臺灣博碩士論文加值系統

論文分為二個部分，第一部分利用分子篩吸附有機硫化物噻吩，第二部分為中孔洞SBA-1穩定性的研究
第一部分所使用之沸石吸附劑為商業化沸石。以液態離子交換法 (Liquid phase ion exchange) 與氣態離子交換法 (Vapor phases ion exchange) 將銅離子負載於商業化沸石上，利用固定床式吸附法 (fixed-bed filters) 進行吸附研究，探討銅離子對吸附噻吩分子的影響，並使用熱程控還原 (Temperature programmed reduction, TPR) 、感應耦合電漿質譜儀 (Inductively coupled plasma-mass spectrometer, ICP-MS) 、X-光螢光分析儀 (X-ray Fluorescence Spectrometer, XRF ) 和反射式紫外-可見光光譜儀 (UV-VIS Spectrophotometer) 等儀器進行分析。由結果發現吸附沸石的能力與沸石自身的孔洞大小有關，商業化沸石中孔洞較大者具有較佳的吸附效果，且經由負載一價銅離子可藉由 π-complexation 的作用力提升吸附能力。文中並探討負載銅離子的方法，發現以氣態離子交換法相較於傳統的液態離子交換法更能有效的負載一價銅於沸石上，吸附能力依序如下 Cu(I)-Ferrierite < Cu(I)-Mordenite < Cu(I)-CaX < Cu(I)-ZSM-5 < Cu(I)-Beta < Cu(I)-Y。除了商業化沸石之外，本研究還利用孔洞較大的中孔洞 SBA-15 進行吸附研究，但由於 SBA-15 的孔洞太大，反而不能有效的吸附噻吩分子。
第二部分為中孔洞 SBA-1 穩定性的研究，利用四種矽源 TMOS (Tetramethyl orthosilicate)、TEOS (Tetraethyl orthosilicate)、TPOS (Tetrapropyl orthosilicate) 和 TBOS (Tetrabutyl orthosilicate) 合成 SBA-1，此四種矽源水解速率不同且水解亦產生不同的醇類，對微胞的影響也不同，因而影響堆積常數的數值，造成孔洞材料結構的差異。發現以 TMOS 為矽源可在較大的溫度範圍 (273 K ~ 323 K) 合成出 SBA-1，TEOS 與 TPOS 則因溫度的影響，會合成出 SBA-1 與 SBA-3 的混相，而 TBOS 則無法合成 SBA-1。文中並深入探討以 TMOS 所合成 SBA-1 的熱穩定性與水煮穩定性，在熱穩定性部分發現耐熱溫度可達 1123 K，且仍有 642 m2/g 的孔洞表面積。水煮穩定性部分，則發現耐水煮時間最少可到達 4 小時，水煮時間達 8 小時和 12 小時後仍為有結晶性的 SBA-1 ，但 XRD 的強度較弱，相較於 TEOS 有較好的水煮穩定性。

The thesis is divided into two parts. First, adsorption of the organic sulfur compounds thiophene (TP) by zeolites which were ion exchanged either by vapor phase ion exchange (VPIE) or liquid phase ion exchange (LPIE). The adsorptions were studied in a fixed-bed adsorber operated at ambient temperature and pressure. The vapor phase ion exchange method can effectively exchange cation with the proton in zeolite more than liquid phase ion exchange method. The adsorbability tests for surfur adsorption capacity at breakthrough follow the order Cu(I)-Ferrierite < Cu(I)-Mordenite < Cu(I)-CaX < Cu(I)-ZSM-5 < Cu(I)-Beta < Cu(I)-Y. After adsorption, some zeolites have color changed due to polymerization of thiohpene. Besides zeolite, mesoporse SBA-15 was also used to adsorb thiophene but it can not adsorb thiophene.
In the second part of the thesis, the critical role of silica precursors in the synthesis of the cubic SBA-1 mesophase under strongly acidic condition at different synthesis temperatures has been investigated. The present of higher concentration of corresponding alcohol due to the hydrolysis of silica precursors, which effectively serve as cosolvent or as cosolution to interference the surfactant parking parameter, is a key factor for mesoporous to shape up. Further, we also used TMOS as main silica precursor to synthesis SBA-1 and then tested the thermal stability and boiling water stability of it. At the thermal stability part, the heat-resistant of SBA-1 can stand at least 1123K and still have the pore surface 642 m2/g. At the boiling water stability part, TMOS can stand at least four hours and without decrease the intensity of XRD and is better than using TEOS as silica precursor.

