NMR investigation on the occurrence of Na species in porous carbons prepared by NaOH activation Original Research Article

A detailed investigation was conducted about the process of alkali activation of charred rice hulls using NaOH. A carbon-rich precursor was initially prepared from the pyrolysis of rice hulls under N2 atmosphere, part of it being leached with HF to remove silica. The precursor was then mixed with NaOH, heat-treated at activation temperatures from 600 to 800 °C, and part of the product was finally washed with distilled water. Thermogravimetric curves under O2 flux showed a strong reduction in the ash content of the activated samples, indicating the consumption of silica during the activation process. From X-ray diffractometry, 29Si, and 23Na NMR spectroscopy, it was possible to identify the formation of sodium carbonate and silicates in the non-washed samples. After washing, all these compounds were removed and specific surface area measurements indicated a substantial porosity development, with larger surface area values obtained for the samples prepared from the HF-leached precursor. The use of 23Na NMR spectroscopy indicated the retention of sodium in the washed samples, in a chemical environment distinct from carbonates and silicates. The shapes and positions of the observed resonance lines pointed to a disordered environment, associated with oxygenated surface groups within the porous structure of the activated carbons.