近年來台灣空氣污染的情形越來越嚴重，硫成分存在於燃料油品中，經過引擎燃燒後排放成為SO2，逐漸在空氣中反應變成硫酸再藉由沉降形成所謂的酸雨，更嚴重的話會形成二次氣膠降低行車及行人的視線造成交通上的危害。而曝露於低濃度的二氧化硫中，會造成部分敏感族群的支氣管收縮，對於人們呼吸道疾病及肺功能影響皆會造成嚴重的問題。本研究探討再生燃料油脫硫之可行性，生產超低硫燃料，以具有較高比表面積的擔體NaY沸石，先利用氫氧化鈉的溶出性來提升沸石本身中孔(介孔)，並搭配微波製備液相離子交換的方法，將金屬離子引入沸石的骨架中改質成為脫硫吸附劑，後續再進行脫硫試驗並探討出脫硫之可行性。經由實驗來探討吸附材料之吸附效能、吸附容量、再生燃料油脫硫效能，並利用ICP、XRD、SEM、TEM、BET、NH3-TPD、FTIR等儀器分析吸附劑物化特性。

In recent years, the situation of air pollution in Taiwan has become more and more serious. The sulfur component is present in the fuel oil. After being burned by the engine, it is discharged into SO2. It gradually reacts in the air to become sulfuric acid and then forms a so-called acid rain by sedimentation. If it is more serious, it will form. The secondary gas glue reduces the visibility of traffic and pedestrians and causes traffic hazards. Exposure to low concentrations of sulfur dioxide can cause bronchoconstriction in some sensitive groups, which can cause serious problems for people with respiratory diseases and lung function.This study explores the feasibility of desulfurization of regenerated fuel oil, producing ultra-low sulfur fuel, with a higher specific surface area of the carrier NaY zeolite, first using the dissolution of sodium hydroxide to enhance the pores (mesopores) of the zeolite itself, and With the method of microwave preparative liquid phase ion exchange, the metal ions are introduced into the framework of the zeolite to be converted into a desulfurization adsorbent, followed by desulfurization test and the feasibility of desulfurization. The adsorption performance, adsorption capacity, and desulfurization efficiency of regenerated fuel oil were investigated by experiments. The physicochemical properties of the adsorbents were analyzed by ICP, XRD, SEM, TEM, BET, NH3-TPD, FTIR and other instruments.

學位論文審定書 i
謝誌 ii
摘要 iii
ABSTRACT iv
目錄 vi
圖目錄 ix
表目錄 xiii
第一章 前言 1
1-1 研究緣起 1
1-2 研究目的 2
第二章 文獻回顧 3
2-1 沸石基本性質 3
2-1-1 沸石發現與進展 3
2-1-2 沸石結構與分類 3
2-1-3 沸石孔洞特性 5
2-1-4 沸石的應用 6
2-2 吸附 7
2-2-1 吸附基本簡介 7
2-2-2 吸附機制 8
2-2-3 吸附影響因素 9
2-2-4 選擇性吸附 10
2-2-5 吸附等溫曲線 10
2-2-6 脫附遲滯曲線 13
2-2-7 吸附脫硫原理 15
2-3 吸附劑 16
2-3-1 吸附劑特性 16
2-3-2 吸附劑鹼處裡改性 17
2-3-3 吸附劑金屬披覆改質方法 18
2-3-4 吸附系觸媒之活性衰退現象 19
2-3-5 改質後吸附劑特性相關研究 20
2-4 空氣污染二氧化硫 22
2-4-1 二氧化硫危害特性 22
2-4-2 二氧化硫危害影響 23
第三章 研究方法 24
3-1 研究架構與流程 24
3-1-1 NaY沸石利用微波法溶解改性前處裡 25
3-1-2 CuNaY液相微波製備離子交換法 26
3-1-3 利用改質吸附劑進行吸附脫硫試驗 27
3-2 實驗材料與藥品 28
3-3 實驗設備與原理介紹 29
3-3-1 感應耦合電漿原子發射光譜儀 29
3-3-2 元素分析儀 30
3-3-3 環境掃描式電子顯微鏡 31
3-3-4 X光粉末繞射分析儀 32
3-3-5 比表面積分析儀 33
3-3-6 熱重分析儀 34
3-3-7 穿透式電子顯微鏡 35
3-3-8 化學分析電子能譜儀 36
3-3-9 程溫脫附儀 37
3-3-10 傅立葉轉換紅外光譜儀 38
3-3-11 X射線螢光光譜儀 39
3-3-12 密閉式微波設備 40
3-3-13 高溫鍛燒爐 41
3-3-14 循環式送風式烘箱 41
3-3-15 液壓薄片機 42
3-3-16 離心機 42
第四章 結果與討論 43
4-1 NaY沸石基本特性分析 43
4-1-1全量分析(ICP-MS) 43
4-1-2單點元素分析(EDS) 44
4-1-3表面型態鑑定(SEM) 45
4-1-4 X光粉末繞射分析(XRD) 46
4-1-5 比表面積分析(BET) 47
4-2 NaY沸石利用NaOH鹼處裡改性 48
4-2-1不同濃度NaOH對製備中孔吸附劑影響(ICP) 48
4-2-2不同濃度NaOH對製備中孔吸附劑影響(SEM) 50
4-2-3不同濃度NaOH對製備中孔吸附劑影響(TEM) 54
4-2-4不同濃度NaOH對製備中孔吸附劑影響(XRD) 55
4-2-5不同濃度NaOH對製備中孔吸附劑影響(BET) 57
4-2-6不同濃度NaOH對製備中孔吸附劑影響(TPD-NH3) 60
4-2-7不同濃度NaOH對製備中孔吸附劑影響(TGA) 61
4-3 利用微波輻射製備改質金屬銅CuNaY吸附劑 62
4-3-1利用微波輻射製備改質CuNaY吸附劑(ICP) 62
4-3-2利用微波輻射製備改質CuNaY吸附劑(SEM) 64
4-3-3利用微波輻射製備改質CuNaY吸附劑(TEM) 67
4-3-4利用微波輻射製備改質CuNaY吸附劑(XRD) 68
4-3-5利用微波輻射製備改質CuNaY吸附劑(BET) 70
4-3-6利用微波輻射製備改質CuNaY吸附劑(TPD-NH3) 75
4-3-7利用微波輻射製備改質CuNaY吸附劑(TGA) 76
4-3-7利用微波輻射製備改質CuNaY吸附劑(XPS) 77
4-4 利用改質CuNaY吸附劑進行脫硫試驗 78
4-4-1不同硝酸銅濃度對脫硫之影響 78
4-4-2不同加熱溫度對脫硫之影響 79
4-4-3不同吸附時間對脫硫之影響 80
4-4-4脫硫後吸附劑官能基鑑定 81
4-5 成本效益分析 82
4-5-1設備及人力成本估算 82
4-5-2設備操作成本估算 83
4-5-3原料成本估算 84
第五章 結論與建議 86
5-1結論 86
5-2 建議 87
參考文獻 88
 