中文摘要 I
英文摘要 III
目錄 IV
圖目錄 VIII
表目錄 XII
PART I 1
第一章 序論 1
1.1 簡介 1
1.2 柴油中硫含量規範 2
1.3 油品含硫成份 4
1.4 沸石與分子篩 6
第二章 文獻回顧 10
2.1 油品脫硫研究 10
2.1.1 加氫脫硫 11
2.1.2 生物脫硫技術 13
2.1.3 液體/液體萃取脫硫法 16
2.1.3.1 具綠色化學概念的溶劑－室溫離子液體 16
2.1.4 氧化脫硫 18
2.1.5 吸附劑脫硫法 21
2.1.5.1 S Zorb 製程 21
2.1.5.2 IRVAD 製程 21
2.2 吸附劑特性 22
2.2.1 熱力學特性 22
2.2.2 動力學特性 22
2.2.2.1 固定床 (fixed-bed) 反應器 23
2.2.3 穩定性 26
2.2.4 其他特性 26
2.3沸石吸附劑吸附硫化物 27
第三章 實驗部分 30
3.1實驗藥品與儀器 30
3.1.1 實驗藥品 30
3.1.2實驗儀器 31
3.2實驗裝置與操作步驟 32
3.2.1 實驗裝置 32
3.2.2 操作步驟 33
3.3 實驗裝置校正 35
3.3.1 噻吩產生器之攜帶氣體流量校正 35
3.3.2. 混合空氣流量校正 37
3.3.3 thiophene 流量與濃度關係 38
3.4 吸附劑製備 39
3.4.1 液態離子交換 39
3.4.2 氣態離子交換 39
3.5 液態吸附實驗 40
第四章 實驗結果與討論 42
4.1 物性分析 42
4.1.1 還原溫度測試 42
4.2. 不同沸石對噻吩的吸附研究 45
4.2.1 商業化沸石對噻吩的吸附研究 45
4.2.2 二價銅離子對噻吩吸附的影響 47
4.2.3 一價銅離子對噻吩吸附的研究 49
4.3 Y 沸石對噻吩的吸附測試 52
4.3.1 不同陽離子對噻吩吸附的影響 52
4.3.2 X 光螢光分析儀 (X-Ray Fluorescence Spectrometer, XRF) 元素分析 55
4.3.3 不同負載溫度對噻吩吸附的影響 56
4.4 Beta 沸石對噻吩的吸附研究 57
4.4.1 負載一價銅於 Beta 對噻吩吸附的影響 57
4.4.2 不同矽鋁比 HBeta 對噻吩吸附的影響 59
4.4.3 氣態離子交換法負載一價銅於沸石上的吸附研究 60
4.4.4 吸附劑顏色變化探討 63
4.5 利用中孔洞沸石吸附噻吩研究 67
4.5.1官能基化中孔洞分子篩簡介 67
4.5.2含鋁 SBA-15 中孔洞分子篩 68
4.5.3 Cu+/Al-SBA-15之合成 69
4.5.3.1 Al-SBA-15之合成步驟 69
4.5.4 Al-SBA-15之鑑定 71
4.5.4.1 XRD 結果 71
4.5.4.2 氮氣等溫吸脫附結果 73
4.5.4.3 27Al NMR 結果 75
4.5.4.4 Cu+負載於中孔洞材料 76
4.5.5 中孔洞沸石對噻吩的吸附研究 77
第五章 結論 80
參考文獻 (part I) 82
PART II 89
第一章 序論 89
1.1 中孔徑分子篩簡介 89
1.1.1 分子篩的發展 89
1.2 中孔洞分子篩的形成機制 91
1.2.1 界面活性劑的微胞性質介紹 91
1.2.2 微胞的形成與種類 92
1.2.3 中孔洞分子篩的合成機制介紹 95
1.2.3.1 液晶模板機制 (Liquid Crystal Templating Mechanism) 96
1.3 文獻回顧 103
1.3.1 SBA-1 中孔洞分子篩 103
1.3.2 SBA-1 的形成機制 103
1.3.3中孔洞材料結構的轉變 105
1.3.4 SBA-1 的鑑定 110
1.4 研究動機與目的 116
第二章 文獻回顧 117
2.1 化學藥品 117
2.2 實驗設備 118
2.2.1 實驗合成設備 118
2.2.2 實驗鑑定儀器 118
2.3 SBA-1分子篩的合成步驟 119
2.3.1 界面活性劑之合成 119
2.3.2 使用不同矽源的 SBA-1 之合成 119
2.3.3 SBA-1 熱穩定性測試 119
2.3.4 SBA-1 水洗測試 120
2.3.5 SBA-1 水煮測試 120
2.4 鑑定儀器之條件與原理 120
2.4.1 同步輻射中心光束線 (NSRRC Beam Line) 120
2.4.2 X 光粉末繞射 (Powder X-Ray Diffractometer；XRD) 120
2.4.3 氮氣等溫吸附/脫附測量 (Nitrogen sorption measurements) 122
2.4.4 低真空掃描式電子顯微鏡 (LV-SEM) 125
2.4.5 固態核磁共振 (Solid State NMR) 125
2.4.5.1 29Si MAS NMR 126
第三章 結果與討論 127
3.1 不同矽源合成SBA-1之研究 127
3.2 SBA-1穩定性研究 137
3.2.1 SBA-1 熱穩定性研究 137
3.2.2 耐水性研究 166
3.2.2.1 水洗研究 166
3.2.2.2 水煮研究 168
3.2.3增加合成酸量對 SBA-1 穩定性的研究 188
第四章 結論 199
參考文獻 (part II) 201
附錄 A CsHPW 204
A-1 HPW 簡介 204
A-2 研究動機 204
A-3 實驗部份 205
A-4 結果 206
A-4-1 XRD結果 206
A-4-2 NMR結果 209
A-5 REDOR (Rotational-Echo Double Resonance) 實驗 220
參考文獻 (附錄) 232

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