臺灣博碩士論文加值系統

本研究以含鋅的金屬有機骨架(CHU-212及ZIF-8)做為硬模板，並以蒸汽輔助結晶法(Steam-assisted crystallization, SAC)製備出Zn/HZSM-5，同時與傳統初濕含浸法製備的Zn/HZSM-5進行比較並探討於甲醇芳香化反應的差異。物化性鑑定顯示，所有含鋅觸媒的鋅皆良好地分散於HZSM-5的骨架中，而鋅物質可細分為ZnO及[Zn(OH)]+，其鋅物質組成的比例會受合成觸媒的方法與硬模板材料而有所差異，其中以ZIF-8為硬模板且使用蒸汽輔助結晶法製備的觸媒有最多的[Zn(OH)]+，而[Zn(OH)]+為具有脫氫的活性，因此於甲醇芳香化反應中有最好的觸媒反應性。一系列的觸媒物化性鑑定，例如: XRD、ICP、TEM、SEM、BET、TGA、NH3-TPD、IPA-TPD、Pyridine-IR、CO-IR、XPS、CO-TPSR及Methanol-TPSR等，將於本論文中詳細探討。

In this research, we used zinc-based MOFs (CHU-212 and ZIF-8) as hard templates and combined steam-assisted crystallization (SAC) to synthesize zinc-modified HZSM-5. These MOFs-derived catalysts were compared with conventional impregnation. Physicochemical characterization exhibited all zinc-modified catalysts had finely dispersed zinc species, including zinc oxide and [Zn(OH)]+ within HZSM-5; however, the relative ratio of zinc oxide and [Zn(OH)]+ varied depending on different synthesis strategies and hard templates. Using ZIF-8 as the hard template in combined with SAC strategy produced the highest concentration of [Zn(OH)]+ in all zinc-modified HZSM-5. The highest concentration of [Zn(OH)]+ of Zn/HZ-ZIF is related to its better performances in the aromatization of methanol due to the dehydrogenation activity of [Zn(OH)]+. All the tested catalysts were characterized by using various techniques, including XRD, ICP-AES, TEM, SEM, BET, TGA, NH3-TPD, IPA-TPD, Pyridine-IR, CO-IR, XPS, CO-TPSR and Methanol-TPSR.

摘要 I
英文延伸摘要 II
誌謝 VII
目錄 VIII
表目錄 XI
圖目錄 XII
第一章、前言 1
第二章、文獻回顧 3
2.1金屬有機骨架(Metal-organic frameworks, MOFs) 3
2.2沸石觸媒的特性 9
2.3甲醇芳香化的反應機制 14
2.4沸石觸媒改質的研究 18
第三章、實驗 21
3.1 實驗藥品與設備 21
3.2儀器介紹和操作條件 25
3.2.1 X光繞射儀(X-ray diffraction, XRD) 25
3.2.2 X光電子能譜儀(X-ray photoelectron spectroscopy, XPS) 26
3.2.3氮氣吸脫附(Nitrogen adsorption-desorption) 27
3.2.4高解析穿透式電子顯微鏡(High-resolution transmission electron microscopy, HR-TEM) 28
3.2.5高解析掃描式電子顯微鏡(High-resolution scanning electron microscopy, HR-SEM) 29
3.2.6感應耦合電漿原子放射光譜儀(Inductively coupled plasma atomic emission spectroscopy, ICP-AES) 30
3.2.7自動式化學吸脫附儀(AutoChem) 31
3.2.8傅里葉紅外光譜儀(Fourier-transform infrared spectroscopy, FTIR) 33
3.2.9熱重分析儀(Thermogravimetric analysis, TGA) 36
3.2.10氣相層析儀(Gas chromatography, GC) 36
3.3觸媒合成和命名 40
3.4甲醇芳香化反應和觸媒壽期測試 42
第四章、結果與討論 44
4.1觸媒結構和組成鑑定 44
4.1.1結晶性鑑定(XRD) 44
4.1.2觸媒組成鑑定(ICP-AES) 48
4.1.3觸媒高解析度穿透式電子顯微鏡圖像(HR-TEM) 48
4.1.4硬模板材料與觸媒表面形貌鑑定(HR-SEM) 50
4.1.5觸媒氮氣物理吸脱附結果(BET) 55
4.2觸媒酸性鑑定 58
4.2.1觸媒氨氣程溫脫附(NH3-TPD) 58
4.2.2觸媒異丙胺程溫脫附(IPA-TPD) 58
4.2.3吡啶化學吸附紅外光譜(Py-IR) 59
4.3觸媒中鋅物質的鑑定 65
4.3.1一氧化碳化學吸附紅外光譜(CO-IR) 65
4.3.2 X光電子能譜儀(XPS) 66
4.3.3一氧化碳程溫表面反應(CO-TPSR) 68
4.4觸媒於甲醇芳香化反應 70
4.4.1反應性探討 70
4.4.2觸媒壽期和積碳 74
第五章、結論 77
第六章、參考文獻 78
附錄 88

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