博碩士論文 100324027 詳細資訊




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姓名 褚雅婷(Ya-ting Chu)  查詢紙本館藏   畢業系所 化學工程與材料工程學系
論文名稱 奈米金觸媒在對氯硝基苯氫化反應的研究
(noun)
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摘要(中) 奈米金觸媒於對-氯硝基苯氫化反應上有極佳的反應活性及選擇性。本研究中,首先探討奈米金擔載於不同擔體上在對-氯硝基苯氫化反應上活性的差異。再來比較金與不同金屬形成雙金屬擔載於二氧化鈦後,用於對-氯硝基苯氫化反應上活性的差異。最後比較不同比例之金鈀形成雙金屬擔載於二氧化鈦上,探討其在對-氯硝基苯氫化反應上活性的影響。不同擔體方面,以沉積沉澱法將金擔載於擔體上。而雙金屬觸媒部分,先以沉積沉澱法分別加入金與不同金屬,最後以硼氫化鈉還原之。製作不同金屬與不同比例之金鈀觸媒,探討最佳比例的反應觸媒。以X光繞射儀、穿透式電子顯微鏡、高解析度穿透式電子顯微鏡、X光能譜散佈分析儀、X光光電子能譜儀和程式升溫還原分析法等儀器鑑定觸媒之物理、化學特性和表面性質;利用液相選擇性對-氯硝基苯氫化反應來測試觸媒的活性與選擇性,反應條件設定為:反應器為半批式反應器(Parr Reactor 4842);反應溫度為373 K與室溫;壓力為1.1 MPa與0.55 MPa;攪拌速率300 rpm;反應溶劑為甲醇;反應時間180分鐘;反應起始之p-CNB濃度為0.2M (2.54 g p-CNB溶於80 ml甲醇);反應觸媒為0.5 g。結果顯示,不同擔體中以二氧化鈦反應活性最佳,雙金屬中則以加入鈀的觸媒反應活性與選擇性為最好,且加入少量的鈀,可以提升反應活性與選擇性。在金與鈀不同比例的觸媒比較中,相同反應條件下p-CNB轉化率都能在短時間內達到100%,甚至可降低反應環境條件,達到低壓且常溫下發生反應。根據鑑定結果分析,可看出加入鈀金屬之後可降低金觸媒的氧化態、增加反應活性基點且硼的氧化物可保護金顆粒避免氧化。因此,利用金觸媒的良好選擇性與鈀觸媒提高轉化率可使觸媒應用更將廣泛。
摘要(英) Nano-gold catalyst has been reported to have high activity and selectivity for liquid phase hydrogenation reaction. In this study, gold was loaded on different supports. The gold-containing bimetals were loaded on titanium-oxide. The catalyst was then optimize the molar ratio of Pd to Au on TiO2 for p-CNB hydrogenation reaction to have high activity.The monometallic Au catalysts were made by deposition-precipitation method. For bimetallic catalysts, gold and different metal solutions were added by the deposition-precipitation method, using NaBH4 to reduce them. Different metals and different molar ratios of Pd/Au were tested to find the high activity for p-CNB hydrogenation reaction. These catalysts were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy(XPS) and temperature programmed reduction (TPR). The catalytic properties of these catalysts were studied for hydrogenation of p-chloronitrobenzene (p-CNB). The conditions for hydrogenation reaction were 1.1 MPa and 0.55 MPa as H2 pressure, 373 K and room temperature as reaction temperature and 300 rpm stirring speed. Methanol was used as the solvent, the concentration of p-CNB was 0.2 M (2.54 g p-CNB in 80 ml methanol) and the amount of gold based catalyst was 0.5g. As results, titanium-oxide had a higher reaction activity than others, and adding palladium into gold base catalysts showed the high activity and selectivity. Comparing with different metals, adding palladium showed obviously a higher activity and selectivity. All of Pd/Au catalysts could reach 100% conversion of p-CNB on the same reaction conditions in short times. The reaction even It also could take place at room temperature and low hydrogen pressure. Only very small amount of palladium could improve the reaction activity and selectivity. According to the characteristics of the catalysts, adding palladium could reduce gold-valence state, increase reaction active sites. Therefore, gold and palladium catalysts could promote conversion and selectivity for hydrogenation reaction.
