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Synthesis and Characterization of Nanocomposite-Based Heteropolyacid, and its Catalytic, Photocatalytic and Electrochemical Performances

机译:纳米复合杂多酸的合成,表征及其催化,光催化和电化学性能

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This work reports the synthesis and characterization as well as catalytic, photocatalytic and electrochemical performances of a novel supported catalyst based on H5PMo10V2O40 Keggin type polyoxometalate (PMoV) immobilized on melamine grafted graphene oxide (Mel-GO). The supported catalyst (PMoV@Mel-GO) was characterized by X-ray diffraction spectroscopy (XRD), field emission scanning electron microscopy (FESEM), furrier transforms infrared spectroscopy (FT-IR), cyclic voltammetry (CV) and UV-vis diffuse reflectance spectroscopy (UV-DRS). Electrochemical characterizations revealed that modified graphene oxide nano-sheets have excellent photocatalytic activity towards electron transfer. Electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) spectroscopy confirmed the role of Keggin type polyoxometalate in charge transfer and electron transfer changes. The electroactive surface areas of the pure CPE and catalyst/CPE were appraised by CV technique confirming that for supported catalyst, modified electrode is approximately greater than that for pure CPE. For the optimization of main factors in photocatalytic activity, a statistical method called response surface methodology (RSM) based on the central composite design (CCD) was used to economize on the number of experiments and their meaningful interpretations. The supported catalyst showed high photocatalytic activity and reusability in the degradation of methylene blue (denoted as MB) as pollutant. Optimization results for initial dye concentration 20 mg/L showed that maximum degradation efficiency, 97.71%, was achieved at optimum conditions, catalyst amount 17.5 mg and pH= 6.1 for reaction time 66 min. In addition, the catalyst showed high activity in the desulfurization of dibenzothiophene (abbreviated as DBT) to dibenzothiophene sulfone product o (denoted as DBTO2) using formal batch method with 98.2% conversion at 50 C. In addition, the sulfone product was characterized by NMR, FT-IR, Mass spectroscopy and GC analysis. The optimal ° conditions for conversion of DBT were found to be; H2O2 / DBT3:1, reaction temperature 50 C and reaction time 120 min for 0.05 g catalyst amount.
机译:这项工作报告了基于H5PMo10V2O40固定在三聚氰胺接枝氧化石墨烯(Mel-GO)上的H5PMo10V2O40 Keggin型多金属氧酸盐(PMoV)的新型负载型催化剂的合成,表征以及催化,光催化和电化学性能。负载型催化剂(PMoV @ Mel-GO)通过X射线衍射光谱(XRD),场发射扫描电子显微镜(FESEM),傅里叶变换红外光谱(FT-IR),循环伏安法(CV)和紫外可见光谱进行表征。漫反射光谱法(UV-DRS)。电化学特征表明,改性的氧化石墨烯纳米片对电子转移具有优异的光催化活性。电化学阻抗光谱(EIS)和循环伏安法(CV)光谱证实了Keggin型多金属氧酸盐在电荷转移和电子转移变化中的作用。通过CV技术评估了纯CPE和催化剂/ CPE的电活性表面积,证实了负载型催化剂的改性电极大约比纯CPE的大。为了优化光催化活性的主要因素,基于中央复合设计(CCD)的统计方法称为响应表面方法(RSM)被用于节省实验次数及其有意义的解释。负载型催化剂在降解作为污染物的亚甲基蓝(表示为MB)方面显示出高的光催化活性和可重复使用性。初始染料浓度20 mg / L的优化结果表明,在最佳条件,催化剂量17.5 mg和pH = 6.1的条件下,反应时间66分钟,最大降解效率达到97.71%。另外,该催化剂在50℃下以98.2%的转化率使用正式间歇法在二苯并噻吩(缩写为DBT)脱硫为二苯并噻吩砜产物o(表示为DBTO2)中表现出高活性。此外,该砜产物通过NMR进行了表征。 ,FT-IR,质谱和GC分析。发现DBT转化的最佳°条件为: H2O2 / DBT3:1,反应温度为50℃,反应时间为120分钟(对于0.05克催化剂)。

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