<p>This study addresses practical challenges associated with Hummers’ method and its modified protocols for the synthesis of graphene oxide (GO). The extensive use of harsh chemicals such as sodium nitrate (NaNO<sub>3</sub>), hydrogen peroxide (H<sub>2</sub>O<sub>2</sub>), and hydrochloric acid (HCl) during large-scale production complicates both the synthesis and purification processes. In the present approach, these commonly used chemicals were completely eliminated through controlled oxidation and a stirring-assisted diffusion technique, which ensured uniform chemical distribution and promoted the formation of well-defined GO structures. X-ray diffraction (XRD), Fourier-transform infrared (FTIR), Raman, UV–visible (UV–Vis), and ICP mass spectroscopic analyses confirmed that complete oxidation could be achieved using the diffusion method, with results comparable to those obtained using centrifugation. Furthermore, magnetic-stirring-assisted diffusion significantly accelerated the GO purification process. Detailed analysis revealed that the addition of H<sub>2</sub>O<sub>2</sub> could be entirely avoided through precise control of the oxidation process, whereas HCl washing could be eliminated by incorporating additional diffusion-based purification steps. This simplified protocol improved both the oxidation and purification stages, yielding highly oxidized graphite oxide with an interlayer spacing of 8.4&#xa0;Å. Mechanistic investigations further indicated that water plays a critical role in facilitating complete graphite oxidation. Consequently, the overall process was reduced to the use of only sulfuric acid (H<sub>2</sub>SO<sub>4</sub>) and potassium permanganate (KMnO<sub>4</sub>), followed by purification through diffusion in pure water. This work represents a significant advancement in the synthesis and purification of graphene oxide, providing a practical route toward the large-scale, cost-effective production of high-quality graphene-based materials.</p> Graphical abstract <p></p>

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Simplified water-assisted production of highly-oxidized graphene oxide via controlled oxidation and stirring-based diffusion

  • A M K L Abeykoon,
  • I K Fernando,
  • M H T Dulaj,
  • R C L De Silva,
  • R V Coorey,
  • I R M Kottegoda

摘要

This study addresses practical challenges associated with Hummers’ method and its modified protocols for the synthesis of graphene oxide (GO). The extensive use of harsh chemicals such as sodium nitrate (NaNO3), hydrogen peroxide (H2O2), and hydrochloric acid (HCl) during large-scale production complicates both the synthesis and purification processes. In the present approach, these commonly used chemicals were completely eliminated through controlled oxidation and a stirring-assisted diffusion technique, which ensured uniform chemical distribution and promoted the formation of well-defined GO structures. X-ray diffraction (XRD), Fourier-transform infrared (FTIR), Raman, UV–visible (UV–Vis), and ICP mass spectroscopic analyses confirmed that complete oxidation could be achieved using the diffusion method, with results comparable to those obtained using centrifugation. Furthermore, magnetic-stirring-assisted diffusion significantly accelerated the GO purification process. Detailed analysis revealed that the addition of H2O2 could be entirely avoided through precise control of the oxidation process, whereas HCl washing could be eliminated by incorporating additional diffusion-based purification steps. This simplified protocol improved both the oxidation and purification stages, yielding highly oxidized graphite oxide with an interlayer spacing of 8.4 Å. Mechanistic investigations further indicated that water plays a critical role in facilitating complete graphite oxidation. Consequently, the overall process was reduced to the use of only sulfuric acid (H2SO4) and potassium permanganate (KMnO4), followed by purification through diffusion in pure water. This work represents a significant advancement in the synthesis and purification of graphene oxide, providing a practical route toward the large-scale, cost-effective production of high-quality graphene-based materials.

Graphical abstract