三維結構具官能基之中孔洞材料製備含銀鎳合金奈米顆粒於催化之應用

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姓名

夏汝安(Nu-An Hsia) 查詢紙本館藏

畢業系所

化學學系

論文名稱

三維結構具官能基之中孔洞材料製備含銀鎳合金奈米顆粒於催化之應用
(Synthesis of Ag/Ni Alloy Nanoparticles Confined in Carboxylic Acid Functionalized Cubic SBA-1 Mesoporous Silica Nanoparticle as Efficient Catalysts for Reduction of 4-Nitrophenol and Degradation Reactions)

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摘要(中)

本論文主要分為兩部分，第一部分是利用陽離子型界面活性劑Hexadecyl pyridinium chloride (CPC) 及陰離子型高分子Poly(acrylic acid) (PAA) 為模板，在鹼性環境下合成具羧酸官能基之中孔材料SBA-1，簡稱為CS-1B-x，且x = [CES / (CES + TEOS) ]，修飾官能基後，仍能保有SBA-1系列的Pm3n規則結構，接著將所合成CS-1B-x吸附金屬離子，可成功還原成銀奈米金屬顆粒以及銀鎳合金奈米顆粒在此中孔材料上。在形成金屬奈米粒子的過程中，能受到孔洞大小空間之限制以及羧酸官能基之影響，其尺寸約於3 – 10 nm之間。吸附奈米金屬後，CS-1B-x材料結構也無崩解的情形發生，可以發現銀奈米粒子最佳含浸量為0.3 mmol，而銀奈米顆粒的尺寸為3.2 nm。
將此系列材料進一步應用於4-Nitrophenol之還原催化反應，並將催化數據帶入Pseudo-first order得出反應速率常數，可發現銀的奈米顆粒愈小，催化活性會有較好的表現；但當銀鎳比是6:4時其催化效果是最好的，其反應速率常數3.0 x 10-2 s-1，其催化反應在2-3分鐘便能結束。
第二部分是將此含奈米金屬之中孔材料進行染料之催化降解反應，以Methyl orange以及Rhodamine B做為示範染料進行降解，可以發現Ag06Ni04-CS-1B-10對於Methyl orange的降解能力是最好的，反應速率常數為6.9 x 10-2 s-1；而Ag08Ni02-CS-1B-10對於Rhodamine B有最高的反應速率，其反應速率常數為2.7 x 10-2 s-1。結果顯示本實驗所製備之含奈米合金之中孔洞料對於染料降解也能有非常優異的催化活性。

摘要(英)

Silver nanoparticles (Ag NPs) with a particle size about 3 nm are successfully confined within the cage-type mesopores of cubic SBA-1 mesoporous silica nanoparticles (MSNs) functionalized with carboxylic acid (-COOH) groups (CS-1B-x). Under alkaline condition of pH 9, the –COOH groups deprotonate and become -COO- groups, and thus can effectively interact with the Ag+ ions and allow facile fabrication of Ag NPs. We also used Ag+ and Ni2+ to synthesis Ag/Ni alloy incorporated in CS-1B-10. The materials were characterized by powder X-ray diffraction (XRD), solid-state 13C and 29Si MAS NMR spectroscopy, nitrogen adsorption-desorption measurements, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS).
In the first project, the catalytic activity of these Ag NPs based SBA-1 materials were tested for reduction of 4-nitrophenol. As the catalyst for the reduction of 4-NP, the Ag-0.3-CS-1B-10 exhibit a very high catalytic activity with the activity parameter of 120 ( s-1 g-1 cat.), and Ag06Ni04-CS-1B-10 is 150 ( s-1 g-1 cat.).
Then we further used Ag/Ni alloy incorporated in CS-1B-10 for dye degradation. The degradation of methyl orange and rhodamine b follows the pseudo first order kinetics. As the catalyst for the degradation of methyl orange, Ag06Ni04-CS-1B-10 exhibits a good catalytic activity with the activity parameter of 345.0 ( s-1 g-1 cat.), also processing rhodamine b degradation by using Ag08Ni02-CS-1B-10, the activity parameter is 135.0 ( s-1 g-1 cat.). This remarkable catalytic activity for the reduction of 4-nitrophenol and degradation of methyl orange/rhodamine b can be attributed to the ultra-small Ag/Ni NPs confined in cage-type mesopores of SBA-1 MSNs, which have the particle size around 500 nm.

