CuO/Ce1-xMnxO2-Al2O3觸媒於富氫中CO的選擇性氧化反應研究

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彭均婷(Chun Ting) 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

CuO/Ce1-xMnxO2-Al2O3觸媒於富氫中CO的選擇性氧化反應研究
(CuO/Ce1-xMnxO2-Al2O3 catalysts for the preferential oxidation of CO in H2-rich gases)

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摘要(中)

摘要
本研究嘗試於CeO2引入不同比例的Mn，製備Ce1-xMnxO2擔體及CuO/Ce1-xMnxO2觸媒。為了增進觸媒之機械強度與穩定度，另外於Ce1-xMnxO2¬擔體中引入不等量Al2O3與製備CuO/Ce1-xMnxO2-Al2O3觸媒。本研究分別探討CuO/Ce1-xMnxO2觸媒與CuO/Ce1-xMnxO2-Al2O3觸媒之CO選擇性氧化反應特性，並採用BET、TPR、XPS、Raman、CO脈衝吸附與Auger等分析方法探討觸媒之物理特性與表面性質。CO/O/H2/He = 1/1/50/48進料及F/W = 10,000 ml hr-1 g-1下，進行CuO/Ce1-xMnxO2-Al2O3觸媒的活性測試。
CeO2擔體中引入少量的錳(x = 0.1~0.3)，錳是以正四價的形式固溶於CeO2擔體晶格中，形成良好固溶的氧化物Ce1-xMnxO2，Ce1-xMnxO2氧化物較易釋出晶格氧，有較佳redox特性。當錳的引入量大於0.3，會有分離相的產生，錳是以三價的形式存在。
7%CuO/Ce1-xMnxO2觸媒，引入少量Mn (x = 0.1)，觸媒活性增加，達CO完全轉化的T100下降5°C (90~95°C)，此時選擇S100約為100%；Mn引入量0.20.5時，則不利於觸媒活性。反應溫度小於100°C，選擇率均維持100%，反應溫度大於100°C，選擇率始明顯下降。
7%CuO/Ce1-xMnxO2-20%Al2O3觸媒與未引入Al2O3之觸媒相較，其T100大約上升5~10°C。Mn的引入量x = 0.1~0.2，T100為95~100°C與未引入Mn之觸媒相較，下降5°C；x = 0.3，T100為100~105°C，與未引入之Mn之觸媒T100相當。Mn引入量對7%CuO/Ce1-xMnxO2與7%CuO/ Ce1-xMnxO2-20%Al2O3之影響相似。
7%CuO/Ce0.9Mn0.1O2-x%Al2O3觸媒，Al2O3引入量x = 10~30%，觸媒活性差異不大，T100溫度95~100°C，Al2O3引入量大於30%，才稍不利於CO選擇性氧化反應。Al2O3引入量x = 40%時，T100溫度略升 5°C，溫度為100~105°C，選擇率由100%下降至95%。
CO2及H2O對 7%CuO/Ce0.9Mn0.1O2-20%Al2O3觸媒明顯影響，於進料氣中引入15% CO2，T100明顯增至130~135°C，S100下降至71%；於進料中引入10% H2O，會造成觸媒床堵塞，以致無法順利進行。若以無CO2及H2O的進料在100°C下進行7%CuO/Ce0.9Mn0.1O2-20%Al2O3觸媒的穩定性測試，經200小時反應，轉化率由100%僅降至93%。7%CuO/ Ce0.9Mn0.1O2-20%Al2O3觸媒有強吸水性，不適用於燃料電池的CO去除反應，但仍適用於一般的CO氧化反應上。

摘要(英)

