Abstract
This study presents the development of an environmentally benign and economically viable methodology for the synthesis of graphene-containing carbon materials derived from renewable agricultural residues, specifically walnut shells, rice husks, and apricot stones. The proposed synthesis route involves sequential stages of controlled pre-carbonization, desilicification, chemical activation with potassium hydroxide (KOH), and subsequent mild exfoliation, resulting in the formation of few-layer graphene with a high degree of structural ordering. Pre-carbonization carried out at 523–573 K, followed by activation at 1123 K, yields graphene sheets exhibiting a specific surface area of 1300–1800 m2/g, a carbon content of 60–90%, and an average pore diameter below 100 nm. The synthesized materials were subjected to comprehensive physicochemical characterization using BET surface area analysis, Raman spectroscopy, FTIR spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atomic absorption flame emission spectrophotometry. Raman spectroscopic analysis revealed an I_G/I_2D intensity ratio of approximately 1.5–2.0, indicating the presence of graphene structures consisting of approximately four to five layers. To enhance adsorption performance, the graphene-containing carbon materials were further functionalized with sulfuric acid, and the successful incorporation of surface functional groups was confirmed by FTIR spectroscopy. The adsorption properties of the functionalized graphene-containing carbon materials were evaluated in aqueous solutions containing sodium, potassium, calcium, and magnesium salts, demonstrating adsorption efficiencies of up to 80%. Compared to conventional biomass-derived graphene synthesis methods, the developed approach produces materials with enhanced porosity, higher graphitic ordering, and improved chemical purity. These characteristics highlight the strong potential of the synthesized graphene-containing carbon materials for applications in energy storage systems, adsorption-based water purification technologies, and environmentally sustainable nanotechnological applications.