具羧酸官能基三維結構中孔洞材料製備含釕金屬及銅鎳金屬奈米顆粒之催化應用

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具羧酸官能基三維結構中孔洞材料製備含釕金屬及銅鎳金屬奈米顆粒之催化應用

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至系統瀏覽論文 (2024-6-30以後開放)

摘要(中)

本篇論文分成兩個部分，第一部分為在鹼性環境下合成具有羧酸官能
基中孔洞材料 SBA-1，簡稱 CS-1B-x，其中 x = [CES/(CES+TEOS)]。將合成好的材料 CS-1B-x含浸釕金屬離子前驅液，利用化學還原法將釕金屬離子還原成釕金屬奈米顆粒，形成金屬奈米顆粒的過程中，受到材料孔洞大小及官能基的影響，其金屬顆粒大小約在 2-4 nm間。再將含浸釕金屬奈米顆粒的材料應用於硼烷氨水解製氫反應中，在 Ru(1)-CS-1B-10時，達到最佳的催化活性，其 TOF值為 202.4 H2 mol/metal mol min、活化能為 24.13 kJ/mol。
第二部分為將 CS-1B-x含浸銅及鎳金屬離子前驅液，利用熱還原法將
金屬離子還原成金屬奈米顆粒。過程中，在鹼性環境下 (pH = 9) 吸附金屬離子，此時材料上的羧酸官能基 (COOH) 會去離子化形成負離子
( 能夠有效吸附金屬離子進入材料中。將合成好的材料應用於 4-Nitrophenol之催化還原反應，將得到的數據帶入 Pseudo-first order得出反應速率常數，得知在銅及鎳的比例為 8 2時，達到最佳的催化活性，其反應速率 k值高達 205.3 s-1g-1。

摘要(英)

I have two part in my study. In the first part, ruthenium Nanoparticles (Ru NPs) are successfully confined within the cage-type mesopores of cubic mesoporous silica nanoparticles (MSNs) SBA-1 (sample denoted as Ru(y)-CS-1B-x) functionalized with carboxylic acid (-COOH) groups. The Ru NPs were forms inside the pores of SBA-1 by using chemical reduction with aqueous solution of NaBH4 and NH3BH3. The synthesized Ru(y)-CS-1B-x materials were characterized by nitrogen adsorption-desorption isotherms, powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), solid-state 13C and 29Si MAS NMR spectroscopy. According to the TEM images, it can be known that particle size of Ru NPs is about 2-4 nm. The Ru(1)-CS-1B-10 catalyst exhibits high catalytic activity in the catalytic hydrogen generation through hydrolysis of NH3BH3. The turnover frequency of 202.4 H2 mol/metal mol min and activation energy of 24.13 kJ/mol. The remarkable activity for hydrolysis of NH3BH3 can be attributed to the ultra-small Ru NPs confined in mesoporous of SBA-1 MSNs.
In the second part, the copper/nickel alloy incorporated in CS-1B-x (CuyNi10-y-CS-1B-x), Under alkaline condition (pH=9), the –COOH groups on the surface deprotonate and become –COO- group, with efficiently interact with Cu2+/Ni2+ cations and allow facile fabrication of Cu-Ni NPs. The CuyNi10-y-CS-1B-x were used for reduction of 4-nitrophenol, and the Cu8Ni2-CS-1B-10 shows high catalytic activity with the activity parameter of 205.3 (s-1gcat.-1). The synergistic effect between Cu and Ni plays an important role for reduction of 4-nitrophenol.

