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石墨相氮化碳与甲磺酰氯的合成后衍生化：合成、表征及光催化作用

Post-Synthetic Derivatization of Graphitic Carbon Nitride with Methanesulfonyl Chloride: Synthesis, Characterization and Photocatalysis.

作者信息

Praus Petr, Smýkalová Aneta, Foniok Kryštof, Velíšek Petr, Cvejn Daniel, Žádný Jaroslav, Storch Jan

机构信息

Department of Chemistry, VŠB-Technical University of Ostrava, 700 80 Ostrava, Czech Republic.

Institute of Environmental Technology, VŠB-Technical University of Ostrava, 708 00 Ostrava, Czech Republic.

出版信息

Nanomaterials (Basel). 2020 Jan 22;10(2):193. doi: 10.3390/nano10020193.

DOI:10.3390/nano10020193
PMID:31979003
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC7074974/
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 (CHSO) 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.

摘要

通过在550℃下加热三聚氰胺合成了块状石墨相氮化碳（CN），并通过在500℃下加热CN制备了剥离的CN（ExCN）。通过加热硫脲合成了硫掺杂的CN（S-CN），并通过基于CN与甲磺酰（CH₃SO₂）氯进行后合成衍生化的新方法制备了硫掺杂的CN（Mes-CN和Mes-ExCN）。通过常用的表征方法对所得纳米材料进行了研究，并通过在紫外A（UVA）照射下分解酸性橙7（AO7）来测试它们的光催化活性。改性CN中硫的含量按Mes-ExCN > Mes-CN > S-CN的顺序降低。光吸收以相反的方式降低，但未观察到对带隙能量有影响。通过高分辨率质谱（HRMS）确认了连接到伯胺和仲胺基团上的甲磺酰（甲磺基）基团。光催化活性按Mes-ExCN > ExCN > CN ≈ Mes-CN > S-CN的顺序降低。Mes-ExCN和ExCN的最高活性归因于吸附的酸性橙7（AO7）的量最多。此外，在Mes-ExCN的情况下，掺入CN晶格中的氯离子也增强了光催化活性。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/e426a22cabbd/nanomaterials-10-00193-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/2e296dc69bc8/nanomaterials-10-00193-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/09cb21932d5a/nanomaterials-10-00193-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/5588ca69e0aa/nanomaterials-10-00193-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/d9b59642513f/nanomaterials-10-00193-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/ed83291308a1/nanomaterials-10-00193-g005a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/a0574aafd3ec/nanomaterials-10-00193-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/81b95ba4ebb3/nanomaterials-10-00193-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/763087f2c433/nanomaterials-10-00193-g008.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/1a750dfccb18/nanomaterials-10-00193-g009.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/e426a22cabbd/nanomaterials-10-00193-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/2e296dc69bc8/nanomaterials-10-00193-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/09cb21932d5a/nanomaterials-10-00193-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/5588ca69e0aa/nanomaterials-10-00193-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/d9b59642513f/nanomaterials-10-00193-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/ed83291308a1/nanomaterials-10-00193-g005a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/a0574aafd3ec/nanomaterials-10-00193-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/81b95ba4ebb3/nanomaterials-10-00193-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/763087f2c433/nanomaterials-10-00193-g008.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/1a750dfccb18/nanomaterials-10-00193-g009.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ce10/7074974/e426a22cabbd/nanomaterials-10-00193-g010.jpg

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