臺灣博碩士論文加值系統

　　整合式氣化複循環發電技術( Integrated Gasification Combined Cycle，IGCC )因其具有氣化材料之進料選擇多、低成本高效能，且接近零碳排的特點是現今國內外積極研究發展的項目之一。將催化型薄膜反應器應用於IGCC發電技術，被視為可有效降低發電成本之可行技術之一；催化型薄膜反應器為一項整合IGCC發電程序中水氣轉移催化反應與生成氣體H2、CO2分離之新穎技術，其目的為透過將反應生成之產物於過程中立即的移除，藉此破壞熱力學平衡以提升催化反應之效能。本研究將管柱式碳分子篩選薄膜結合Cu/Zn/SBA–16觸媒建構成催化型薄膜反應器，將其應用於模擬合成氣進行水氣轉移反應並對其效能進行評估。
管柱式碳分子篩選薄膜因具有高比表面積且易與觸媒整合之特點，同時碳膜材料本身具備高滲透分選及耐水熱和化學穩定性等優點，為一項適用於水氣轉移薄膜反應器之薄膜材料。本研究以真空輔助浸塗法製備管柱式碳分子篩選薄膜，探討之製備參數包含鑄膜液濃度、基材浸沒鑄膜液時間、以TiO2修飾層改質基材等，對碳分子篩選薄膜氣體分選效能之影響。研究結果顯示，薄膜厚度會隨著鑄膜液濃度、基材浸沒鑄膜液時間之提高而有增加之趨勢；透過TiO2修飾層改質基材不僅可有效地修飾基材內部之缺陷，降低鑄膜液過度滲入基材而造成低滲透率的情形，同時能夠提升對氣體之滲透選擇率；最佳條件為以1350 ℃鍛燒之塗覆四層TiO2修飾層作為基材、鑄膜液濃度為20 wt.%、基材浸沒鑄膜液時間20秒、塗覆2層，其H2/CO2選擇係數為3.59，H2滲透率為2,312 Barrer、CO2滲透率為768 Barrer。接著利用共沉澱法製備出Cu/Zn/SBA–16水氣轉移觸媒，將其應用於固定床催化反應中，結果顯示CO轉化率、H2生成率隨反應溫度提高、空間速度降低皆有增加之趨勢。最佳之催化效果出現於操作在反應溫度為300 ℃、空間速度2,500 h-1及水氣含量S/C (Steam /CO ratio) = 1時，CO轉化率為82.76%。最後以相同操作參數將Cu/Zn/SBA–16觸媒應用於薄膜反應器內，結果顯示CO轉化率相較於固定床反應器提升了4.19%，透過使用催化型薄膜反應器不僅能有效提升CO轉化率和H2生成率，同時能夠縮短反應達平衡的時間。

To develop clean electricity, Integrated Gasification Combined Cycle (IGCC) electricity generation technology has been considered as a key role in 21st century. In the IGCC process, the production of hydrogen (H2) with carbon dioxide (CO2) via water gas shift (WGS) reaction was applied after gasification system to enhance the H2 generation capacity. However, due to the thermodynamic limits of equilibrium, the WGS reaction should be occurred at low temperature and the CO conversion rate cannot be high. The increase of the CO conversion above the equilibrium values appears to be possible when product, i.e. H2 and CO2, is removed through the membrane. Therefore, in this study, the carbon molecular sieve (CMS) membrane will be integrated into the IGCC system to combine the WGS system into the catalytic membrane reactor (MR). The effect of feeding pure reagents on the MR efficiency was evaluated to determine the best conditions in terms of CO conversion. At this purpose, experimental tests were carried out in two different systems of reaction: (1) traditional fixed-bed reactor, and (2) MR with CMS membrane.
As being membrane material for membrane reactor, CMS has the advantages of high specific area and could be integrated with catalyst easily. Besides, carbon membrane also exhibits high selectivity and good chemical stabilization. In this study, the CMS membrane was prepared using polyethyleneimine as precursor and then coated on porous Al2O3 macroporous tubes to form tubular CMS membrane. Parameters including concentration of casting solution, immerse time of substrate and TiO2/Al2O3 substrate modified were evaluated in terms of gas permeaselectivity. The results indicated that the thickness of membrane become larger with the increasing concentration of casting solution and immerse time of substrate. With the modification of TiO2, not only the defects of substrate has been mitigated which leads to the prevention of exceeding access of casting solution into the substrate, but promotes the permeaselectivity. The best parameter in this work is Ti4_1350-20w-20s-2L, gas selectivity of H2/CO2 = 3.59, the permeability of H2 2,312 Barrer and CO2 768 Barrer.

