博碩士論文 90324029 詳細資訊




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姓名 伍家慶(Cha-Chin Wu)  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 汽機車尾氣在富氧條件下NOx之去除
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摘要(中) 近年來,又愈來愈多有關汽機車尾氣在富氧條件下之NOx去除的研究,因為富氧的條件下去除汽機車尾氣可以節省油料的消耗。NOx 在富氧的條件下被觸媒所吸附儲存;而在缺氧的條件之下, 被儲存的NOx 會被還原成無害的N2。本研究利用濕式含浸法與反應沉澱法合成去除NOx的觸媒。在觸媒中加入可以作為吸附用的鹼土族(Ba,Sr)以作為吸附NOx之成分。另外再加入Ce與La作為提供氧氣儲存的成分。在鑑定樣品的物理性質上,藉掃描式電子顯微鏡與穿透式電子顯微鏡觀察顆粒大小;由氮吸附、脫附分析測定表面積;另外,對觸媒進行循環測試(cycle test),測試其吸附能力與反應性,並探討溫度對觸媒吸附力的影響與研究觸媒的吸附耐力測試。由實驗結果得知,利用反應沉澱法合成去除NOx的觸媒,雖然有極相同的成果,但由於反應沉澱法較為費時,而濕式含浸法在合成上較為簡便,故我們選用濕式含浸法。由一系列的濕式含浸法所得的觸媒比較,含有Ce的觸媒有較高的NO吸附能力;從實驗所得的圖形,可以知道被吸附的NO是由丙烯(C3H6)所還原而得氮氣。另外,比較Ce與La的效果,可以得知在反應一開始時,Ce的效果遠比La佳,因為La在一開始時吸附效果為零。但做耐力測試的結果,Ce與La有極相同的成果。由循環測試及耐力測試的結果作探討比較,我們得到最好的觸媒是利用濕式含浸法所配製的Pt2.5Ce30.5Ba33.4Al100 與 Pt2.5Ce22.5Ba41.7Al100,其中下標數字代表重量比。我們把濕式含浸法的觸媒做描式電子顯微鏡與穿透式電子顯微鏡分析,發現其顆粒為不規則與不均勻的聚集,顆粒大小約0.1μm到5.0μm,且為不規則的形狀,而且分散度不佳。
摘要(英) The performance and durability of NOx storage catalyst were studied. The catalysts were used to reduce nitrogen oxides from lean-burn condition. There are increasing interests in car engines in the lean-burn condition to improve fuel economy. In the catalysts, NOx emitted from an engine at lean A/F operation was stored and this stored NOx was reduced at rich-burn operation. The incipient-wetness impregnation and precipitation methods were used to synthesize the catalysts. The properties of the catalysts were characterized by scanning electron microscopy, transmission electron microscopy, N2 sorption. The catalysts were tested by the lean-rich cycle. The effects of reaction temperature for storage capacity and duration were also tested. To investigate the storage capability of the catalyst, the samples were prepared with different alkaline-earth metal additives and different rare-earth metal oxides. Comparing the effects of preparation methods between incipient-wetness impregnation and precipitation, both samples had similar storage capability, but the incipient-wetness impregnation was more convenient to synthesize the samples. Therefore, this method was used in this study. The transient experiments comprise a storing phase using a lean NO/O2/N2/C3H6/CO gas mixture, and a regeneration phase where the O2 flow was switched off. The De-NOx catalysts consisted of nonuniform aggregates of very small and distinct particles. The catalysts containing barium had better storage capability and duration. On the other hand, the catalyst containing cerium had a higher NO storage capability than that having no cerium.
關鍵字(中) ★ 還原
★ 循環測試
★ 缺氧條件
★ 富氧條件
★ NOx儲存觸媒
★ 再生
關鍵字(英) ★ cycle test
★ rich-burn condition
★ lean-burn condition
★ storage catalyst
★ NOx
論文目次 Table of Contents
Page
Abstract………………………………………………………………...…i
Table of Contents…………………………………………………...……....iii
List of Tables………………………………………………………………vii
List of Figures……………………………………………………….…viii
CHAPTER 1. INTRODUCTION………………………………………...1
1.1 Carbon monoxide (CO)…………………………...2
1.2 Nitrogen oxide (NOx)………………………..……….…………........2
1.3 Hydrocarbons………...…………………………………………........3
1.4 Heavy metal.........................................................................................5
1.4-1 Lead (Pb)………………………………………………………...5
1.5 Objective and Scope………………………………………………….6
CHAPTER 2. LITERATURE REVIEW……………………………….8
2.1 Process for the Operation of NOx Storage Catalysts………...…..........9
2.1-1 Lean/Rich Cycle…………………………………………..……...9
2.1-2 Influence of Inlet Gas Compositions……………………….......13
2.1-3 Influence of Temperature……………………………………….15
2.1-4 Break-Through Peaks…………………………………………...15
2.1-5 Removal of NOx from the Exhaust of a Lean–Burn Engine........17
2.2 Characteristics of the De-NOx Catalysts…………………………….19
2.2-1 Alumina (Al2O3)………………………………………………...21
2.2-2 Effects of Additives on γ-Alumina……………………………...22
2.2-3 Effects of Cerium Additives…………………………………….22
2.2-4 Effects of Lanthanum Additive……………………………........23
2.2-5 Effects of Alkaline-Earth Metals Additives…………………….25
2.2-6 Effects of Platinum Additive………………………………........28
2.3 Synthesis Procedure of De-NOx catalysts…………………………….28
2.3-1 Precipitation Methods………………………………………........30
2.3-2 Incipient-Wetness Impregnation Method………………………...30
2.3-3 Coating on a Ceramic Honeycomb…………………………........31
CHAPTER 3. EXPERIMENTAL…………………………………………..33
3.1 Chemicals………………………………….……………………..33
3.2 Synthesis Procedure………..……………….…………………….33
3.2-1 Synthesis with Incipient-Wetness Impregnation Method………33
