二氧化矽負載鈮氧化物的製備與優化應用於催化甘油縮醛反應之研究

甘瑋甄

doi:10.6342/NTU201700577

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二氧化矽负载铌氧化物的制备与优化应用於催化甘油缩醛反应之研究

Synthesis and Optimization of SiO2 Supported Niobium Oxide for the Catalytic Acetalization of Glycerol

甘玮甄 , 硕士　　导师：刘雅瑄　　

繁体中文 DOI： 10.6342/NTU201700577

甘油；丙酮；含浸法；缩醛化；丙酮缩甘油；铌氧化物； Glycerol ； Acetone ； Impregnation ； Solketal ； Niobium oxide

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摘要 │ 参考文献 (63) │ 国际计量

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Silica oxide supported niobium oxide was prepared through the impregnation method. We use niobium(V) chloride as a precursor instead of niobium ethoxide which is a high-cost precursor. However, it presented a problem that strong bonding between niobium and chloride causes residual chloride compound on the surface. In the synthesis process, three optimized steps were adopted to improve surface property. First, the step of ultasonication is to disperse niobium oxide on silica for improving the surface homogeneity which is one of shortcomings in impregnation method. Raman Spectra shows that sonication for 1 hour improves the surface homogeneity. Second, DI water was used to remove surface chloride compound. Energy-dispersive X-ray spectrum shows that DI water removed the residual chloride successfully. Finally, calcined condition was changed to modified the surface niobium species for obtaining more acidity sites. UV-Vis adsorption spectrum and X-ray diffraction spectrum indicated that material calcined at 550°C in 10 wt% niobium loading exhibited the formation of Nb2O5 crystalline phase. Moreover, the material calcined 500°C for 1 hour posscesses distorted amorphous NbO4 which has more acid sites.   
Silica supported niobium oxide is applied in glycerol acetalization, increasing the economic benefits of glycerol and integrating production chain of biodiesel industry. Glycerol can be acetalized with acetone to produce 5-membered ring 2,2-dimethyl-1,3-dioxolane-4-ylmethanol (solketal) and the 6-membered ring 2,2-dimethyl-1,3-dioxan-5-ol. Despite of the solketal selectivity and glycerol conversion, we use Operando Raman Spectroscopy to monitor the reaction. Operando Raman offers the interaction of molecular to understand the path of reaction.  
Different loading niobium supported on silica were applied in glycerol acetalization. The conversion results show that higher niobium loading causes high glycerol conversion, and 15 wt% niobium loading possesses the best glycerol conversion (45.6%). However, 30 wt% and 40 wt% have low glycerol conversions relatively. From the characteristic analysis, UV-Vis adsorption spectrum results indicated that low loading niobium materials present distorted amorphous niobium species, however, high niobium loading materials cause small niobium crystallinity on the surface. The acidity analysis includes Pyridine adsorption- Fourier Transform Infrared Spectroscopy (Pyridine adsorption-FTIR) and NH3-Temperature Programmed Desorption (NH3-TPD). The NH3-TPD result shows that the glycerol conversion related to the amount of acid sites. Pyridine adsorption-FTIR indicated that low loading niobium materials only have Lewis acid sites, and more than 15 wt% niobium loading materials posscess Br?nsted acid sites and Lewis acid sites. Operando Raman spectra during reaction indicated that Br?nsted afforded more on converting hemiacetal into production.

参考文献 ( 63 ) 〈TOP〉

Aresta, M., Dibenedetto, A., Pastore, C. (2003). Synthesis and characterization of Nb(OR)4[OC(O)OR] (R = Me, Et, Allyl) and their reaction with the parent alcohol to afford organic carbonates. Inorganic Chemistry, 42(10), 3256–61.
连结：
Aronne, A., Marenna, E., Califano, V., Fanelli, E., Pernive, P., Trifuoggi, M. (2007). Sol-gel synthesis and structural characterization of niobium-silicon mixed-oxide nanocomposites. Sol-Gel Sci Techanol, 43(2), 193–204.
连结：
Brayner, R., Bozon-Verduraz, F. (2003). Niobium pentoxide prepared by soft chemical routes: morphology, structure, defects and quantum size effect. Physical Chemistry Chemical Physics, 5(7), 1457–1466.
连结：
Brown, W. H. (1999). Introduction to organic chemistry: 2nd Edition. Wiley, New York
连结：
Brunauer, S., Emmett, P. H., Teller, E. (1938). Gases in Multimolecular Layers. Journal of the American Chemical Society, 60(1), 309–319.
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DOI可强化引用精确性、增强学术圈连结，并给予使用者跨平台的良好使用经验，目前在全世界已有超过五千万个对象申请DOI。如想对DOI的使用与概念有进一步了解，请参考（）。