製備奈米鈀金屬於具羧酸官能基中孔洞矽材在有機催化反應之應用

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許茗郡(Ming-Chun Hsu) 查詢紙本館藏

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製備奈米鈀金屬於具羧酸官能基中孔洞矽材在有機催化反應之應用

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至系統瀏覽論文 (2026-2-1以後開放)

摘要(中)

本論文主要分為兩大部分，在第一部分研究中，超小奈米鈀金屬還原在具羧酸官能基之二維結構SBA-15中孔洞矽材(S15C20)以及三維結構KIT-6中孔洞矽材(K6C20)之中。利用化學還原劑使金屬還原速率上升，並藉由S15C20以及K6C20表面原有的羥基及官能化的羧酸基，使離子鈀金屬能快速平均分散並負載在孔洞之中並還原奈米鈀金屬顆粒。由於S15C20以及K6C20具有高比表面積以及良好的孔洞體積，故使用S15C20以及K6C20作為載體可以提高奈米鈀金屬分散率和負載率從而提高催化活性。本實驗將製成的Pd(x)@S15C20以及Pd(x)@K6C20應用在催化氯苯加氫脫氯反應當中，分別探討二維結構以及三維結構以及不同溶劑對催化活性之影響。經過一系列的研究使用Pd(2)@K6C20作為催化劑去進行氯苯加氫脫氯反應，其轉換頻率 (TOF) 達50 h-1。在這項研究中，Pd(2)@K6C20展示了其應用於催化氯苯加氫脫氯是高活性的催化劑。
在第二部分研究中，接續使用與第一部分相同的催化劑。本實驗將Pd(x)@S15C20以及Pd(x)@K6C20應用在催化六價鉻還原反應當中。在催化六價鉻還原反應的研究中Pd(0.5)@S15C20表現出很高的催化活性，其TOF高達8.85 min-1。在這項研究中，Pd(0.5)@S15C20展現出其作為催化六價鉻還原反應的催化劑是非常具有前景的。

摘要(英)

The use of palladium nanoparticles (Pd NPs) as catalysts for various c catalytic reactions is getting tremendous attention recently because of their high catalytic activity and stability. However, the Pd NPs aggregates very easily due to the high surface energy, which reduces the stability of the catalyst considerably. Synthesis of stable and highly dispersed Pd nanoparticles remains a great challenge. In this thesis, synthesis of highly dispersed Pd NPs using –COOH functionalized 2D hexagonal mesoporous silica SBA-15 (S15C20) and –COOH functionalized 3D cubic mesoporous silica KIT-6 (K6C20) as the supports have been reported. Mesoporous silica supports S15C20 and K6C20 are prepared by one pot co-condensation method. The Pd nanoparticles are immobilized within the mesopores of the supports S15C20 and K6C20 by double agent chemical reduction method. The particle size of Pd NPs ranges from 5.0 to 6.3 nm and 4.8 to 6.0 nm for Pd(x)@S15C20 and Pd(x)@K6C20, respectively, depending on molar amount of Pd loadings. The formation of highly dispersed Pd nanoparticles within the supports could be attributed to the homogenous distribution of the –COOH functional groups in S15C20 and K6C20. The prepared Pd(x)@S15C20 and Pd(x)@K6C20 are used as catalysts for the catalytic hydrodechlorination of chlorobenzene, and the catalytic reduction of environmentally harmful Cr(VI) to Cr (III).
Pd(x)@S15C20 and Pd(x)@K6C20 exhibited superior catalytic activity for the catalytic hydrodechlorination of chlorobenzene under mild conditions with ammonium formate (HCOONH4) as a hydrogen donor. Amongst all the catalysts, Pd(2)@K6C20 exhibits the highest turnover frequency (TOF) of 50 h-1. The Pd(2)@K6C20 also exhibited excellent stability after used for three successive cycles without significant loss of its catalytic activity.
Both the prepared catalysts Pd(x)@S15C20 and Pd(x)@K6C20 could effectively reduce environmentally harmful Cr(VI) to Cr (III) in presence of reducing agent formic acid (HCOOH) and promoter sodium formate (HCOONa) under mild conditions. Amongst all the catalysts, Pd(0.5)@S15C20 exhibited the highest turnover frequency of 8.85 min-1. In addition, Pd(0.5)@S15C20 showed excellent stability and recyclability which could retain high conversion after reuse for five times.

