Porous carbons are a highly versatile class of materials with applications inelectrochemical & energy devices, environmental remediation, membranes, and beyond. However, their performance critically depends on careful and controlled synthesis to impart essential properties. In particular, controlling the nanostructure is crucial for tuning surface area and porosity, which directly influences their effectiveness in applications such as batteries, supercapacitors and carbon capture. This study examines the role of a novel hypergolic synthetic protocol to produce highly porous activated carbons. Electron Spin Resonance (ESR) spectroscopy alongside complementary characterization techniques, was employed to investigate the presence and role of carbon radicals, shedding light on the underlying mechanism of KOH activation. Finally, these Hypergolic Porous Activated Carbons were tested as catalysts for the activation of peroxymonosulfate in the remediation of organic dyes. ESR analysis provided deeper insights into the free-radical driven degradation mechanism involved in pollutant removal.