In this work, the
role of phenolic compounds in the hydrothermal
synthesis of carbon-encapsulated iron nanoparticles (CEINs) was studied.
To model phenolic compounds, gallic acid (GA) was selected, with glucose
as the carbon source. Iron was found as α-Fe2O3, γ-Fe2O3, Fe3O4, and zero-valent iron (ZVI) depending on the synthesis pH
and GA/Fe molar ratio. For GA/Fe = 1, the CEINs’ yield increased
significantly. In the samples with phenolics, increasing the initial
pH increased the amount of γ-Fe2O3 and
Fe3O4 and enhanced the iron oxide encapsulation
due to enhanced chelating ability. Reducing the GA/Fe ratio to 0.2
resulted in CEINs with stronger magnetization due to the presence
of Fe3O4. Ash weight, HCl digestion, and Raman
spectroscopy were used in conjunction to characterize the composition
of the CEINs. The magnetization of the samples was compared using
a simple magnetic weight setup. A scheme for the reactions occurring
during the hydrothermal carbonization of GA–Fe complexes was
proposed.