Abstract
In our previous studies, doping MnOx into CeO2 increase the mobility of lattice oxygen and enhanced the activity of the activity of the 7%CuO/Ce1-xMnxO2 catalyst in the selective oxidation of CO in the H2-rich feed. In order to promote of mechanical strength and the stability of support, moreover to Alumina was incorporated with the solid solution of Ce1-xMnxO2 to form Ce1-xMnxO2-Al2O3 mixed oxides, by the suspension /co-precipitation method, to be used as supports ofCuO/Ce1-xMnxO2-Al2O3 catalyst. They were characterized and effects of Al2O3 on the selective oxidation of CO in excess hydrogen were examined. Characterization of catalysts were performed by XRD, TPR, XPS, Auger. All catalysts were reduced to room temperature in helium and then the feed H2/CO/O2/He(50/1/1/48) mixed was diverted to the reactor at a flow rate of 30ml/ min (F/W = 10,000ml/g h).
For Ce1-xMnxO2 with x = 0.1~0.3, incorporating an appropriate amount of Mn4+ into the CeO2 lattice to form a solid solution facilitated the release of the bulk lattice oxygen. Some MnOx might aggregate and be split out from the solid solution of Ce1-xMnxO2 as the fraction of Mn incorporated excess 0.3, and then Mn3+ into the CeO2.
7%CuO/Ce0.9Mn0.1O2 catalyst was the most active one, it was more active than the 7%CuO/CeO2 catalyst, with a T100 temperature (90-95°C) for complete conversion that was above 5°C less than that of 7%CuO/CeO2 (95-100°C) and the selective oxidation of CO was still 100%. The promotion of CO oxidation became weaker as the fraction of Mn incorporated increase above 0.5.
For doping appropriate small friction as the amount of Mn about o.1 into the Ce1-xMnxO2 for 7%CuO/Ce0.9Mn0.1O2-x%Al2O3 catalysts. This interfacial perimeter also decreased as the amount of Al2O3 incorporated into Ce0.9Mn0.1O2-x%Al2O3 increased above 30%, so that CO oxidation became weaker.
Because a gas stream from reformer always contains CO2 and H2O, so that a catalyst of selective oxidation of CO must be resistant to both CO2 and H2O. The 7%CuO/Ce1-xMnxO2-20%Al2O3 catalyst rose by about 35°C from 95-100°C to 130-135°C when an H2-rich feed in presence of 15%CO2. The 7%CuO/Ce1-xMnxO2-20%Al2O3 created the catalyst bed to stop up and reaction can not finish, so that the catalyst had the hygroscopicity. A long (200 h) run over the 7%CuO/Ce0.9Mn0.1O2-20%Al2O3 catalyst was conducted at 100°C, with about 93% conversion; the performance was stable when the feed no CO2 and H2O.

關鍵字(中)

★ 含浸法
★ 富氫中CO氧化

關鍵字(英)

