二氧化碳作為排放量最大的溫室氣體，如何抑止二氧化碳的排放在現今引起人們廣泛的注意，也因此發展出了許多策略來減緩二氧化碳排放至大氣中所引發的相關問題。其中將二氧化碳氫化轉換成碳氫化合物被認為是一個十分有效的方式，對於能源與化學品提供了有效的循環利用。本研究選用以銅金屬作為基底之混成式奈米材料作為觸媒，探討二氧化碳氫化反應合成化學品之應用。
第一部分的研究為探討以溶膠-凝膠法製備而成的Cu-ZnO混成式奈米材料催化二氧化碳氫化產甲醇之反應。在此方法中，以透過膠體穩定化之Al2O3奈米粒子作為載體，使用共沉澱合成方法將Cu (活性金屬)與ZnO (促進劑)擔載在載體上，形成分散良好的Cu-ZnO@Al2O3奈米粒子團簇。透過分析發現添加Al2O3奈米粒子作為載體，會增進樣品之金屬的分散度以及Cu-ZnO界面形成的鹼性點位數量，且透過胺基矽烷將Al2O3奈米粒子的表面官能化也有助於提升此混成結構的活性金屬表面積。透過使用Cu-ZnO@Al2O3奈米粒子團簇催化二氧化碳氫化產甲醇之反應，可以觀察到二氧化碳之轉化率與活性金屬表面積具有正相關的關係；當Al2O3於觸媒內的擔載量達到35-36 %時，具有最佳的選擇率 (47-49 %)，此結果與在該組成下觸媒材料具有最高的中等鹼性位點相符合。此部分研究顯示出基於對材料特性的理解所合成之混成式奈米材料針對二氧化碳氫化產甲醇之反應具有優異的催化表現。
在本研究的第二部分中，發展出能夠提高二氧化碳之平衡轉化率及甲醇選擇率之二氧化碳之氫化反應系統。在實驗上，透過加入一氧化碳與二氧化碳共同進行氫化反應來達成，並以擔載於Al2O3載體上的銅基底混成式觸媒作為催化劑。結果顯示出一氧化碳/二氧化碳之加氫甲醇化在低溫(220 °C)、高壓(30 bar)的反應條件下其甲醇空間產率(STYMeOH)最高可以達到6.1 mmolgcat-1h-1，約為原來的3.2倍。此部分的研究顯示出開發之混成式奈米觸媒材料在對催化一氧化碳/二氧化碳之加氫甲醇化反應具有相當優異的表現，並且對於Cu-ZnO界面在催化反應上的機制具有更深入的了解。
此研究為混成式奈米觸媒材料之合成開闢了新的視野，有助於對二氧化碳氫化反應於觸媒上的協同催化提供了更深入的了解與探討，期望可以再達成減少溫室氣體排放的同時也將其轉換為具有附加價值之化學品的目標。

Carbon dioxide (CO2) is by far the most emitted greenhouse gas; and the restraint of CO2 emission is yielding a great interest. There are several methods to mitigate the issue of CO2 emission to the atmosphere. CO2 hydrogenation to hydrocarbons, which in the past has showed great promise among these methods. It also offers an opportunity to build a sustainable strategy for energy and chemical production. A systematic study is carried out based on the development of facile approaches for fabricating Cu-based hybrid nanostructures as catalysts for the hydrogenation of CO2 to produce useful chemicals.
In the first stage of our research work, a facile sol-gel approach is demonstrated for the fabrication of Cu-ZnO-based hybrid nanostructures for the catalytic CO2 hydrogenation to methanol. The method combines colloid stabilization of Al2O3 nanoparticles (as support material) and controlled co-precipitation of Cu (active metal) and ZnO (promoter) onto the Al2O3 nanoparticles. The results show a successful synthesis of ultrafine Cu-ZnO nanocrystallites deposited on the Al2O3 nanoparticle clusters (Cu-ZnO@Al2O3). Hybridization with Al2O3 nanoparticles enhances metal dispersion and number of basic sites of the Cu-ZnO-based nanocatalyst. Aminosilane-based surface functionalization on the Al2O3 nanoparticle increases metal surface area in the hybrid nanostructure. The CO2 conversion catalyzed by the synthesized Cu-ZnO@Al2O3 is shown to be proportional to active surface area of the hybrid nanostructure. An optimum selectivity of the synthesized catalyst is identified (47-49 %) when the mass fraction of Al2O3 is 35-36 %, in correspondence to the highest moderate basicity of the synthesized hybrid nanostructures. The work demonstrates a prototype study of fabricating high-performance hybrid nanocatalyst with the support of mechanistic understanding in material synthesis for the synergistic catalysis of CO2 hydrogenation to methanol.
In the second stage, a catalytic reaction system is developed for the study of the CO2 hydrogenation with improved both equilibrium conversion ratio of CO2 and selectivity to methanol. Experimentally, a combined (CO2 + CO) hydrogenation process is proposed as an alternative two-stage route for methanol production. Cu-based hybrid catalysts supported on alumina nanoparticle clusters were developed for promoting methanol production. The results show an increase of 3.2 times in methanol space-time yield (STYMeOH) at 220 C by incorporating CO to the CO2 hydrogenation process, and the maximum STYMeOH, 6.1 mmolgcat-1h-1, was achievable under a low-temperature (220 C), moderate high-pressure operation (30 bar). The work demonstrates a rational design of hybrid nanostructured material to achieve superior catalytic performance in the combined (CO2 + CO) hydrogenation. The mechanistic understanding gives insights into the interfacial catalysis by Cu-ZnO hybrid nanostructured materials for methanol production.
In summary, we demonstrate a facile route for the fabrication of hybrid nanostructured catalyst material. The mechanistic understanding presented in this study gives insight into the study of synergistic catalysis for the CO2 conversion, achieving the goal of simultaneous production of value chemical production and reduction of greenhouse gas.

