Abstract
Bulk graphitic carbon nitride (CN) was synthetized by heating of melamine at 550 °C, and the exfoliated CN (ExCN) was prepared by heating of CN at 500 °C. Sulfur-doped CN was synthesized by heating of thiourea (S-CN) and by a novel procedure based on the post-synthetic derivatization of CN with methanesulfonyl (CH3SO2−) chloride (Mes-CN and Mes-ExCN). The obtained nanomaterials were investigated by common characterization methods and their photocatalytic activity was tested by means of the decomposition of acetic orange 7 (AO7) under ultraviolet A (UVA) irradiation. The content of sulfur in the modified CN decreased in the sequence of Mes-ExCN > Mes-CN > S-CN. The absorption of light decreased in the opposite manner, but no influence on the band gap energies was observed. The methanesulfonyl (mesyl) groups connected to primary and secondary amine groups were confirmed by high resolution mass spectrometry (HRMS). The photocatalytic activity decreased in the sequence of Mes-ExCN > ExCN > CN ≈ Mes-CN > S-CN. The highest activity of Mes-ExCN and ExCN was explained by the highest amounts of adsorbed Acetic Orange 7 (AO7). In addition, in the case of Mes-ExCN, chloride ions incorporated in the CN lattice enhanced the photocatalytic activity as well.
Highlights
Graphitic carbon nitride is a semiconducting nanomaterial that has been intensively studied during the last decade owing to its interesting properties such as high thermal, chemical, and photochemical stability [1,2]
Unlike these synthesis procedures from S-containing precursors, our new approach was based on the post-synthetic derivatization of already prepared bulk and exfoliated carbon nitride (CN) [44] with suitable highly reactive chemical agents having sulfur in their structure such as mesyl chloride
The content of sulfur in S-CN, Mes-CN, and Mes-exfoliated CN (ExCN) was determined by the X-ray fluorescence spectroscopy (SPECTRO Xepos, SPECTRO Analytical Instruments GmbH Kleve, Germany) and elemental analysis (EA); see Table 1
Summary
Graphitic carbon nitride is a semiconducting nanomaterial that has been intensively studied during the last decade owing to its interesting properties such as high thermal, chemical, and photochemical stability [1,2]. The common way is the synthesis of CN from sulfur-rich organic compounds, such as benzyl disulphide [29], thiourea [30,31,32,33,34,35,36], trithiocyanuric acid [37,38,39,40], elemental sulfur [41], H2S [42], and sulfuric acid [43] Unlike these synthesis procedures from S-containing precursors, our new approach was based on the post-synthetic derivatization of already prepared bulk and exfoliated CN [44] with suitable highly reactive chemical agents having sulfur in their structure such as mesyl chloride. All new nanomaterials were prepared and their properties were studied by means of common characterization and the photocatalytic decomposition of the commonly utilized dye Acid Orange (AO7)
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