金屬有機骨架(Metal-Organic Frameworks, MOFs)是一種無機金屬簇或離子與有機配位基結合的高度多孔材料，其具高度有序的結構、高孔隙率、高比表面積、可設計自身結構，這些特點使得MOFs成為優良的吸附材料，廣泛應用於氣體吸附分離、藥物傳輸、觸媒催化反應以及廢水處理上。有研究表示通過與其他材料的結合，能夠有效提高MOFs的性能，如奈米碳管(Carbon Nanotubes, CNTs)或是殼聚醣(Chitosan, CS)等。其中CNTs具獨特的構造，有良好的熱穩定性、導電性與疏水性，而CS具優異的螯合性能，結構中的氨基基團反應活性強，使其具有優異的生物學功能並能進行化學修飾反應，集結MOFs與CNTs、CS的優點，期望可以製作出性能優異的複合材料。因MOFs為微細粉末狀，在固液分離上無法全回收，若將其賦予磁性，為磁性MOFs(Magnetic Metal-Organic Frameworks, MMOFs)，能有效減少材料的分離時間和能耗，還能以簡單的方式精準定位，這使得其應用性大大提升。通過使用微波法，可以以更短的時間合成MOF，且還有快速成核、高產率這些優點。本研究利用微波法製備MOF複合材料，以最佳產率及其物化特性評估出最適合成條件，再利用此條件添加磁性載體進而合成MMOF與CS/MMOF複合材料。合成的材料通過SEM、TEM、XRD、FTIR、BET、TGA、pHpzc、SQUID與穩定性實驗以了解其物理化學性質，而為了瞭解應用在水環境上的可行性，將MOF與MMOF複合材料作為吸附劑，去除水中污染物亞甲基藍(Methylene blue, MB)，建立吸附動力模式及等溫吸附曲線以了解材料進行吸附之傳輸途徑。實驗結果顯示，根據SEM、TEM觀察其外觀結構，XRD、FTIR進行晶相與官能基鑑定，證實成功合成MOF、MMOF與CS/MMOF複合材料，而BET比表面積分析可得知MOF與MMOF複合材料最高比表面積分別為1263.30 m2/g、1287.38 m2/g，TGA結果得知添加越多CNTs量，重量損失越少，經SQUID測試所得結果，最大飽和磁化強度為4.26 emu/g。MOF複合材料與MMOF複合材料之吸附動力學結果皆與Elovich rate equation模擬較為吻合，而等溫吸附曲線則與Langmuir isotherm及Freundlich isotherm皆為吻合。經水穩定性實驗，得知CS@MMOF複合材料在水中穩定性高。本研究成功以微波法合成MMOF複合材料，並應用於水中污染物之吸附去除。

Metal-Organic Frameworks are fabricated through linking metal ions and organic linkers. They have many advantages such as large surface areas, high pore volume, and the selection of the organic ligand and metal. Due to these reasons, MOFs are excellent adsorption materials. They are being used in various applications such as gas storage, drug delivery and wastewater treatment. A research finds some materials can improve MOF properties, such as carbon nanotube and chitosan. Due to the unusual electrical, thermal and hydrophobic properties of CNTs, CNTs are used as composite fillers in various applications. Chitosan is a biodegradable polymeric material with exceptional chelating properties and chemical reactivity due to the presence of hydroxyl and amino groups. Combining the advantages of MOFs, CNTs, and CS, it is expected that composite materials with excellent performance can be synthesized. Because MOFs are powders, they cannot be fully recovered in solid-liquid separation. Adding magnetic particles to MOF is the Magnetic Metal-Organic Frameworks, which can effectively reduce the separation time and energy consumption of materials, and locate in a simple way. It can improve the applicability of MOF. Since hydrothermal methods generally need up to several days, it is important to develop facile, rapid ways to the production. Recently, the microwave heating method has been applied successfully for the synthesis of metal-organic frameworks with high phase purity and high yield ,and decreasing reaction time of Cu-BTC synthesis up to a few minutes. This study uses microwave method to prepare MOF composite material. According to the best yield, physical and chemical properties, the most suitable conditions are evaluated. Add magnetic particles and use this condition to synthesize MMOF and CS/MMOF composite materials. And, the materials were characterized by SEM, TEM, XRD, FTIR, BET, TGA, pHpzc, SQUID and stability experiment. In order to understand the feasibility of application in the water environment, the MOF and MMOF composite materials were used in removal of MB. And the adsorption data were analyzed by adsorption isotherm and adsorption kinetics model to understand the transport path of the material for adsorption. The experimental results showed that the morphology was observed by SEM and TEM, and the crystal phase and functional groups were identified by XRD and FTIR, which confirmed that MOF, MMOF and CS/MMOF composite materials were successfully synthesized. BET specific surface area analysis shows that the highest specific surface areas of MOF and MMOF composites are 1,263.30 m2/g and 1,287.38 m2/g, respectively. TGA results show that the thermal stability of the microwave method is higher than that of the hydrothermal method. The SQUID result shows that the maximum saturation magnetization is 4.26 emu/g. The results of adsorption kinetics on MOF and MMOF are similar to Elovich rate equation model, and the adsorption isotherms are similar to both Langmuir isotherm and Freundlich isotherm. Through water stability experiments, it is known that the CS@MMOF composite material has high stability in water. In this study, the MMOF composite material was successfully synthesized by the microwave method and applied to removal of MB.