關鍵字(中)

★ 中孔洞材料
★ 金屬奈米顆粒
★ 有機汙染物降解
★ 產氫

關鍵字(英)

論文目次

目錄
中文摘要 i
Abstract ii
目錄 iii
圖目錄 vi
表目錄 xii
第一章序論 1
1-1中孔洞二氧化矽材料 1
1-1-1中孔洞材料介紹 1
1-1-2 中孔洞材料定義 1
1-2界面活性劑與矽酸鹽之介紹 4
1-2-1界面活性劑之種類 5
1-2-2微胞的形成 7
1-2-3 界面活性劑與矽氧化物的作用力 8
1-3官能基化之中孔洞材料 10
1-4 文獻回顧 12
1-4-1 中孔洞材料SBA-1之合成與介紹 12
1-4-2 具羧酸官能基之中孔洞材料及其應用 14
1-4-3 中孔洞材料吸附金屬之文獻 19
1-4-4 金屬奈米顆粒對硼烷氨水解產氫之文獻 23
1-4-5 金屬奈米顆粒對4-Nitrophenol降解反應之文獻 28
1-5 研究動機及目的 35
第二章實驗部分 36
2-1 實驗藥品 36
2-2 實驗步驟 38
2-2-1具羧酸官能基的中孔洞矽材SBA-1合成 38
2-2-2以鍛燒或硝酸溶液去除孔洞中的模板 39
2-2-3 CS-1B-x 吸附釕及銅鎳離子製備金屬奈米顆粒 40
2-2-3.1 利用雙還原劑進行化學還原法還原釕離子製備釕奈米金屬(Ruy-CS-1B-x) 40
2-2-3.2 利用熱還原法還原銅鎳離子製備銅鎳奈米金屬 (CuyNi10-y-CS-1B-x) 42
2-2-4 材料對硼烷氨進行催化水解產氫之反應 43
2-2-4.1 硼烷氨催化水解產氫實驗 43
2-2-4.2 材料回收之重複使用 45
2-2-5材料對4-Nitrophenol進行催化還原反應 46
2-2-5.1 4-Nitrophenol催化還原反應 46
2-2-5.2材料回收之重複使用 46
2-3 實驗設備 48
2-3-1 實驗合成設備 48
2-3-2 實驗鑑定儀器 48
第三章結果與討論 50
3-1 Ruy-CS-1B-x材料系列 50
3-1-1 基本性質鑑定 50
3-1-1.1 SAXRD 繞射圖譜 50
3-1-1.2 WAXRD 繞射圖譜 53
3-1-1.3 13C CP/MAS NMR 55
3-1-1.4 29Si MAS NMR 56
3-1-1.5 FTIR紅外線光譜 58
3-1-1.6 表面電位 59
3-1-1.7 等溫氮氣吸脫附 60
3-1-1.8 TEM影像 64
3-1-1.9 SEM影像 68
3-1-1.10 XPS光譜圖 71
3-1-2 Ru(y)-CS-1B-x之硼烷氨水解產氫反應 72
3-1-2.1 以化學還原法還原不同釕金屬比例之催化活性 73
3-1-2.2 Ru(1)-CS-1B-10之動力學探討 75
3-1-2.3 Ru(1)-CS-1B-10之回收利用 79
3-2 CuyNi10-y-CS-1B-x材料系列 83
3-2-1 基本性質鑑定 83
3-2-1.1 SAXRD 繞射圖譜 83
3-2-1.2 WAXRD 繞射圖譜 86
3-2-1.3 等溫氮氣吸脫附 88
3-2-1.4 TEM 影像 92
3-2-1.5 SEM影像 96
3-2-1.6 XPS圖譜 98
3-2-1.7 ICP-MS結果 99
3-2-2 4-Nitrophenol催化反應 100
3-2-2.1 CuyNi10-y-CS-1B-0之4-Nitrophenol催化活性結果 102
3-2-2.2 CuyNi10-y-CS-1B-0 動力學及催化活性探討 104
3-2-2.3 CuyNi10-y-CS-1B-10之4-Nitrophenol催化活性結果 107
3-2-2.4 CuyNi10-y-CS-1B-x之回收利用 112
第四章結論 116
第五章參考文獻 117

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指導教授

高憲明

審核日期

2019-7-23

推文