總目錄
摘要 i
Abstract iii
表目錄 viii
圖目錄 ix
第一章　前言 1
1.1 研究緣起 1
1.3 研究目的 6
1.4 研究架構 6
第二章　文獻回顧 10
2.1碳捕獲CCS 10
2.2 整合式氣化複循環發電技術IGCC 13
2.2.1 氣化機制 14
2.2.2 薄膜反應器 18
2.3 水氣轉移反應 21
2.3.1 水氣轉移反應概述 21
2.3.2 影響水氣轉移反應之操作參數 23
2.4水氣轉移反應觸媒 29
2.4.1觸媒之催化特性 29
2.4.2 水氣轉移觸媒之催化反應 32
2.4.3 觸媒之種類與組成 33
2.4.4 觸媒擔體材料 34
2.4.5 觸媒的製備方法 36
2.5 薄膜技術 42
2.5.1氣體分離薄膜之種類 42
2.5.2 薄膜之氣體分離原理與傳輸機制 44
2.6 碳分子篩選薄膜簡介 53
2.6.1 碳分子篩選薄膜之製備 54
2.6.2 碳分子篩選薄膜改質技術 59
2.7 文獻總結 60
第三章　實驗設備與方法 62
3.1實驗藥品及氣體 62
3.2 實驗儀器及設備 63
3.3 薄膜製備流程 65
3.3.1 TiO2修飾層之製備 65
3.3.2 製備碳分子篩選薄膜 66
3.4 擔體與觸媒之製備 67
3.4.1 SBA-16擔體之製備流程 67
3.4.2 Cu/Zn/SBA-16觸媒之製備流程 67
3.5 材料特性分析儀器之簡介 69
3.6 薄膜氣體滲透測試 73
3.6.1 單一氣體滲透測試 73
3.6.2 混合氣體於固定床/薄膜反應器之催化分離測試 75
3.7實驗試程 77
第四章　結果與討論 79
4.1 薄膜特性分析 80
4.1.1 TiO2/Al2O3 基材微觀形態 80
4.1.2 TiO2/Al2O3 基材微觀形態 83
4.1.3 TiO2 / Al2O3 基材微觀形態 – AFM分析 85
4.1.4 Carbon/TiO2/Al2O3 機械互鎖能力評估 87
4.1.5 薄膜厚度 89
4.2管柱式碳分子篩選薄膜之氣體分選效能 92
4.2.1鑄膜液濃度與抽真空浸沒時間對C/Al2O3薄膜之影響 92
4.2.2鑄膜液濃度與抽真空浸沒時間對C/TiO2/Al2O3之影響 96
4.2.3 管柱式碳分子篩選薄膜之選擇效能 98
4.3觸媒特性分析 100
4.3.1 擔體與觸媒微觀形態–SEM、TEM分析 100
4.3.2 擔體與觸媒孔洞結構 – BET分析 102
4.3.3 擔體與觸媒孔洞結構 – XRD分析 103
4.4 試驗操作參數對Cu/Zn/SBA–16觸媒催化之影響 105
4.4.1 反應溫度對Cu/Zn/SBA–16觸媒催化反應之影響 105
4.4.2空間速度對Cu/Zn/SBA–16觸媒催化反應之影響 108
4.4.3水汽含量對Cu/Zn/SBA–16觸媒催化反應之影響 111
4.5催化型薄膜反應器對Cu/Zn/SBA–16觸媒催化反應之影響 114
第五章　結論與建議 117
5.1 結論 117
5.1.1管柱式碳分子篩選薄膜 117
5.1.2水氣轉移反應 118
5.1.3催化水氣轉移碳分子篩選薄膜反應器 118
5.2 未來研究與建議 119
參考文獻 120
附錄 135

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