稻殼灰分擔載銅觸媒應用於氧化性甲醇蒸氣重組產製氫氣之研究

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黃志翔(Chih-Hsiang Huang) 查詢紙本館藏

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化學工程與材料工程學系

論文名稱

稻殼灰分擔載銅觸媒應用於氧化性甲醇蒸氣重組產製氫氣之研究
(Hydrogen production by oxidative steam reforming of methanol over Cu/RHA catalysts)

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摘要(中)

本研究以稻殼為起始原料，經過水洗、酸洗、熱解及碳燒等前處理程序，製成稻殼灰分(非晶型SiO2, 99 %以上)。使用沈澱固著法製備稻殼灰分擔體銅觸媒(簡稱為Cu/RHA觸媒)，再利用氧化性甲醇蒸氣重組反應(OSRM)產製氫氣的程序測試其活性。此反應有良好的氫氣產生速率，以及相當低的一氧化碳選擇率，可避免因一氧化碳濃度太高而毒化燃料電池中的鉑電極。本研究也利用感應耦合電漿原子放射光譜儀（ICP-AES）、熱重分析儀（TGA）、X射線繞射儀（XRD）、掃描式電子顯微鏡（SEM）、X射線光電子分析儀（XPS）、程式升溫還原（TPR）及N2O分解吸附（dissociative adsorption of nitrous oxide）等各項儀器與分析技術，分別對擔體及觸媒進行鑑定。
從XRD結果可看出銅的繞射峰不明顯，應為銅晶粒過小且結晶性不佳。由TPR圖譜可得知，銅載量愈高愈難還原，不同的煅燒溫度有相似的還原溫度。N2O分解吸附的結果，可知當銅載量由5.4 wt%增加到29.9 wt%，其分散度降低，平均粒徑則由1.10增加至3.56 nm，而銅觸媒表面積在載量20.4 wt%為最大。由SEM看出當載量、煅燒溫度增加時，觸媒顆粒皆變大。從XPS的結果中發現，銅觸媒中Cu0有利於OSRM反應。經過活性測試後發現，觸媒的活性與銅的顆粒大小及金屬銅表面積有關係。當銅觸媒表面積愈大且顆粒愈小時，氫氣產生速率愈高，故20.4 wt%的Cu/RHA活性反應較佳。而進料中O2/CH3OH及H2O/CH3OH的莫耳比也是影響反應的重要因素，當O2/CH3OH莫耳比為0.3、H2O/CH3OH莫耳比為1時，有較高的甲醇轉化率與氫氣產生速率，且一氧化碳選擇率可維持在2 %以下。而增加反應溫度，甲醇轉化率、氫氣產生速率與一氧化碳選擇率都會上升，523 K為最佳反應溫度。

摘要(英)

In this work, rice husk ash (RHA) was used as a catalyst support. Selective production of hydrogen by oxidative steam reforming of methanol (OSRM) over Cu/RHA catalysts, prepared by deposition-precipitation method was studied. The catalysts were characterized by ICP-MS, TGA, TPR, Dissociative adsorption of nitrous oxide, XRD, SEM and XPS analyses. XRD patterns of Cu/RHA catalysts indicate that the copper species particles, which are amorphous or very small and highly dispersed within the matrix. From TPR, it was difficult to reduce for higher copper loading and higher calcination temperature. From dissociative adsorption of nitrous oxide, copper loading increases from 5.4 to 29.9 wt% with decrease in dispersion and increase in metallic surface area. When calcination temperature is at 673 K, it has the biggest metallic surface area and smallest particle size. SEM observations show that increasing copper loading, particle size become bigger and increasing calcination temperature, the catalyst is sintering. XPS analyses demonstrate that in calcination at 673 K and reduction at 573 K, the copper states change from copper oxide to metallic copper. The catalytic activity of Cu/RHA catalysts for the OSRM reaction significantly depends on the particle size and surface area of metallic copper. Increasing surface area and decreasing particle size raises the hydrogen production rate. In this study, the catalyst with 20.4 wt% loading and calcined at 673 K shows the highest activity for methanol conversion and hydrogen production. The appropriate molar ratios of O2/CH3OH and H2O/CH3OH for reaction are 0.3 and 1.0, respectively. Both hydrogen production rate and methanol conversion increased with increasing reaction temperature. It has lower carbon monoxide selectivity at 523K. Comparing Cu/RHA with the Cu/SiO2 catalysts by OSRM in the same operating condition, we find that both two catalysts have the same hydrogen production rate and methanol conversion, but the Cu/RHA catalysts produce three times less carbon monoxide than the Cu/SiO2 catalysts.

