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研究生： 藍啟軒
Lan, Ci-Syuan
論文名稱： 探討鉀-聚(庚嗪醯亞胺)結構中氰胺基對其光催化性能的作用
Investigate the role of the Cyanamide group within the Potassium-Poly(Heptazine Imide) Structure on its Photocatalytic Performance
指導教授： 劉詠熙
Lau, Vincent Wing-Hei
學位類別： 碩士
Master
系所名稱： 理學院 - 化學系
Department of Chemistry
論文出版年： 2024
畢業學年度： 113
語文別： 英文
論文頁數： 106
中文關鍵詞： 鉀-聚(庚嗪醯亞胺) 、氰胺基 、光催化性能
外文關鍵詞： Potassium Poly(heptazine imide), Cyanamide group, Photocatalytic Performance
相關次數： 點閱：152  下載：30 
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    • Potassium Poly(heptazine imide) (K-PHI) 因其低毒性和高穩定性而被視為具有發展潛力的光催化劑。然而，由於K-PHI較低的結晶性以及結構的不確定性，大幅提高了研究其光物理性質挑戰性，也因此阻礙了提高其光催化效率的研究。近期的文獻表明，結構中的氰胺基對增強光催化性能極其重要。在文獻中使用硫氰酸鉀 (KSCN) 的離子熱合成 (ionothermal synthesis) 使得該官能基存在於結構的邊緣的同時還形成了點缺陷存在於結構中，導致其光催化性能與該官能基之間的相關性變得更加複雜難以釐清。
    本研究旨在通過改善 K-PHI 的結晶性並系統性地增加結構中的氰胺基來探討這一關係。在論文中我們採用紅外光譜 (FT-IR) 來評估氰胺基在K-PHI結構中的相對量，並將具有特定氰胺基相對量的 K-PHI用於後續苯甲醇的光氧化反應中。為更直接證明該官能基與光催化性能間的關係，該反應將在不使用氧化劑的溫和調進下進行反應以此來簡化反應實驗中複雜的變因。論文中所使用的紫外-可見光光譜儀 (UV-Vis) 則被用於監測反應進程，並根據所得的苯甲醛濃度計算並比較各別的反應速率常數。實驗結果表明，含有更多氰胺基的 K-PHI 表現出更高的反應速率。此外在氮氣吸脫附實驗中所得的比表面積數據證明，反應速率的提高與K-PHI的比表面積無關，這表明K-PHI的催化性能的提高主要來自於結構中存在的氰胺基。

    The unclear structure of potassium poly(heptazine imide) (K-PHI) has hindered improvements in catalytic efficiency. Investigating its photophysical properties is challenging due to its poor crystallinity. Recent literature indicates that the cyanamide group within the structure is crucial for enhancing photocatalytic performance. However, ionothermal synthesis using KSCN results in this functional group not only existing at the edge of the structure but also forming a point defect, complicating the correlation between photocatalytic performance and this functional group. This research aims to explore this relationship by improving the crystallinity of K-PHI and systematically increasing the cyanamide groups within the structure. FT-IR spectroscopy was conducted to assess the relative intensity of the cyanamide group in the spectrum. To narrow down the factors influencing the photocatalytic reaction, K-PHI with specific amounts of cyanamide groups will be applied to the photooxidation of benzyl alcohol under mild conditions, without the use of oxidizing agents. We will use UV-Vis spectroscopy to monitor the reaction process and compare the rate constants. The results demonstrate that K-PHI with more cyanamide groups exhibits an increased reaction rate. Furthermore, nitrogen adsorption-desorption studies confirm that the enhancement in reaction rate is not related to surface area, indicating that the improvement in performance is solely due to the influence of the cyanamide groups within the material's structure.

    摘要 i Abstract ii Acknowledgments iii Contents iv Figure Contents vi Table Contents x Abbreviation List xi Chapter 1 Introduction 1 1.1 Motivation 1 Chapter 2 Literature review 3 2.1 Mechanism of Solar Energy Conversion in Semiconductors for Photocatalysis 3 2.2 Features of Inorganic Semiconductors for Solar Energy Utilization 5 2.3 Distinctive Characteristics of Melon Compared to Inorganic Semiconductors 6 2.4 Historical Development of Melon and Potassium Poly(heptazine Imide) 9 2.5 Review on the Synthesis of Potassium Poly(heptazine Imide) Using Ionothermal Techniques 11 2.6 Features and Challenges of Potassium Poly(heptazine Imide) (K-PHI) in Photocatalytic Applications 14 2.7 Research Questions and Objectives Regarding the Role of Cyanamide Groups in K-PHI Photocatalysis 18 Chapter 3 Methodology 19 3.1 Optimizing the Crystallinity of K-PHI 19 3.2 Strategies for Inducing and Quantifying Cyanamide Groups in K-PHI 20 3.3 Evaluating the Role of Cyanamide Groups in K-PHI Photocatalytic Oxidation 21 Chapter 4 Experiment 23 4.1 Manufacturer and Purity of Chemicals 23 4.2 Instruments details 23 4.3 Experimental details 25 Chapter 5 Result and discussion 29 5.1 Optimization of K-PHI Crystallinity 29 5.1.1 Enhancing K-PHI Crystallinity Using Chloride Eutectic Mixtures 33 5.1.2 Enhancing K-PHI Crystallinity with KSCN 37 5.2 Methods for Quantifying and Inducing Cyanamide Groups in K-PHI 41 5.2.1 Inducing Cyanamide Groups by Extending Maximum Temperature Hold Time 43 5.2.2 Inducing Cyanamide group by Raising Maximum Temperature 45 5.2.3 Inducing Cyanamide Groups by Gradually Increasing Chloride Eutectic Ratio 47 5.2.4 Inducing Cyanamide Groups by Increasing KSCN Amount 51 5.2.5 Inducing Cyanamide Groups through the Addition of KCl 53 5.3 Physical properties characterization 56 5.3.1 Characterization of Optical Properties and Structural Binding 56 5.3.2 Nitrogen adsorption and desorption analysis and Elemental analysis 59 5.4 Photocatalytic Reactions of Benzyl Alcohol and Benzaldehyde 63 5.4.1 Blank, Control Experiments and Calibration Curve 64 5.4.2 Benzyl Alcohol Photocatalytic Oxidation Reaction 68 5.4.3 Benzaldehyde Photocatalytic Oxidation Reaction 70 5.4.4 Mechanistic Insights into the Role of Cyanamide group in Photooxidation 72 Chapter 6 Conclusion 77 Chapter 7 Reference 78 Chapter 8 Appendix 84

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