Statistics design for the synthesis optimization of lignin-sulfonate sulfur-doped mesoporous carbon materials: promising candidates as adsorbents and supercapacitors materials

This study employed lignin-sulfonated (LS) to develop biobased carbon materials (LS-Cs) through a sulfur-doping approach to enhance their physicochemical properties, adsorption capabilities, and energy storage potentials. Various characterization techniques, including BET surface area analysis, SEM imaging, XPS, Raman spectroscopy, and elemental composition (CHNS), were employed to assess the quality of the LS-Cs adsorbent and electrode samples. Response Surface Methodology (RSM) was utilized for optimizing the two main properties (specific surface area, A_BET, and mesopore area, A_MESO) by evaluating three independent factors (i.e., activation temperature, ZnCl₂:LS ratio, and sulfur content). According to the statistical analysis, A_BET and A_MESO were affected by ZnCl₂ and sulfur content, while the pyrolysis temperature did not affect the responses in the studied conditions. It was found that increasing the ZnCl₂ and sulfur contents led to an increment of the A_BET and A_MESO values. The LS-C materials exhibited very high A_BETvalues up to 1993 m² g^-1 and with predominantly mesoporous features. The S-doping resulted in LS-Cs with high sulfur contents in their microstructures up to 15% (wt%). The LS-C materials were tested as adsorbents for sodium diclofenac (DCF) adsorption and reactive orange 16 dye (RO-16) and as electrodes for supercapacitors. The LS-Cs exhibited excellent adsorption capacity values for both molecules (197-372 mg g^-1) for DCF, and (223-466 mg g^-1) for RO-16. When tested as electrodes for supercapacitors, notably, LS-C3, which is a doped sample with sulfur, exhibited the best electrochemical performance, e.g. high specific capacitance (156 F/g at 50 mV/s), and delivered an excellent capacitance after 1000 cycles (63 F/g at 1 A/g), which denotes the noteworthy capacitive behavior of the S-doped electrode. Thus, the present work suggests an eco-friendly resource for developing effective, productive carbon materials for adsorbent and electrodes for SC application. However, further studies on the complete application of these materials as adsorbents and electrodes are needed for a deeper understanding of their behavior in environmental and energy storage applications.