關鍵字(中)

★ 銅觸媒
★ 氧化性甲醇蒸氣重組
★ 氫氣
★ 稻殼灰份

關鍵字(英)

★ hydrogen
★ copper catalyst
★ oxidative steam reforming of methanol
★ rice husk ash

論文目次

目錄 I
圖目錄 V
表目錄 X
第一章緒論 1
1.1 前言 1
1.2 燃料電池原理 2
1.3 稻殼灰份介紹 4
1.4 甲醇製氫 5
1.5 擔體銅觸媒 7
1.6 研究內容與論文架構 7
第二章文獻回顧 9
2.1 稻殼的組成與性質 9
2.2 稻殼灰分擔體的製備 9
2.2-1 稻殼的酸洗 13
2.2-2 稻殼的熱解 14
2.3 銅觸媒的發展 15
2.4 沈澱固著法製備擔載銅觸媒 16
2.5 煅燒與還原程序 19
2.5-1 煅燒程序 19
2.5-2 還原程序 20
2.6 擔體效應 21
2.7銅金屬表面積的測定 22
2.8 銅的活性位置 23
2.9 氧化性甲醇蒸氣重組反應 24
第三章實驗方法與裝置 29
3.1 稻殼灰分擔體的製備 29
3.1-1 水洗程序 29
3.1-2 酸洗程序 29
3.1-3 熱解程序 30
3.1-4 碳燒程序 32
3.2 擔載銅觸媒的製備 35
3.3 擔體銅觸媒的鑑定分析 36
3.3-1 感應耦合電漿原子放射光譜儀（ICP-AES）分析 38
3.3-2 熱重分析（TGA） 38
3.3-3 X射線繞射分析（XRD） 39
3.3-4 程式升溫還原（TPR） 42
3.3-5 銅金屬表面積的量測 43
3.3-6 掃描式電子顯微鏡（SEM）分析 47
3.3-7 X射線光電子分析（XPS） 48
3.4 觸媒活性測試—氧化性甲醇蒸氣重組產製氫氣反應 52
3.5 實驗流程與操作變數 54
3.5-1 稻殼灰分(RHA)的製備 54
3.5-2 稻殼灰分擔體銅觸媒 (Cu/RHA) 54
3.6 數據的計算與實例 57
3.6-1 銅觸媒理論載量的定義與計算 57
3.6-2 轉化率的定義與計算 58
3.6-3 選擇率的定義與計算 62
3.6-4 產生速率的定義與計算 64
3.7 藥品、氣體及儀器設備 66
3.7-1 藥品 66
3.7-2 氣體 67
3.7-3 儀器設備 67
第四章結果與討論 69
4.1 稻殼灰分組成的分析 69
4.2 物性分析 71
4.2-1 銅離子濃度對銅金屬載量的影響 71
4.2-2 煅燒條件的選擇 74
4.2-3 程式升溫還原(TPR)分析結果 76
4.2-4 觸媒表面積測定 79
4.2-5 X射線繞射分析(XRD) 84
4.2-6 掃描式電子顯微鏡(SEM) 89
4.2-7 X射線光電子分析(XPS) 93
4.3 化性分析 96
4.3-1 銅載量對觸媒活性的影響 96
4.3-2 煅燒溫度對觸媒活性的影響 100
4.3-3 進料比例對觸媒活性的影響 105
4.3-3-1 不同O2/CH3OH 比的影響 105
4.3-3-2 不同H2O/CH3OH莫耳比的影響 111
4.3-4 反應溫度對觸媒活性的影響 117
4.3-5 Cu/RHA與Cu/SiO2分析比較結果 119
第五章結論 127
參考文獻 131

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指導教授

張奉文(Feg-Wen Chang)

審核日期

2008-7-4

推文