Đurasović Izabela, Štefanić Goran, Dražić Goran, Peter Robert, Klencsár Zoltán, Marciuš Marijan, Jurkin Tanja, Ivanda Mile, Stichleutner Sándor, Gotić Marijan
Laboratory for Molecular Physics and Synthesis of New Materials, Division of Materials Physics, Ruđer Bošković Institute, Bijenička c. 54, 10000 Zagreb, Croatia.
National Institute of Chemistry, Hajdrihova 19, SI-1001 Ljubljana, Slovenia.
Nanomaterials (Basel). 2023 Sep 2;13(17):2481. doi: 10.3390/nano13172481.
In this study, we present a new approach for the synthesis of Pt/SnO catalysts using microwave radiation. Pt(IV) and Sn(IV) inorganic precursors (HPtCl and SnCl) and ammonia were used, which allowed the controlled formation of platinum particles on the anisotropic SnO support. The synthesized Pt/SnO samples are mesoporous and exhibit a reversible physisorption isotherm of type IV. The XRD patterns confirmed the presence of platinum maxima in all Pt/SnO samples. The Williamson-Hall diagram showed SnO anisotropy with crystallite sizes of ~10 nm along the c-axis (< >) and ~5 nm along the a-axis (< >). SEM analysis revealed anisotropic, urchin-like SnO particles. XPS results indicated relatively low average oxidation states of platinum, close to Pt metal. Sn Mössbauer spectroscopy indicated electronic interactions between Pt and SnO particles. The synthesized samples were used for the catalytic reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) in the presence of excess NaBH. The catalytic activity of the Pt/SnO samples for the reduction of 4-NP to 4-AP was optimized by varying the synthesis parameters and Pt loading. The optimal platinum loading for the reduction of 4-NP to 4-AP on the anisotropic SnO support is 5 mol% with an apparent rate constant = 0.59 × 10 s. The Pt/SnO sample showed exceptional reusability and retained an efficiency of 81.4% after ten cycles.
在本研究中，我们提出了一种利用微波辐射合成Pt/SnO催化剂的新方法。使用了Pt(IV)和Sn(IV)无机前驱体（HPtCl和SnCl）以及氨，这使得铂颗粒能够在各向异性的SnO载体上可控形成。合成的Pt/SnO样品为介孔结构，呈现IV型可逆物理吸附等温线。XRD图谱证实了所有Pt/SnO样品中铂峰的存在。威廉姆森-霍尔图显示了SnO的各向异性，其沿c轴（<>）的微晶尺寸约为10 nm，沿a轴（<>）约为5 nm。SEM分析揭示了各向异性的海胆状SnO颗粒。XPS结果表明铂的平均氧化态相对较低，接近Pt金属。Sn穆斯堡尔光谱表明Pt与SnO颗粒之间存在电子相互作用。合成的样品用于在过量NaBH存在下将4-硝基苯酚（4-NP）催化还原为4-氨基苯酚（4-AP）。通过改变合成参数和Pt负载量，优化了Pt/SnO样品将4-NP还原为4-AP的催化活性。在各向异性SnO载体上，将4-NP还原为4-AP的最佳铂负载量为5 mol%，表观速率常数 = 0.59 × 10 s。Pt/SnO样品表现出优异的可重复使用性，经过十次循环后仍保留81.4%的效率。
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