.

Synthesis and characterization of robust terephthalaldehyde-phloroglucinol (TPOL) aerogels as precursors for nanoporous carbons

249th National Meeting (2015)

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