摘要 I
Abstract III
Table of contents V
List of figures VIII
List of tables XI
List of abbreviations XII
Chapter 1: Introduction 1
1.1. CO2 utilization 1
1.1.1. Sources of CO2 1
1.1.2. Carbon capture, utilization and storage 2
1.1.3. CO2-based C1 chemistry 5
1.2. Methanol synthesis from CO2 hydrogenation 6
1.2.1. Methanol 6
1.2.2. CO2 hydrogenation to methanol 9
1.2.3. Combined (CO2 + CO) hydrogenation to methanol 10
1.3. Catalysts for the CO2 hydrogenation 15
1.3.1. Hybrid nanostructure design 15
1.3.2. Heterogeneous catalytic hydrogenation of CO2 to methanol 17
1.3.3. Synthesis methods of hybrid nanostructure 21
1.4. Research objective 24
Chapter 2: Experimental methods 26
2.1. Material 26
2.2. Synthesis of the catalyst 27
2.2.1. Cu-ZnO@Al2O3-based hybrid nanostructures for CO2 hydrogenation to methanol 27
2.2.2. Cu-ZnO/Al2O3 hybrid nanostructures for combined (CO2 + CO) hydrogenation to methanol 30
2.3. Material characterization 34
2.3.1. Field emission high-resolution transmission electron microscope (HR-TEM) coupled with energy dispersive spectrometer (EDS) 34
2.3.2. Field emission scanning electron microscope (FE-SEM) coupled with energy dispersive spectrometer (EDS) 34
2.3.3. X-ray diffraction (XRD) 34
2.3.4. X-ray photoelectron spectroscopy (XPS) 35
2.3.5. Zeta potential measurement 35
2.3.6. Thermogravimetric analysis (TGA) 36
2.3.7. Inductively coupled plasma optical emission spectrometry (ICP-OES) 36
2.3.8. The Brunauer-Emmett-Teller (BET) surface area analyzer 36
2.3.9. Electrospray-Differential Mobility Analyzer (ES-DMA) 36
2.3.10. Chemisorption analyses 37
2.4. High-pressure fixed-bed reaction system 40
2.4.1. Cu-ZnO@Al2O3-based hybrid nanoparticle for catalytic CO2 hydrogenation to methanol 40
2.4.2. Cu-ZnO/Al2O3 hybrid nanostructures for combined (CO2 + CO) hydrogenation to methanol 43
2.5. Calculation of equilibrium conversions of CO2 and CO hydrogenation to methanol over various feedstock conditions 47
Chapter 3: Results and discussion 51
3.1. Cu-ZnO@Al2O3 hybrid nanoparticle for catalytic CO2 conversion to methanol 51
3.1.1. Morphology and composition of the Cu-ZnO@Al2O3 synthesized catalysts 51
3.1.2. Surface area and metal dispersion of the Cu-ZnO@Al2O3 synthesized catalysts 67
3.1.3. Basicity of the Cu-ZnO@Al2O3 synthesized nanocatalyst 71
3.1.4. Redox ability of the Cu-ZnO@Al2O3 synthesized catalyst 75
3.1.5. Activity test of the Cu-ZnO@Al2O3 synthesized catalyst 77
3.2. Low-Temperature Methanol Synthesis via (CO2 + CO) Combined Hydrogenation using Cu-ZnO/Al2O3 Hybrid Nanoparticle Cluster [42] 89
3.2.1. Morphology and Composition of the Cu-ZnO/Al2O3 synthesized catalysts 89
3.2.2. Surface area and metal dispersion of the Cu-ZnO/Al2O3 synthesized catalysts 96
3.2.3. Basicity of the Cu-ZnO/Al2O3 synthesized nanocatalyst 98
3.2.4. Redox ability of the Cu-ZnO/Al2O3 synthesized catalyst 101
3.2.5. Study of H2, CO and CO2 pulse chemisorptions of the Cu-ZnO/Al2O3 synthesized catalyst 108
3.2.6. Activity test of the Cu-ZnO/Al2O3 synthesized catalyst 110
Chapter 4: Conclusions 137
Chapter 5: Future work 139
References 145
Appendix 156

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