奈米金觸媒在富氫氣中選擇性一氧化碳氧化之應用

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陳書卉(Shu-Hui Chen) 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

奈米金觸媒在富氫氣中選擇性一氧化碳氧化之應用
(Selective Oxidation of CO in Hydrogen Stream over gold catalysts)

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摘要(中)

長久以來，金觸媒是一個很熱門的研究並且被廣泛的討論。即使在無數人的努力研究探討之下，金觸媒所擁有高活性的可能原因還是無法找出一個統一的解答，而且隨著實驗室的不同，也產生分歧的見解。一般而言，所有的見解皆研究探討認為擔體是影響金觸媒活性好壞的重要因素。本研究目標是找出高活性的金觸媒，可應用於在富氫氣流中選擇性一氧化碳氧化。我們利用初濕含浸法製備混合雙氧化物擔體，其擔體為二氧化錳-氧化鐵與二氧化鈰-二氧化鈦，並改變錳/鐵和鈰/鈦的莫耳比。混合擔體的莫耳比為1/9、2/8、3/7、4/6、5/5。金觸媒是藉由沉積沉澱法來加以製備，以四氯化氫金來當作金的前驅物，並以二氧化錳-氧化鐵與二氧化鈰-二氧化鈦視為擔體。金/二氧化鈰-二氧化鈦和金/二氧化錳-氧化鐵的酸鹼值分別為7和9，金觸媒乾燥溫度分別為80℃和110℃，煅燒溫度皆為180℃ 4小時，利用連續式反應器將金觸媒進行反應測試轉化率與選擇率，其反應溫度為25-100℃。金觸媒可以利用X光繞射分析儀(XRD)、穿透式電子顯微鏡(TEM)、氮-吸附(BET)、X光電子能譜儀(XPS)、感應耦合電漿質譜分析儀(ICP)等儀器來加以鑑定。
根據氮-吸附得知金/氧化鐵加入二氧化錳後，其BET surface area 和
Langmuir surface area 隨著增加的二氧化錳愈多表面積下降愈多，所以二氧化錳會導致面積下降。對於金/二氧化鈰-二氧化鈦(1:9)和金/二氧化錳-氧化鐵(3:7)在X光繞射分析儀鑑定中，並無發現任何金顆粒的結晶，其表示金顆粒非常小且小於4奈米。由穿透式電子顯微鏡可發現金觸媒金/二氧化鈰-二氧化鈦(1:9)
和金/二氧化錳-氧化鐵(3:7)金顆粒大小平均為2.5奈米。X光電子能譜儀可得知金/二氧化鈰-二氧化鈦(1:9)和金/二氧化錳-氧化鐵(3:7)金表面的氧化態有元素態金、正一價金、正三價的金，元素態金能夠吸附大部分的一氧化碳。感應耦合電漿質譜分析儀可測的擔體表面的金含量，但隨著金含量的增加而導致金顆粒的聚集。
金/二氧化鈰-二氧化鈦(1:9)和金/二氧化錳-氧化鐵(3:7)對於在富氫氣流中選擇性一氧化碳氧化有良好的結果，兩個金觸媒在室溫下進行選擇性一氧化碳氧化時，轉化率及選擇率皆很好。但是在高溫80℃-100℃下時，金/二氧化錳-氧化鐵(3:7)轉化率幾乎完全轉化，選擇率達到50%，顯然地，金/二氧化錳-氧化鐵(3:7)較金/二氧化鈰-二氧化鈦(1:9)穩定。所以，吾人認為金/二氧化錳-氧化鐵(3:7)對於在燃料電池富氫氣流中去移除一氧化碳有很大的幫助。

摘要(英)

