The oxidative exfoliation of graphite is a promising approach to the large-scale production of graphene. Conventional oxidation of graphite essentially facilitates the exfoliation process; however, the oxidation procedure releases toxic gases and requires extensive, time-consuming steps of washing and reduction to convert exfoliated graphene oxide (GO) into reduced graphene oxide (rGO). Although toxic gases can be controlled by modifying chemical reactions, filtration, dialysis, and extensive sonication are unfavorable for large-scale production. Here, we report a complete, scalable, and green synthesis of GO, without NaNO3, followed by reduction with citric acid (CA). This approach eliminates the generation of toxic gases, simplifies the washing steps, and reduces the time required to prepare rGO. To validate the proposed method, we present spectroscopical and morphological studies, using energy-dispersive X-ray spectroscopy (EDS), UV-visible spectroscopy, infrared spectroscopy, Raman spectroscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Thermal gravimetric analysis (TGA) is used to analyze the thermal properties of GO and rGO. This eco-friendly method proposes a complete guideline protocol toward large-scale production of oxidized graphene, with potential applications in supercapacitors, fuel cells, composites, batteries, and biosensors.

Porous carbon materials are currently subjected to strong research efforts mainly due to their excellent performances in energy storage devices. A sustainable process to obtain them is hydrothermal carbonization (HTC), in which the decomposition of biomass precursors generates solid products called hydrochars, together with liquid and gaseous products. Hydrochars have a high C content and are rich with oxygen-containing functional groups, which is important for subsequent activation. Orange pomace and orange peels are considered wastes and then have been investigated as possible feedstocks for hydrochars production. On the contrary, orange juice was treated by HTC only to obtain carbon quantum dots. In the present study, pure orange juice was hydrothermally carbonized and the resulting hydrochar was filtered and washed, and graphitized/activated by KOH in nitrogen atmosphere at 800 °C. The resulting material was studied by transmission and scanning electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy, X-ray diffraction, and nitrogen sorption isotherms. We found porous microspheres with some degree of graphitization and high nitrogen content, a specific surface of 1725 m2/g, and a pore size distribution that make them good candidates for supercapacitor electrodes.

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