博碩士論文 102223042 詳細資訊




以作者查詢圖書館館藏 以作者查詢臺灣博碩士 以作者查詢全國書目 勘誤回報 、線上人數:9 、訪客IP:54.172.234.236
姓名 黃亞揚(Ya-Yang Huang)  查詢紙本館藏   畢業系所 化學學系
論文名稱 具羧酸官能基之中孔洞材料於染料吸附 及製備奈米銀顆粒於催化之應用
(Synthesis of Carboxylic Acid Functionalized Mesoporous Silica SBA-15 : Studies on Dye Adsorption and Fabrication of Silver Nanoparticles for Catalytic Reactions)
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摘要(中) 本論文主要是利用非離子型界面活性劑P123作為模板,將具有羧酸官能基的矽源CES (Carboxyethylsilanetriol sodium salt) 和TEOS (Tetraethyl orthosilicate) 作為共同矽源在酸性條件下以直接共聚合成法進行合成,可得到二維六角柱狀之中孔洞材料,並分別探討羧酸官能基化之中孔洞材料對染料吸附應用和吸附金屬離子加以還原成金屬奈米顆粒及應用兩大部分。
第一部分是利用合成出之羧酸官能基化中孔洞材料,其簡稱STC-x,x = [CES/(CES+TEOS)] 應用在移除廢水中染料亞甲基藍及孔雀石綠。以STC-x (x = 0, 10, 30, 50) 探討對染料的吸附,發現pH值愈高與官能基含量提高皆有助於提高吸附量,並且將吸附數據代入吸附模型,Langmuir等溫吸附模式比 Freundlich等溫吸附模式更適合描述STC-x吸附染料之系統,並且比較此兩種染料的吸附情形,發現STC-x對亞甲基藍之吸附效果較佳。
第二部分則是利用合成出之STC-x,將其應用在吸附銀金屬離子,並利用熱還原法將金屬離子還原成金屬奈米粒子。在形成金屬奈米粒子的過程中因受到孔洞大小的空間限制及羧酸官能基的影響, 可以有效地將金屬顆粒尺寸最小控制在2-3 nm左右。並將其應用在還原4-Nitrophenol之催化反應。
摘要(英) Mesoporous silicas SBA-15 functionalized with various contents of carboxylic acid groups were successfully synthesized via co-condensation of Tetraethyl orthosilicate (TEOS) and Carboxyethylsilanetriol sodium salt (CES) templated with a triblock polymer P123 at low HCl concentrations. All these materials have been characterized by powder X-ray diffraction (XRD), nitrogen sorption measurements, solid-state 13C and 29Si MAS NMR spectroscopy, thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and transmission electron
microscopy (TEM).
In the first project, the prepared mesoporous STC-x materials have been utilized as suitable adsorbent for methylene blue and malachite green. The adsorption process was carefully studied with varies systematic parameters, including the loading amount of CES, the quantity of dye, pH of adsorption system. The isotherm models and kinetic models were analyzed to describe the adsorption behavior of STC-x materials. As comparison, the adsorption capacity was also studied for methylene blue and malachite green. It shows that the adsorption capacity of STC-x for methylene blue is better than that of malachite green.
The aim of the second project was to prepare Ag nanoparticles within the uniform pore channels of STC-x. TEM images showed uniformly distributed nanoparticles inside the pore channels of STC-x. Synthesized Ag nanoparticles incorporated in STC-x were used as a good catalyst for the reduction of
4-nitrophenol to 4-aminophenol.
