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研究生： 劉祐誠
Yu-Cheng Liu
論文名稱： 銥觸媒對甲烷碳-氫鍵活化與碳-氧鍵偶合作用之研究
C-H Activation and C-O Coupling of Methane using Ir Catalysts
指導教授： 林昇佃
Shawn D. Lin
口試委員: 林昇佃
Shawn D. Lin
江志強
Jyh-Chiang Jiang
曾堯宣
Yao-Hsuan Tseng
俞聖法
Sheng-Fa Yu
楊家銘
Chia-Min Yang
學位類別： 博士
Doctor
系所名稱： 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年： 2018
畢業學年度： 106
語文別： 英文
論文頁數： 208
中文關鍵詞： 氧化銥 、臨場光譜分析 、甲烷活化/轉化 、甲烷蒸氣重組 、產氫
外文關鍵詞： IrO2, In situ Spectroscopic Analyses, CH4 Activation/Conversion, Steam reforming of CH4, H2 Production
相關次數： 點閱：412  下載：0 
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    • 金屬氧化物奈米顆粒具有獨特的物理化學及催化特性，是許多學者嘗試開發應用於甲烷低溫轉化處理的催化劑。本研究主要是合成出以銥為主的奈米觸媒，並探討其對於甲烷轉化反應的催化作用，希望藉此能開發出高效甲烷催化觸媒。本研究分為兩大主題：首先是以氧化銥(IrO2)奈米顆粒進行甲烷活化/轉化的測試，另一主題則是將銥原子分散於二氧化鈦載體上，進行甲烷蒸氣重組的評估。
    (I). 在第一個主題，主要以化學氧化/還原法製備IrO2，經500 oC鍛燒後形成約7 nm之金紅石(Rutile)結構IrO2，由臨場拉曼光譜(in situ Rama)觀察到在-105 oC即可催化甲烷活化/轉化，甲烷會進行脫氫，並與表面晶格氧(Obr)進行碳-氧偶合反應，形成CH2Obr與H2Obr物種，同時由臨場X光光譜(in situ XRD)也觀察到同時有IrO2部分還原，臨場紅外光譜(in situ DRIFT)觀察到室溫下甲烷活化/轉化形成CO2與H2O脫附，由電子密度泛函理論(DFT)證實IrO2低溫甲烷活化/轉化之上述反應作用，而IrO2 (211)較IrO2 (110)具有更低的反應能障利於反應進行。
    (II). 在第二主題，則以化學還原法製備高分散性銥擔載觸媒(Ir/TiO2)，所製備之2 wt % Ir/TiO2中Ir平均粒徑為1.31 nm，觸媒分散度為76.5 %，TEM並顯示有單原子分散態的Ir。在質量空間速率(WHSV)為 1.5 gCH4 gcat-1 h-1、蒸氣/甲烷比(S/M)為2.72及溫度350-600 oC條件下可有效進行甲烷蒸氣重組(SRM)，並在500 oC能穩定進行SRM反應48 h無失活現象發生，有接近理論氫氣產率(約4)的高H2產率且無CO生成。In situ Rama觀察到Ir/TiO2觸媒更可低至-125 oC即可進行甲烷活化/轉化反應，搭配in situ DRIFT證實，隨著溫度上升，甲烷脫氫至CHx (1 ≤ x ≤ 2)，並與羥基(OH)和表面晶格氧(Obr)進行碳-氧偶合反應形成CHxOy (0 < x ≤ 2, 1 ≤ y ≤ 3)，隨著脫氫或表面歧化以形成CO2，同時有效產氫。