圖目錄
圖2-1 八面沸石結構 4
圖2-2 A型沸石結構 4
圖2-3 Y型沸石結構 4
圖2-4 吸附過程意象圖 7
圖2-5 物理吸附與化學吸附意象圖 8
圖2-6 Type I 等溫吸附曲線 10
圖2-7 Type II等溫吸附曲線 10
圖2-8 Type III等溫吸附曲線 11
圖2-9 Type IV等溫吸附曲線 11
圖2-10 Type V等溫吸附曲線 12
圖2-11 Type VI等溫吸附曲線 12
圖2-12 脫附遲滯曲線 13
圖2-13凡得瓦力示意圖 15
圖3-1 實驗流程架構圖 21
圖3-2 60 mesh篩網 21
圖3-3 配置NaOH溶液 21
圖3-4 微波輻射處裡 21
圖3-5 抽氣過濾分離 22
圖3-6 經NaOH前處裡載體 22
圖3-7 配置硝酸銅溶液 22
圖3-8 微波輻射處裡 22
圖3-9 抽氣過濾分離 22
圖3-10 高溫爐鍛燒 22
圖3-11 改質CuNaY吸附劑 23
圖3-12 脫硫試驗 23
圖3-13 抽氣過濾分離 23
圖3-14 脫硫後吸附劑 24
圖3-15 感應耦合電漿原子發射光譜儀 26
圖3-16 元素分析儀 27
圖3-17 環境掃描式電子顯微鏡 28
圖3-18 X光粉末繞射分析儀 29
圖3-19 比表面積分析儀 30
圖3-20 熱重分析儀 32
圖3-21 穿透式電子顯微鏡 32
圖3-22 化學分析電子能譜儀 33
圖3-23 程溫脫附儀 34
圖3-24 傅立葉轉換紅外光譜儀 35
圖3-25 X射線螢光光譜儀 36
圖3-26 密閉式微波設備 37
圖3-27 高溫鍛燒爐..................................................................................... 38
圖3-28 循環式送風式烘箱 38
圖3-29 液壓薄片機 39
圖3-30 離心機 39
圖4-1 NaY沸石分析EDS圖譜 44
圖4-2 NaY沸石10000x SEM成像圖 45
圖4-3 NaY沸石20000x SEM成像圖 45
圖4-4 NaY沸石分析XRD圖譜 46
圖4-5 NaY沸石氮氣吸附等溫線 47
圖4-6 在0.5M條件下不同微波溫度及時間對矽鋁比之影響 48
圖4-7 在1.0M條件下不同微波溫度及時間對矽鋁比之影響 49
圖4-8 在1.5M條件下不同微波溫度及時間對矽鋁比之影響 49
圖4-9 在0.5M改性條件在不同微波溫度之SEM成像圖 51
圖4-10 在1.0M改性條件在不同微波溫度之SEM成像圖 52
圖4-11 在1.5M改性條件在不同微波溫度之SEM成像圖 53
圖4-12 母體NaY沸石TEM鏡像圖 54
圖4-13 NaOH改性吸附劑載體TEM鏡像圖 54
圖4-14 在0.5M條件下不同微波溫度XRD圖譜 55
圖4-15 在1.0M條件下不同微波溫度XRD圖譜 56
圖4-16 在1.5M條件下不同微波溫度XRD圖譜 56
圖4-17 不同NaOH濃度及微波溫度對比表面積之影響 58
圖4-18 不同NaOH濃度及微波溫度對孔徑之影響 58
圖4-19 不同NaOH濃度及微波溫度對中孔體積之影響 59
