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A bifunctional POM-based Cu-viologen complex with mixed octamolybdate clusters for rapid oxidation desulfurization and effective photogeneration of hydrogen

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Abstract

The design and synthesis of catalysts for the oxidation desulfurization and production of hydrogen are extremely important for solving environmental pollution and energy shortage. Herein, a novel bifunctional [α-Mo8O26]4−/[β-Mo8O26]4−-based Cu-viologen complex H4[Cu2ICl2(Hbcbpy)4][α-Mo8O26][β-Mo8O26]·H2O (BHU-2, Hbcbpy = 1-(4-carboxybenzyl)-4,4’-bipyridinium) was synthesized and characterized by single-crystal X-ray diffraction (XRD), infrared radiation spectra, powder X-ray diffraction (PXRD) and X-ray photoelectron spectroscopy (XPS) spectra. The structural characteristic of BHU-2 is the presence of two types of octamolybdate clusters [α-Mo8O26]4−/[β-Mo8O26]4− and a new binuclear CuI-Hbcbpy complex linked by Cl-bridges [Cu2ICl2(Hbcbpy)4]4+. BHU-2 as a heterogeneous catalyst exhibits excellent activities to the oxidation desulfurization and photocatalytic hydrogen production. At room temperature, BHU-2 can catalyze 96% conversion of methyl phenyl sulfide with 98% selectivity, and the process obeys the pseudo-first-order reaction kinetic with the half-life of 9.6 min. The notorious 2-chloroethyl ethyl sulfide can achieve 99% conversion with 98% selectivity within only 1 min at the presence of BHU-2, and the turnover frequency (TOF) is up to 7400 h−1. BHU-2 also exhibits high catalytic activity for the oxidation of other aromatic and aliphatic thioethers within short time at room temperature. Furthermore, BHU-2 shows a high catalytic activity for visible-light-driven hydrogen evolution with an H2 evolution rate of 1677.85 µmol·g−1·h−1 within 10 h. Moreover, the catalytic activities do not decrease evidently after three cycles, revealing the prominent structural stability and recyclability.

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摘要

氧化脱硫和产氢催化剂的设计和合成对于解决环境污染和能源短缺问题具有极其重要的意义。本文合成了一种新型的双功能多酸基铜–紫精配合物H4[Cu2ICl2(Hbcbpy)4][α-Mo8O26][β-Mo8O26]·H2O (BHU-2, Hbcbpy = 1-(4-羧苄基)-4,4’-联吡啶), 并通过单晶X-射线衍射、IR、PXRD和XPS光谱等进行了表征。BHU-2的结构特征是存在两种类型的{Mo8}簇[α-Mo8O26]4−/[β-Mo8O26]4−和一种由Cl-桥连接的双核CuI-Hbcbpy配合物 [Cu2ICl2(Hbcbpy)4]4+。BHU-2作为一种非均相催化剂, 对氧化脱硫 (ODS) 和光催化产氢具有良好的活性。在室温下, BHU-2催化氧化甲基苯基硫醚 (MPS) 的转化率为96%, 选择性为98%, 该过程遵循一级反应动力学, 半衰期为9.6 min。在BHU-2存在下, 2-氯乙基乙基硫醚 (CEES) 在1 min内转化率可达到99%, 选择性为98%, TOF高达7400 h−1。BHU-2在室温及短时间内对其他芳香族和脂肪族硫醚的氧化也具有较高的催化活性。此外, BHU-2对可见光驱动的产氢具有较高的催化活性, 在10 h内产氢速率为1677.85 µmol·g−1·h−1。此外, 三次循环后催化活性没有明显下降, 表明结构具有较好的稳定性和可回收性。

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Acknowledgements

This study was financially supported by the National Natural Science Foundation of China (Nos. 22271021, 21901018 and 21971024), the Natural Science Foundation of Liaoning Province (No. 2022-MS-373) and Liaoning Revitalization Talents Program (No. XLYC1902011)

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  1. Lin Yang and Zhong Zhang have contributed equally to this work.

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  1. College of Chemistry and Materials Engineering, Bohai University, **zhou, 121013, China

    Lin Yang, Zhong Zhang, Chao-Nan Zhang & **u-Li Wang

  2. Professional Technology Innovation Center of Liaoning Province for Conversion Materials of Solar Cell, Bohai University, **zhou, 121013, China

    Lin Yang, Zhong Zhang, Chao-Nan Zhang & **u-Li Wang

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Yang, L., Zhang, Z., Zhang, CN. et al. A bifunctional POM-based Cu-viologen complex with mixed octamolybdate clusters for rapid oxidation desulfurization and effective photogeneration of hydrogen. Rare Met. 43, 236–246 (2024). https://doi.org/10.1007/s12598-023-02435-5

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  • DOI: https://doi.org/10.1007/s12598-023-02435-5

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