關鍵字(中)

★ 中孔洞材料
★ 銀鎳合金
★ 4-硝基苯酚
★ 染料降解

關鍵字(英)

★ mesoporous material
★ Ag/Ni nanoparticle
★ 4-nitrophenol
★ dye degradation

論文目次

中文摘要 i
Abstract ii
謝誌 iii
目錄 iv
圖目錄 vii
表目錄 xiii
第一章緒論 1
1-1 中孔洞二氧化矽材料 1
1-1-1 中孔洞材料之沿革 1
1-2 界面活性劑之性質簡介 3
1-2-1 界面活性劑的種類 3
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 7
1-3 官能基化之中孔洞材料 11
1-4 文獻回顧 13
1-4-1 中孔洞材料SBA-1之合成與介紹 13
1-4-2 以聚電解質及界面活性劑搭配合成之中孔洞材料 14
1-4-3 具羧酸官能基中孔洞材料之發展 16
1-4-4 中孔洞材料吸附金屬之應用發展 22
1-4-5 金屬奈米顆粒對4-Nitrophenol催化還原反應之簡介 27
1-4-6 金屬奈米顆粒對有機染料催化降解之簡介 39
1-5 研究動機及目的 46
第二章實驗方法 47
2-1 實驗藥品 47
2-2 實驗步驟 49
2-2-1 合成具羧酸官能基的中孔洞SBA-1 (CS-1B-x) 49
2-2-2 以硝酸溶液裂解孔洞中的模板 49
2-2-3 CS-1B-x吸附銀金屬製備奈米銀金屬顆粒(Ag-y-CS-1B-x) 50
2-2-4 利用CS-1B-10同時吸附銀及鎳金屬製備銀鎳合金內嵌在中孔洞SBA-1中(AgzNi1-z-CS-1B-10) 50
2-2-5 材料對4-Nitrophenol進行催化還原反應 51
2-2-6 材料對Methyl Orange及Rhodamine B之催化降解反應 51
2-2-7 材料於催化反應的重複使用性 52
2-3 實驗設備 53
2-3-1 實驗合成設備 53
2-3-2 實驗鑑定儀器 53
第三章結果與討論 55
3-1 基本性質鑑定 55
3-1-1 XRD繞射圖譜 55
3-1-2 13C CP/MAS NMR 63
3-1-3 29Si MAS NMR 65
3-1-4 等溫氮氣吸脫附 67
3-1-5 SEM影像 71
3-1-6 TEM影像 73
3-1-7 XPS圖譜 76
3-1-8 ICP-AES結果 77
3-2 CS-1B-x吸附奈米金屬之4-Nitrophenol催化還原反應 78
3-2-1 4-Nitrophenol之催化還原反應 78
3-2-2 Ag-y-CS-1B-x對4-Nitrophenol催化還原反應之結果探討 80
3-2-3 動力學及催化速率探討 83
3-2-4 AgzNi1-z-CS-1B-10對於4-Nitrophenol催化還原反應之結果探討 86
3-3 CS-1B-x吸附奈米金屬之染料催化降解反應 90
3-3-1 有機染料催化降解反應之結果探討 90
3-3-1.1 AgzNi1-z-CS-1B-10對Methyl Orange之催化降解反應結果 91
3-3-1.2 AgzNi1-z-CS-1B-10對Rhodamine B之催化降解反應結果 94
3-3-2 動力學及催化速率探討 97
3-3-3 AgzNi1-z-CS-1B-10對於其他染料之催化降解反應結果 100
3-4 材料於催化反應的重複使用性 102
第四章結論 104
第五章參考文獻 105

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指導教授

高憲明(Hsien-Ming Kao)

審核日期

2017-7-24

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