圖4-20 不同NaOH濃度及微波溫度對孔體積之影響 59
圖4-21 母體NaY沸石、NaY-NaOH吸附劑載體TCD曲線圖 60
圖4-22 NaY-NaOH吸附劑載體TGA曲線圖 61
圖4-23 不同微波時間對NaY-NaOH銅離子交換之影響 62
圖4-24 不同濃度硝酸銅改質對NaY-NaOH之影響 63
圖4-25 硝酸銅濃度0.1 M條件下SEM成像圖 64
圖4-26 硝酸銅濃度0.2M條件下SEM成像圖 64
圖4-27 硝酸銅濃度0.5M條件下SEM成像圖 65
圖4-28 硝酸銅濃度1.0 M條件下SEM成像圖 65
圖4-29 硝酸銅濃度1.5M條件下SEM成像圖 66
圖4-30 硝酸銅濃度2.0 M條件下SEM成像圖 66
圖4-31 NaOH改性吸附劑載體TEM鏡像圖 67
圖4-32 CuNaY改質吸附劑TEM鏡像圖 67
圖4-33不同濃度下改質CuNaY之XRD圖譜 68
圖4-34 NaY、NaY-NaOH、CuNaY之XRD圖譜 69
圖4-35 不同濃度下改質CuNaY之比表面積圖 70
圖4-36 CuNaY-0.1M氮氣吸附等溫線 71
圖4-37 CuNaY-0.2M氮氣吸附等溫線 71
圖4-38 CuNaY-0.5M氮氣吸附等溫線 72
圖4-39 CuNaY-1.0M氮氣吸附等溫線 72
圖4-40 CuNaY-1.5M氮氣吸附等溫線 73
圖4-41 CuNaY-2.0M氮氣吸附等溫線 73
圖4-42 不同濃度下改質CuNaY之孔徑圖 74
圖4-43 不同濃度下改質CuNaY之孔體積圖 74
圖4-44 NaY沸石、NaY-NaOH、CuNaY之TCD曲線圖 75
圖4-45 NaY-NaOH、CuNaY之TGA曲線圖 76
圖4-46 改質CuNaY吸附劑XPS分析圖譜 77
圖4-47 不同濃度下改質CuNaY吸附劑對再生燃料油脫硫之影響 78
圖4-48 不同濃度下改質CuNaY吸附劑對再生燃料油去硫率之分析 79
圖4-49 不同加熱溫度條件下對再生燃料油去硫率之分析 79
圖4-50 不同反應時間條件下對再生燃料油去硫率之分析 80
圖4-51 NaY 沸石、NaY-NaOH、 CuNaY之FTIR分析圖譜 81



 
表目錄
表2-1 IUPAC定義孔徑大小 5
表2-2 物理吸附與化學吸附之差異 8
表2-3 各種改質沸石相關文獻參考 18
表2-4 各種吸附劑相關用途介紹 18
表3-1 實驗使用藥品及耗材 25
表4-1 NaY沸石之組成份 43
表4-2 NaY沸石比表面積分析數據 47
表4-3 IUPAC定義孔徑範圍 47
表4-4 不同NaOH濃度及微波溫度對比表面積之結果 57
表4-5 NaY沸石元素分析結果 61
表4-6 不同硝酸銅濃度對比表面積之結果NaY沸石元素分析結果 70
表4-7 設備及人力成本估算 80
表4-8 操作設備電費成本 81
表4-9 電價表 81
表4-10 年平均電價計算 82
表4-11 原料成本分析估算 82
表4-12 微波進行吸附劑製備所需成本分析 83

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