關鍵字(中) ★ 中孔洞
★ 染料
★ 奈米金屬
★ 羧酸官能基
關鍵字(英) ★ mesoporous
★ dyes
★ nanoparticles
★ Carboxylic acid groups
論文目次 中文摘要 i
Abstract ii
謝誌 iii
目錄 iv
圖目錄 viii
表目錄 xii
第一章 緒論 1
1-1中孔洞分子篩材料簡介 1
1-2界面活性劑簡介 3
1-2-1界面活性劑結構與種類 4
1-2-2微胞的形成與結構 5
1-2-3界面活性劑與矽氧化物的交互作用力 7
1-2-4共聚高分子 (Block copolymer) 11
1-3表面修飾官能基之中孔洞材料 13
1-3-1中孔洞材料表面之官能基修飾方法 13
1-3-2具羧酸官能基中孔洞材料之發展 16
1-4中孔洞材料之吸附發展及應用 20
1-4-1中孔洞材料吸附染料之發展應用 20
1-4-2中孔洞材料吸附金屬之發展應用 26
1-4-3金屬奈米顆粒對4-Nitrotrophenol催化還原反應之簡介 32
1-5研究動機與目的 42
第二章 實驗部分 43
2-1實驗藥品 43
2-2實驗步驟 44
2-2-1合成具羧酸官能基之SBA-15 (STC-x) 44
2-2-2以硫酸溶液裂解孔洞中的模板 44
2-2-3染料檢量線配置 44
2-2-4利用STC-x在不同濃度吸附染料實驗 45
2-2-5 STC-x在不同時間吸附染料實驗 45
2-2-6 STC-x對不同染料之吸附實驗 46
2-2-7 STC-x在不同pH值下吸附亞甲基藍實驗 46
2-2-8 STC-x對吸附亞甲基藍之重複使用性 47
2-2-9利用STC-x吸附銀金屬製備奈米銀金屬顆粒 47
2-2-10利用STC-x-Ag-y對4-Nitrophenol進行催化還原反應 48
2-2-11 STC-x-Ag-y催化還原反應的重複使用性 48
2-3實驗設備 49
2-3-1實驗合成設備 49
2-3-2實驗鑑定儀器 49
2-4鑑定儀器之原理 51
2-4-1 X射線粉末繞射 (Powder X-Ray Diffractometer) 51
2-4-2氮氣吸脫附等溫曲線、表面積與孔洞特性鑑定 52
2-4-3傅立葉紅外線吸收光譜 (Fourier Transform Infrared Spectroscopy; FTIR) 55
2-4-4紫外光-可見光光譜 (UV/Vis Absorption Spectrocopy) 55
2-4-5熱重分析儀 (Thermogravimetric Analyzer) 57
2-4-6穿透式電子顯微鏡 (Transmission Electron Microscope; TEM) 58
2-4-7低真空掃描式電子顯微鏡 (Scanning Electron Microscope; SEM) 59
2-4-8固態核磁共振 (Solid State NMR) 60
2-4-9感應耦合電漿原子發射光譜分析儀 (Inductively-Coupled Plasma Atomic Emission Spectroscopy ; ICP-AES) 67
第三章 結果與討論 68
3-1合成不同矽源比例的 STC-x 68
3-1-1 XRD繞射圖譜 68
3-1-2等溫氮氣吸脫附 70
3-1-3 FT-IR紅外線光譜 73
3-1-4 13C CP/MAS NMR 75
3-1-5 29Si MAS NMR 76
3-1-6熱重分析 78
3-1-7 TEM影像 80
3-1-8 SEM影像 81
3-1-9表面電位 82
3-2 STC-x吸附染料吸附實驗 83
3-2-1染料檢量線 83
3-2-2 STC-x在不同初始濃度下對染料吸附之影響 84
3-2-3 STC-x在不同時間下對染料吸附之影響 86
3-2-4等溫吸附模式 88
3-2-5動力學吸附探討 93
3-2-6 STC-x 對不同染料之吸附比較 98
3-2-7 STC-x在不同pH值下對亞甲基藍吸附之影響 100
3-2-8 STC-x 對亞甲基藍之重複吸附性 101
3-3利用STC-x吸附銀金屬 102
3-3-1 STC-x-Ag-y之XRD結果 102
3-3-2 STC-x-Ag-y之TEM結果 106
3-3-3 STC-x-Ag-y之氮氣等溫吸脫附結果 110
3-3-4 STC-x-Ag-y之FT-IR結果 113
3-3-5 STC-x-Ag-y之ICP-AES結果 114
3-4 STC-x-Ag-y催化還原4-Nitrophenol之應用 115
3-4-1 4-Nitrophenol之催化還原反應 115
3-4-2 STC-x-Ag-y對4-Nitrophenol催化還原反應之結果探討 117
3-4-3動力學及催化速率探討 119
3-4-4 STC-x-Ag-y對4-Nitophenol之重複催化還原性 122
第四章 結論 123
第五章 參考文獻 124
附錄 136









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指導教授 高憲明(Hsien-ming Kao) 審核日期 2015-7-29
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