    In recent years, several studies have demonstrated that metal oxides have excellent prospects for use in catalysis reaction owing to their physical and chemical properties. Recent experimental studies indicate a high interest in using metal-oxide catalysts for the C-H activation and for converting methane (CH4).under mild condition. The conversion of CH4 not only reduces the unnecessary emission of CH4 but also harvests useful chemicals. The goal of this research was to synthesize the high-performance of Ir-based nanomaterials for converting the CH4. Two kinds of CH4 application with important significance and applications were selected for study and development; namely, subambient CH4 activation/conversion and steam reforming of CH4 (SRM). The following research topics have been addressed in this dissertation:
    (I). The similarly facile subambient CH4 activation/conversion over IrO2 nanoparticles under atmospheric pressure was studied. The IrO2 nanoparticles were prepared by a modified chemical redox method. The prepared IrO2 nanoparticles after calcined at 500 oC exhibited the rutile structure with an average particle size of ~7 nm. In situ Raman and X-ray diffraction (XRD) analyses reveal that CH4 activation/conversion begins with C-H cleavage followed by C-O coupling with the surface bridged (Obr) oxygen on IrO2 as low as -105 oC, while partial reduction of IrO2 appeared. Besides, C-H of CH2Obr and CH2 and OH of H2Obr adspecies can be observed. In situ diffuse reflectance infrared Fourier-transformed spectroscopy (DRIFTS) elucidates CH4 activation/conversion over IrO2 nanoparticles at ambient temperature and further converted to gaseous CO2 and H2O. Furthermore, the IrO2 (211) facet was more active than IrO2 (110) facet according to the lower reaction barriers on IrO2 (211) facet by density functional theory (DFT) calculation. This clearly shows that CH4 activation/conversion on IrO2 is a structure-sensitive reaction and the results of this study can provide insights for the development of efficient catalysts for CH4 utilization.
    (II). SRM has been an extremely important process for the production of H2 and syngas and is utilized on the industrial scale. The atomically dispersion Ir/TiO2 catalysts prepared by chemical reduction method was studied. The Ir/TiO2 catalysts with 2 wt % of Ir loading can achieve that high Ir dispersion (76.5 %) even at low metal loading, while Ir/TiO2 catalysts with an average Ir size of 1.31 nm were observed by TEM. The 2 wt % Ir/TiO2 catalysts readily catalyzed SRM to nearly the thermodynamic conversion at the weight hourly space velocity (WHSV) of 1.5 gCH4 gcat-1 h-1 and steam/CH4 = 2.7 from 350 - 600 oC. The catalyst stability under reaction conditions was confirmed by no coke formation after 48 h isothermal reaction at 500 oC and a H2 yield of approximately 4 mol per mol CH4 reacted was achieved, where CO2 is the main carbon-containing product without any CO selectivity. In situ Raman spectra indicate that CH4 can be activated as low as - 125 oC. In situ DRIFT spectra indicate that the proposed SRM mechanism over Ir/TiO2 catalysts involves CH4 dehydrogenation to CHx (1 ≤ x ≤ 2), followed by C-O coupling with surface bridged oxygen (Obr) and hydroxy group (OH) to form CHxOy (0 < x ≤ 2, 1 ≤ y ≤ 3) adspecies when temperature was ramping; these adspecies can be further converted to CO2 with accompanying the H2 formation through dehydrogenation and disproportionation. Thus, SRM over Ir/TiO2 catalysts can become an effective and sustainable approach for H2 production.

    Acknowledgement………………………………………………………………………………………I Chinese Abstract………………………………………………………………………………III English Abstract……………………………………………………………………………………V Table of Contents……………………………………………………………………………VII List of Figures………………………………………………………………………………………X List of Tables………………………………………………………………………………XVIII List of Tables……………………………………………………………………………………XIX Chapter 1 Introduction 1 1.1 Background 1 1.2 Objectives and Scope 3 Chapter 2 Literature Review 5 2.1 Partial Oxidation of Methane (POM) 9 2.1.1 Partial Oxidation of CH4 to CH3OH and HCHO 10 2.1.2 Direct Formation of CH3COOH from CH4 17 2.2 Methane Coupling Reactions 22 2.2.1 Oxidative Coupling of Methane (OCM) 23 2.2.2 Direct Coupling of Methane (DCM) 24 2.3 Other Oxidizers for Methane Activation/Conversion 28 2.3.1 H2S Steam Reforming of CH4 29 2.3.2 Sulfur as A Soft Oxidant for CH4 33 2.4 Steam Reforming of CH4 (SRM) 36 Chapter 3 Experiments Materials and Apparatus 40 3.1 Chemicals and gases 40 3.2 Instruments and Apparatus 42 3.3 Experimental procedures 51 3.3.1 Materials preparation 51 3.3.2 Computational Methods 55 3.3.3 Characterization and analyses 56 3.3.4 Test for Steam Reforming of Methane 58 Chapter 4 Subambient C-H Activation of Methane and Ethane over IrO2 Nanoparticles Probed by In situ Spectroscopic and Theoretical Studies 62 4.1 Introduction 62 4.2 Results and Discussion 66 4.2.1 Characterization of IrO2 66 4.2.2 In situ Raman and in situ XRD for CH4 activation 68 4.2.3 Thermogravimetric analysis of IrO2 74 4.2.4 In situ DRIFTS for activation/conversion of CH4 at ambient temperature 77 4.2.5 In situ DRIFTS for activation/conversion of CH4 at ambient temperature 80 4.2.6 H2O formation on IrO2 87 4.2.7 C2H6 activation by in situ Raman and in situ DRIFTS 90 4.3 Discussion 93 4.4 Summary 97 Chapter 5 Highly Active Supported Iridium Catalysts for Sustainable Hydrogen Production by Steam Reforming of Methane 98 5.1 Introduction 98 5.2 Results and Discussion 100 5.2.1 Characterization of Ir-TiO2 Catalyst 100 5.2.2 SRM test using Ir-TiO2 Catalyst 108 5.2.3 In situ Raman for SRM 118 5.2.4 In situ DRIFTS, ex situ UV-vis and ex situ UPS for SRM 121 5.3 Discussion 128 5.4 Summary 133 Chapter 6 Conclusions and Recommendation 133 Appendix A 136 Appendix B 141 Appendix C 153 Reference 158

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