關鍵字(中) ★ 奈米金觸媒
★ 二氧化鈦
★ 液相氫化反應
★ 對氯硝基苯
關鍵字(英) ★ Nanoalloy gold catalyst
★ titanium-oxide
★ hydrogenation
★ chloronitrobenzene
論文目次 中文摘要…………………………………………………………………………….…I
Abstract………………………………………………………………………………..II
Table of Contents…………………………………………………………………….IV
List of Tables………………………………………………………………………VIII
List of Schemes……………………………………………………………………....IX
List of Figures………………………………………………………………………...X
Chapter 1 Introduction………………………………………………………………...1
Chapter 2 Literature Review…………………………………………………………..5
2.1 Nano-gold catalysts………………………………………………………..5
2.1.1 Reactions of gold catalysts……………………………………………5
2.1.2 Applications of gold catalysts………………………………………...6
2.2 Nanogold-containing bimetallic catalysts…………………………………7
2.2.1 Gold-containing bimetallic catalysts………………………………….7
2.2.2 Pd-Au bimetallic catalysts…………………………………………….7
2.2.3 Application of gold-based bimetallic catalysts………………………..8
2.3 Preparation of bimetallic catalysts………………………………………...9
2.3.1 Deposition precipitation method……………………………………...9
2.3.2 Impregnation method………………………………………………...11
2.3.3 Coprecipitation method……………………………………………...11
2.3.4 Chemical vapor deposition (CVD) method………………………….12
2.3.5 Photo-deposition method…………………………………………….12
2.4 Hydrogenation……………………………………………………………13
2.4.1 Liquid phase hydrogenation of p-CNB……………………………...14
2.4.2 Hydrogenation over gold catalysts…………………………………..18
Chapter 3 Experimental………………………………………………………………25
3.1 Chemicals………………………………………………………………...25
3.2 Preparation of catalysts…………………………………………………..25
3.2.1 Preparation of Au/X catalysts………………………………………25
3.2.2 Preparation of M-Au/TiO2 catalysts………………………………..25
3.2.3 Preparation of PdAu/TiO2 catalysts………………………………..26
3.3 The characterization of catalysts…………………………………………26
3.3.1 X-ray diffraction (XRD)……………………………………………27
3.3.2 Transmission electron microscopy (TEM)…………………………27
3.3.3 High resolution transmission electron microscopy & energy dispersive spectrometer (HRTEM & EDS)…………………………27
3.3.4 X-ray photoelectron spectroscopy (XPS)…………………………..28
3.3.5 Temperature-programmed reduction (TPR)………………………..28
3.4 Catalytic activity testing………………………………………………….29
Chapter 4 Hydrogen of p-chloronitrobenzene on Au catalysts: Effects of Support…………………………………………………………………….33
4.1 Introduction………………………………………………………………33
4.2 Results and discussion……………………………………………………33
4.2.1 XRD ………………………………………………………………...33
4.2.2 TEM………………………………………………………………….33
4.2.3 XPS…………………………………………………………………..34
4.2.4 Reaction Test………………………………………………………...35
4.2.5 Reaction rate constant……………………………………………….37
4.3 Conclusion……………………………………………………………….38
Chapter 5 Hydrogen of p-chloronitrobenzene on M-Au/TiO2 catalysts……………..50
5.1 Introduction………………………………………………………………50
5.2 Results and discussion……………………………………………………50
5.2.1 XRD………………………………………………………………..50
5.2.2 TEM………………………………………………………………...50
5.2.3 XPS…………………………………………………………………51
5.2.4 Reaction Test……………………………………………………….52
5.2.5 Reaction rate constant……………………………………………...54
5.3 Conclusion………………………………………………………………..55
Chapter 6 Hydrogen of p -chloronitrobenzene on Pd-Au/TiO2………………………69
6.1 Introduction………………………………………………………………69
6.2 Results and discussion……………………………………………………69
6.2.1 XRD………………………………………………………………..69
6.2.2 TEM………………………………………………………………...69
6.2.3 HRTEM…………………………………………………………….70
6.2.4 XPS…………………………………………………………………71
6.2.5 TPR…………………………………………………………………73
6.2.6 Reaction Test……………………………………………………….74
6.2.7 Reaction rate constant……………………………………………...76
6.3 Conclusion…………………………………………………………………77
Chapter 7 Summary…………………………………………………………………..98
7.1 Hydrogenation of p-chloronitrobenzene on Au/X catalysts………………99
7.2 Hydrogenation of p -chloronitrobenzene on M-Au/TiO2 catalysts………99
7.3 Hydrogenation of p -chloronitrobenzene on modified Pd-Au/TiO2……………………………………………………………..100
Appendix A Reaction rate constant…………………………………………………102
A.1 Au/X catalysts…………………………………………………………...103
A.2 M-Au/TiO2 catalysts……………………………………………………..105
A.3 Pd-Au/TiO2 catalysts…………………………………………………….107
Appendix B Mass transfer effect on liquid phase hydrogenation of p-chloronitrobenzene…………………………………………………109
B.1 Introduction…………………………………………………………..109
B.2 The mass transfer effect theory………………………………………..110
B.2.1The approach to evaluate gas-holdup effect……………………..110
B.2.2 The approach to evaluate the external mass transfer effect……112
B.2.3The approach to evaluate the intra-particle (pore diffusion) mass transfer effect………………………………………………….116
B.3 The estimations for the hydrogenation of p-CNB over the Au-based catalysts………………………………………………………………119
B.3.1The estimations for the hydrogenation of p-CNB over the Au/TiO2 catalyst under 373 K, 1.1 MPa and 0.2M p-CNB…119
B.3.2The estimations for the hydrogenation of p-CNB over the PdAu/TiO2 catalyst under 298 K, 0.55 MPa and 0.2 M p-CNB………………………………………………………...125
B.4 Conclusion…………………………………………………………...130
Appendix C Other catalysts test…………………………………………………….136
C.1 Pt/C catalysts for activity test…………………………………………136
C.2 NiMoB catalysts for DSC test…………………………….…………..137
C.3 La-NiMoB (0.2) catalysts for TGA test……………………………….138
C.4 PdAu/TiO2 (0.5:3) catalyst for activity test…………………………..138
Literature Cited……………………………………………………………………..139
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指導教授 陳郁文(Yu-wen Chen) 審核日期 2013-6-26
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