關鍵字(中)

★ 中孔洞矽材

關鍵字(英)

論文目次

中文摘要 I
ABSTRACT II
謝誌 IV
目錄 VI
圖目錄 XI
表目錄 XVII
第一章序論 1
1-1 中孔洞二氧化矽 1
1-1-1中孔洞材料之介紹 1
1-1-2中孔洞二氧化矽合成方法 4
1-1-3軟性模板-微胞結構 6
1-2 二維及三維中孔洞二氧化矽 10
1-2-1二維與三維的差異 10
1-2-2二維結構SBA-15 11
1-2-3三維結構KIT-6 12
1-3 有序中孔洞有機矽材（PMO’s） 13
1-3-1中孔洞材料表面之官能基修飾方法 14
1-3-2含羧酸官能基之中孔洞材料發展 16
第壹部分鈀金屬催化氯苯加氫脫氯反應 19
1-4 鈀金屬催化氯苯加氫脫氯反應 19
1-4-1金屬催化氯苯加氫脫氯反應機制介紹 19
1-4-2奈米金屬鈀催化氯苯加氫脫氯反應文獻回顧 20
第貳部分鈀金屬催化六價鉻還原反應 23
1-5 鈀金屬催化六價鉻還原反應 23
1-5-1六價鉻介紹 23
1-5-2金屬催化六價鉻還原機制介紹 24
1-5-3奈米金屬鈀催化六價鉻還原反應文獻回顧 25
1-6 研究動機與目的 27
第二章實驗部分 29
2-1 實驗藥品 29
2-2 實驗設備 31
2-2-1實驗合成設備 31
2-2-2實驗鑑定儀器 31
2-3 鑑定儀器之原理 33
2-3-1同步輻射光束線 33
2-3-2 X射線粉末繞射（PXRD） 35
2-3-3傅立葉紅外線吸收光譜儀（FTIR） 36
2-3-4固態核磁共振（Solid State NMR） 37
2-3-5氮氣吸脫附等溫曲線、表面積與孔洞特性鑑定 46
2-3-6穿透式電子顯微鏡（TEM） 51
2-3-7光電子能譜（XPS） 53
2-3-8紫外光-可見光光譜儀（UV-Vis） 54
2-4 實驗步驟 55
2-4-1具羧酸官能基中孔洞矽材SBA-15 (S15C20) 合成 55
2-4-2具羧酸官能基中孔洞矽材KIT-6 (K6C20) 合成 56
2-4-3以硫酸溶液裂解孔洞中的模板 57
2-4-4以PdCl2做為前驅物還原至S15C20與K6C20之中 57
2-5 催化氯苯加氫脫氯重複使用實驗 59
2-5-1 Pd(x)@S15C20與Pd(x)@K6C20催化氯苯加氫脫氯實驗 59
2-5-2催化氯苯加氫脫氯重複使用實驗 60
2-6 鈀金屬催化六價鉻還原反應實驗 61
2-6-1 Pd(x)@S15C20與Pd(x)@S15C20催化六價鉻還原實驗 61
2-6-2催化六價鉻還原重複實驗 61
第三章結果與討論 62
3-1 Pd(x)@S15C20及Pd(x)@K6C20基本性質鑑定 62
3-1-1 SAXRD繞射圖譜 62
3-1-2 WAXRD繞射圖譜 66
3-1-3 FT-IR光譜 68
3-1-4 13C CP/MAS NMR 70
3-1-5等溫氮氣吸脫附 71
3-1-6 TEM圖像 77
3-1-7 XPS結果分析 89
第壹部分鈀金屬在中孔洞矽材催化氯苯加氫脫氯反應 92
3-2 鈀金屬催化氯苯加氫脫氯反應實驗 92
3-2-1 Pd(x)@S15C20氯苯加氫脫氯 92
3-2-2 Pd(x)@K6C20氯苯加氫脫氯 94
3-2-3不同材料對催化氯苯加氫脫氯反應之比較 96
3-2-4不同溶劑對催化氯苯加氫脫氯反應之比較 98
3-2-5不同溫度對催化氯苯加氫脫氯反應之比較 100
3-2-6不同鹵苯對催化加氫脫鹵反應之比較 102
3-2-5 Pd(2)@K6C20催化氯苯加氫脫氯重複利用之實驗 105
3-2-5.1 Pd(2)@K6C20 5th回收利用 105
3-2-5.2 Pd(2)@K6C20 5th WAXRD繞射圖譜 105
3-2-5.3 Pd(2)@K6C20 5th TEM圖譜 107
第貳部分鈀金屬在中孔洞矽材催化六價鉻還原反應 109
3-3 Pd(x)@S15C20及Pd(x)@K6C20六價鉻還原反應 109
3-3-1 Pd(x)@S15C20六價鉻還原 111
3-3-2 Pd(x)@K6C20六價鉻還原 113
3-3-3 Pd(0.5)@S15C20催化六價鉻還原重複利用之實驗 116
3-3-3.1 Pd(0.5)@S15C20 5th回收利用 116
3-3-3.2 Pd(0.5)@S15C20 5th WAXRD繞射圖譜 117
3-3-3.3 Pd(0.5)@S15C20 5th TEM圖譜 118
第四章結論 120
第五章參考文獻 122

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指導教授

高憲明

審核日期

2021-1-29

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