縮寫表 1
摘要 4
Abstract 6
目錄 8
表目錄 12
圖目錄 13
第一章、 緒論 16
1.1 研究背景 16
1.2 研究目的 17
1.3 研究流程 18
第二章、 文獻回顧 19
2.1金屬有機骨架材料(MOFs)之簡介 19
2.1.1 金屬有機骨架材料 19
2.1.2 金屬有機骨架之合成方法 21
2.2金屬有機骨架複合材料之簡介 24
2.2.1金屬有機骨架複合材料 24
2.2.2金屬有機骨架複合材料之合成方法 25
2.3 磁性金屬有機骨架材料(MMOFs)之簡介 33
2.3.1 磁性材料種類 33
2.3.2 磁性材料之介紹 34
2.3.2 磁性金屬有機骨架 35
2.3 亞甲基藍 36
2.4 吸附理論 38
2.4.1 等溫吸附模式 38
2.4.2 整體性動力模式 39
第三章、 研究方法與材料 43
3.1實驗藥品 43
3.2 實驗設備與分析儀器 44
3.2.1實驗設備 44
3.2.2分析儀器與器材 45
3.3金屬有機骨架之製備 46
3.4金屬有機骨架複合材料之合成程序 46
3.4.1 官能化MWCNTs材料製備 46
3.4.2 以微波法製備CNTs@Cu-BTC 46
3.4.3 以水熱法製備CNTs@Cu-BTC 46
3.5磁性金屬有機骨架之合成程序 47
3.5.1 磁性顆粒之製備 47
3.5.3 M/CNTs@Cu-BTC之製備 47
3.6 CS/M/CNTs@Cu-BTC之合成程序 48
3.6.1 CS/M/CNTs@Cu-BTC之製備 48
3.6.2 CS/M/CNTs@Cu-BTC於無氧環境之製備 48
3.7 亞甲基藍吸附實驗 49
3.7.1等溫吸附實驗 49
3.7.2吸附動力實驗 49
3.8 樣品穩定性實驗 49
3.9 零點電荷實驗 49
第四章、 結果與討論 50
4.1 CNTs@Cu-BTC 50
4.1.1 合成溫度對材料的影響 50
4.1.1.1 表面結構觀察(SEM) 51
4.1.1.2 晶相鑑定 52
4.1.1.3 官能基鑑定 53
4.1.2 合成時間對材料的影響 55
4.1.2.1 表面結構觀察(SEM) 56
4.1.2.2 晶相鑑定 57
4.1.2.3 官能基鑑定 58
4.1.3合成溶劑比例對材料的影響 60
4.1.3.1 表面結構觀察(SEM) 61
4.1.3.2 晶相鑑定 62
4.1.3.3 官能基鑑定 63
4.1.4 CNTs質量對材料的影響 65
4.1.4.1 表面結構觀察(SEM) 66
4.1.4.2 表面結構觀察(TEM) 68
4.1.4.3 晶相鑑定 69
4.1.4.4 官能基鑑定 70
4.1.5 合成方式對材料的影響 72
4.1.5.1 表面結構觀察(SEM) 73
4.1.5.2 晶相鑑定 74
4.1.5.3 官能基鑑定 75
4.1.6 比表面積分析 77
4.1.7 熱重分析 81
4.1.8 結論 83
4.2 M/CNTs@Cu-BTC 84
4.2.1 表面結構觀察(SEM與TEM) 85
4.2.2 晶相鑑定 87
4.2.3 官能基鑑定 88
4.2.4 比表面積分析 90
4.2.5 熱重分析 94
4.2.6 零電位點 96
4.2.7 飽和磁化強度 98
4.3 CNTs@Cu-BTC與M/CNTs@Cu-BTC之吸附特性分析 101
4.3.1 不同CNTs質量之CNTs@Cu-BTC對亞甲基藍之吸附量 101
4.3.2 CNTs@Cu-BTC對亞甲基藍之等溫吸附 104
4.3.3 CNTs@Cu-BTC對亞甲基藍之吸附動力學 106
4.3.4 M/CNTs@Cu-BTC對亞甲基藍之吸附量 111
4.3.5 M/CNTs@Cu-BTC對亞甲基藍之等溫吸附 112
4.3.6 M/CNTs@Cu-BTC對亞甲基藍之吸附動力學 114
4.3.7 CNTs@Cu-BTC與M/CNTs@Cu-BTC對亞甲基藍之吸附特性比較 119
4.4 CNTs@Cu-BTC與M/CNTs@Cu-BTC之穩定性探討 120
4.4.1 表面結構觀察(SEM) 120
4.4.2 官能基鑑定 124
4.5 CS/M/CNTs@Cu-BTC 128
4.5.1 表面結構觀察(SEM) 129
4.5.2 晶相鑑定 130
4.5.3 官能基鑑定 132
4.5.4 熱重分析 134
4.5.5 比表面積分析 135
4.5.6 飽和磁化強度 138
4.5.7 穩定性分析 140
4.6 創新性 145
第五章、 結論與建議 146
5.1 結論 146
5.2 建議 147
參考文獻 148

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