六角型中孔洞氧化釩觸媒的合成、鑑定及催化氧化反應

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题名:	六角型中孔洞氧化釩觸媒的合成、鑑定及催化氧化反應
其它题名:	Hexagonal Mesostructured Vanadium Oxide （HMVO）：Synthesis、Characterization and Catalytic Oxidation
作者:	朱芳瑩 Chu, F.Y
贡献者:	柯安男 Ko, An-Nan 東海大學化學系
关键词:	中孔型氧化釩 HMVO
日期:	2007
上传时间:	2011-03-21T06:33:24Z (UTC)
摘要:	利用直接水熱法合成六角型中孔洞的氧化釩觸媒（HMVO），比較其和傳統的V2O5以及V2O5/Al2O3兩種觸媒在氧化反應中的催化性質。HMVO的物性鑑定設備包括X射線繞射儀、霍氏紅外線光譜儀、氫氣溫度程控還原、熱重分析儀、氮氣吸附儀、固態核磁共振儀以及掃描式電子顯微鏡。X射線繞射圖譜顯示未鍛燒的觸媒結構似層狀，鍛燒後之HMVO變成六角型；霍氏紅外線光譜呈現六角型中孔洞氧化釩的V=O鍵結；熱重分析儀測量升溫過程中觸媒重量的減少，獲知結構之變化；51V-NMR圖譜顯示觸媒在鍛燒前後皆為扭曲的四面體鍵結，結構並未被破壞，而購買的V2O5則為八面體的結構鍵結；氫氣溫度程控還原可以觀察出HMVO和V2O5的還原性質。利用批次反應器，催化二苯甲烷和第三丁基過氧化氫（TBHP）在一大氣壓下生成苯甲酮的烷基芳香族氧化反應。結果顯示反應條件：溫度60℃、轉速200 rpm、觸媒重量0.075 g以及溶劑醋酸具有良好的催化活性，除此之外，比較不同觸媒可以發現HMVO的反應活性大於V2O5及V2O5/Al2O3兩種觸媒，根據研究推論是因為觸媒HMVO有不同的組成、孔洞大小和結構。 The hexagonal mesostructured vanadium oxide（HMVO）was synthesized via hydrothermal method.Its catalytic properties were compared with those of traditional V2O5 and V2O5/Al2O3 catalysts. The samples were characterized by XRD, FT-IR, TRR of H2, TGA, N2-adsorption, 51V solid NMR and SEM techniques. The powder XRD patterns of uncalcined catalysts show lamellar structures, but hexagonal structures after calcinations. The FT-IR spectra reveals V=O bonding in the HMVO samples. The TGA technique shows the lose of catalyst weight with rising temperature, indicating its structural change. According to the 51V solid NMR results, both uncalcined and calcined HMVO exhibit distorted tetrahedral bonding, whereas V2O5 shows octahedral bonding. The reduction properties of both HMVO and V2O5 are obtained from TRR of H2.The catalysts were utilized in the oxidation reaction of diphenylmethane（DPM） and tert-butyl hydroperoxide to produce benzophenone at 1 atm in a batch reactor. Good catalytic results are observed under the following reaction conditions : 60℃, stirring speed 200 rpm, catalyst weight 0.075g and acetic acid as the solvent. In addition, HMVO owns the best catalytic activity as compared to V2O5 and V2O5 / Al2O3 due to its characteristic composition, pore size and structure.
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