★ MnOx
★ CeO2
★ TPR

論文目次

目錄
摘要 i
Abstract iii
誌謝 v
目錄 vi
圖目錄 ix
表目錄 xii
第一章緒論１
第二章文獻回顧３
2-1 燃料電池的發展背景３
2-2 CO選擇性氧化觸媒５
2-2-1 Au觸媒５
2-2-2 Pt觸媒６
2-2-3 Rh、Ru觸媒８
2-2-4 CuO觸媒９
2-3 CeO2擔體與CuO-CeO2觸媒１１
2-4 CexZr1-xO2共氧化物與CuO/CexZr1-xO2觸媒１５
2-5 CexSn1-xO2共氧化物與CuO/CexSn1-xO2觸媒１７
2-6 Ce1-xMnxO2共氧化物１８
第三章實驗方法與設備２０
3-1 Ce1-xMnxO2-Al2O3擔體之製備２０
3-2觸媒製備２０
3-3氫-程溫還原 (H2-TPR) ２１
3-4脈衝式CO吸附２２
3-5全表面積量測２３
3-6 X-射線繞射分析(XRD) ２４
3-7顯微拉曼光譜儀２４
3-8 X-射線光電子光譜(XPS) ２５
3-9元素組成分析(ICP) ２６
3-10 CuO/Ce1-xMnxO2-Al2O3於富氫下CO選擇性氧化反應研究２７
3-11 CO2與H2O影響實驗２８
3-12 轉化率與選擇率之計算２８
3-13 使用藥品３１
第四章結果與討論３２
4-1 Ce1-xMnxO2、Ce1-xMnxO2-Al2O3擔體之製備與鑑定３２
4-1-1 ICP元素組成分析及BET比表面積測量３２
4-1-2 XRD結構分析３３
4-2擔體與觸媒表面性質分析３６
4-2-1氫程溫還原(TPR) ３６
4-2-2脈衝式CO吸附３７
4-2-3 觸媒XPS表面分析４０
4-2-4 擔體結構之拉曼(Raman)分析４３
4-3富氫中的CO選擇性氧化反應４５
4-3-1 7%CuO/Ce1-xMnxO2觸媒之CO選擇性氧化反應４５
4-3-2 CuO/Ce1-xMnxO2-x%Al2O3觸媒之CO選擇性氧化反應５０
4-3-2-(a) Mn引入量的影響５０
4-3-2-(b) Al2O3引入量的影響５３
4-3-2-(c) CuO負載量的影響５６
4-3-2-(d) F/W質流比的影響５９
4-3-2-(e) CO2與H2O的影響６２
4-3-2-(f) 200小時反應穩定性測試６５
結論６６
總結６７
參考文獻６８
圖目錄
圖2-1 CuO/CeO2 之結構示意圖１３
圖2-2 CuO與CeO2擔體行CO氧化協同作用模式１４
圖2-3 A possible structur of Ce0.5Zr0.5O2 １６
圖3-1 氫氣程溫還原裝置圖２２
圖3-2 脈衝式CO吸附裝置圖２５
圖3-3 CO選擇性氧化反應實驗裝置示意圖２９
圖3-4 CO2與H2O引入之實驗裝置示意圖３０
圖4-1 Ce1-xMnxO2擔體之X-ray繞射光譜圖３４
圖4-2 x%CuO/Ce0.9Mn0.1O2觸媒之X-ray繞射光譜圖３５
圖4-3 Ce1-xMnxO2擔體之H2-TPR圖譜３８
圖4-4 7%CuO/Ce1-xMnxO2觸媒之H2-TPR圖譜３９
圖4-5 7%CuO/Ce1-xMnxO2觸媒之XPS圖譜４１
圖4-6 7%CuO/Ce1-xMnxO2觸媒之Auger圖譜４２
圖4-7 Ce1-xMnxO2擔體之Raman譜圖４４
圖4-8(a) 7%CuO/Ce1-xMnxO2觸媒於CO選擇性氧化反應之轉化率４８
圖4-8(b) 7%CuO/Ce1-xMnxO2觸媒於CO選擇性氧化反應之選擇率４９
圖4-9(a) 7%CuO/Ce1-xMnxO2-20%Al2O3觸媒於CO選擇性氧化反應之轉化率５１
圖4-9(b) 7%CuO/Ce1-xMnxO2-20%Al2O3觸媒於CO選擇性氧化反應之選擇率５２
圖4-10(a) 7%CuO/Ce0.9Mn0.1O2-x%Al2O3觸媒於CO選擇性氧化反應之轉化率５４
圖4-10(b) 7%CuO/Ce0.9Mn0.1O2-x%Al2O3觸媒於CO選擇性氧化反應之選擇率５５
圖4-11(a) x%CuO/Ce0.9Mn0.1O2-20%Al2O3觸媒於CO選擇性氧化反應之轉化率５７
圖4-11(b) x%CuO/Ce0.9Mn0.1O2-20%Al2O3觸媒於CO選擇性氧化反應之選擇５８
圖4-12(a) 不同F/W對7%CuO/Ce0.9Mn0.1O2-20%Al2O3觸媒於CO選擇性氧化反應轉化率之影響６０
圖4-12(b) 不同F/W對7%CuO/Ce0.9Mn0.1O2-20%Al2O3觸媒於CO選擇性氧化反應選擇率之影響６１
圖4-13(a) CO2與H2O對7%CuO/Ce0.9Mn0.1O2-20%Al2O3觸媒於CO選擇性氧化反應轉化率之影響６３
圖4-13 (b) CO2與H2O對7%CuO/Ce0.9Mn0.1O2-20%Al2O3觸媒於CO選擇性氧化反應選擇率之影響６４
圖4-14 7%CuO/Ce0.9Mn0.1O2-20%Al2O3觸媒200 h穩定性測試之CO轉化率６５

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指導教授

陳吟足(Yin-Zu Chen)

審核日期

2008-7-17

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