Supported gold catalyst has been a subject of intense investigation. In spite of these efforts, there is still great uncertainty of the cause of the high activity and there is a wide variation in the activities reported among different laboratories. Superficially, all results suggest that the catalytic activity depends on the support. The aim of this study was to develop a method to prepare CeO2-TiO2 and MnO2-Fe2O3 to be used as supports by incipient-wetness ingeneration method. We change the molar ratio Ce/Ti and Mn/Fe to obtain different CeO2-TiO2 and MnO2-Fe2O3 supports. The molar Ce/Ti and Mn/Fe ratio was 1/1, 2/8, 3/7, 4/6, and 5/5. Used to HAuCl4 as the Au precursor to prepare Au/CeO2-TiO2 and Au/MnO2-Fe2O3 catalysts by deposition-precipitation. The gold catalysts Au/CeO2-TiO2 and Au/MnO2-Fe2O3 were maintained pH value 7 and 9. Au/CeO2-TiO2 and Au/MnO2-Fe2O3 were dried at 80℃ and 110 ℃ for overnight dividedly. The calcination temperature was at 180℃ for 4 h. The activity and selectivity of PROX was measured using a Pyrex fixed-bed continuous flow reactor at various temperatures (25

關鍵字(中)

★ 金觸媒
★ 二氧化錳
★ 氧化鐵
★ 一氧化碳
★ 二氧化鈰
★ 二氧化鈦

關鍵字(英)

★ TiO2
★ CeO2
★ carbon monoxide.
★ MnO2
★ Fe2O3
★ gold catalysts

論文目次

Chapter 1. Introduction………………………………………………………….. 01
Chapter 2. Literature Review…………………………………………………..... 03
2.1 Preparation method……………………………………………………….. 03
2.2 Active state of Au........................................................................................ 05
2.3 Au-support interaction................................................................................. 06
2.4 Applications in catalysis………………………………………………….. 06
2.4.1 CO oxidation………………………………………………………..... 06
2.4.2 VOC oxidation………………………………………………………... 06
2.4.3 water-gas shift reaction……………………………………………….. 07
2.4.4 Chemical processing………………………………………………….. 07
2.4.5 Epoxidation of propylene……………………………………………... 07
2.4.6 Electronics applications………………………………………………. 07
2.5 CO oxidation……………………………………………………………… 10
2.5.1 Particle size effect…………………………………………………… 10
2.5.2 Support effect………………………………………………………… 10
2.5.3 Promoter……………………………………………………………… 11
2.5.4 Reaction mechanism………………………………………………… 12
2.6 Selective CO oxidation in H2 stream……………………………………… 13
Chapter 3. Experimental………………………………………………………… 17
3.1 Chemical………………………………………………………………… 17
3.2 Catalyst preparation……………………………………………………… 17
3.2.1 Preparation of Iron oxide support…………………………………… 17
3.2.2 Preparation of MnO2-Fe2O3 support………………………………… 17
3.2.3 Preparation of CeO2-TiO2 support…………………………………… 21
3.2.4 Preparation of gold catalysts………………………………………...... 23
3.3. Characterization………………………………………………………… 27
3.3.1 N2-sorption…………………………………………………………… 27
3.3.2 X-ray diffraction……………………………………………………… 27
3.3.3 Transmission electron microscope…………………………………… 27
3.3.4 X-ray photoelectron spectroscope…………………………………… 28
3.3.5 Inductively coupled plasma mass spectrometry……………………… 28
3.4 Reaction testing…………………………………………………………… 28
3.4.1 Selective CO oxidation in H2 stream………………………………… 29
Chapter 4. Au/CeO2-TiO2 catalysts on selective CO oxidation………………….. 31
4.1 Introduction……………………………………………………………….. 31
4.2 Effect of preparation method……………………………………………… 35
4.3 Effect of Ce/Ti ratio……………………………………………………...... 54
4.4 Effect of gold loading……………………………………………………... 64
4.5 Summary…………………………………………………………………... 75
Chapter 5. Au/MnO2-Fe2O3catalysts on selective CO oxidation………………… 77
5.1 Introduction………………………………………………………………... 77
5.2 Effect of preparation method……………………………………………… 79
5.3 Effect of Mn/Fe ratio……………………………………………………… 82
5.4 Effect of gold loading……………………………………………………... 101
5.5 Effect of CO/O2 ratio……………………………………………………… 111
5.6 Effect of pH……………………………………………………………...... 111
5.7 Summary…………………………………………………………………... 116
Chapter 6. Conclusion……………………………………………………………. 118
Literature Cited…………………………………………………………………... 121

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指導教授

陳郁文(Yu-Wen Chen)

審核日期

2007-7-16

推文