3.2-2 Synthesis with Precipitation Method…………………………...34
3.3 Characterization………………………………………………….38
3.3.1 N2 adsorption-desorption isotherms………………………........38
3.3.2 Scanning electron microcopy (SEM)……………………….38
3.3.3 Transmission electron microscopy (TEM)…………………….38
3.3.4 Catalytic activity measurement………………………………...39
CHAPTER 4. Results and Discussion………………………….…….…….46
4.1 Morphology (SEM and TEM)………………….…………………...46
4.1-1 SEM……..………………………………………………….......46
4.1-2 TEM…………………………………………………………….52
4.2 BET Surface Area………………………………………...…………57
4.3 Catalytic activity measurements…………………………………….59
4.3-1 Pt2.5Ce30.5Ba33.4Al100 and Pt2.5Ce22.5Ba41.7Al100………………….59
4.3-2 Pt2.5Ce30.5Sr33.4Al100 and Pt2.5Ce22.5Sr41.7Al100…………….…….61
4.3-3 Pt2.5La30.5Ba33.4Al100 and Pt2.5La22.5Ba41.7Al100………………….62
4.3-4 Pt2.5La30.5Sr33.4Al100 and Pt2.5La22.5Sr41.7Al100……………….......62
4.3-5 Comparing the Storage Capacity of Strontium (Sr) and Barium (Ba)………………………………………………………………..64
4.3-6 Effects of Cerium Additives…………………………………….64
4.3-7 Comparing the Effects of Cerium and Lanthanum Additives…..65
4.3-8 The Precipitation Methods……………………………………………..66
4.3-9 The relationship between barium content and NOx storage…….65
CHAPTER 5. CONCLUSION …………………………………………….87
REFERENCE………………………………….………………………..88
Appendix: Synthesis and Characterization of Nano-Sized Zeolites……….93
摘要…………….…………………………………………………………..94
Abstract…………………………………………………………………….95
CHAPTER 1. INTRODUCTION………………………………………….96
1.1 Synthesis and Characteristics of Zeolites……..………...…………...96
1.2 Objective and Scope………………………..……………..................97
CHAPTER 2. LITERATURE REVIEW………….………………………..98
2.1 Applications of Nano-Sized Zeolites…………….…………………..98
2.2 The Formation Mechanism of Zeolites…………….………………..99
2.3 Synthesis and Characteristics of Nano-Sized Zeolites…….……….100
CHAPTER 3. EXPERIMENT…………………………………………....110
3.1 Chemical…………………………………………………………...110
3.2 Synthesis Method…………………………………………………..110
3.2-1 Synthesis of Silicate-1…………………………………………110
3.3 Characterization…………………………………………………….114
3.3-1 X-ray diffraction (XRD)………………………………………114
3.3-2 N2 sorption…………………………………………………….114
3.3-3 Scanning electro microscopy (SEM)………………………….114
3.3-4 Transmission electron microscopy (TEM)…………………….115
Chapter 4. RESULTS AND DISCUSSION………………………………116
4.1 Effects of Synthesis Temperature………………………………..116
4.1-1 Effects of the Synthesis Temperature on Silicalite-1………….116
4.1-2 Effects of the Synthesis Temperature on ZSM-5……………..121
4.2 Effects of Templates………………..………………………........125
4.3 Effects of Synthesis Time and SiO2/Al2O3Ratio………………...129
4.3-1 Effects of Synthesis Time………………………………………..129
4.3-2 Effects of SiO2/Al2O3 Ratio………………..…………………….136
Chapter 5. CONCLUSION……………………………………………….140
REFERENCE……………………………………………………………..141
List of Tables
Table 1-1 Volatile organic emissions of an Otto engine (Dulson, 1981)…….4
Table 2-1 Gas compositions in the different experiments (Fridell et al., 1998)………………….………………………………………..14
Table 3-1 De-NOx catalysts prepared by various additives and different synthesis procedure...………………………………………........37
Table 3-2 The inlet gas compositions…………………………………........45
Table 4-1 BET specific surface areas (SBET) of De-NOx catalysts..……….58
Table 4-2 The NO storage amounts of Pt2.5Ce30.5Ba33.4Al100 and Pt2.5Ce22.5Ba41.7Al100 for cycle test……………………………….67
Table 4-3 The NO storage amounts of Pt2.5Ce30.5Sr33.4Al100 and Pt2.5Ce22.5Sr41.7Al100 for cycle test………………………………..71
Table 4-4 The NO storage amounts of Pt2.5La30.5Ba33.4Al100 and Pt2.5La22.5Ba41.7Al100 for cycle test……………………………...75
Table 4-5 The NO storage amounts of Pt2.5La30.5Sr33.4Al100 and
Pt2.5La22.5Sr41.7Al100 for cycle test………………………………..79
Appendix: Synthesis and Characterization of Nano-Sized Zeolites
Table 3-1. The samples prepared by various conditions………………….111
Table 4-1. The physical properties of silicalite-1 prepared with various synthesis times…………………………………………….....135
List of Figures
Figure 2-1. NOx storage reduction mechanism (Matsumoto, 1996)….........10
Figure 2-2. The NO and NO2 concentration traces during a transient with the
gas compositions quoted in Table 2-1 over a Pt-Rh/BaO/Al2O3
catalyst. The dashed vertical lines mark the switches in gas
composition where the rich phase is indicated by the double arrow (Fridell et al., 1998)…….................................................12
Figure 2-3.1The NOx storage vs. inlet gas temperature with either NO or NO2 in the feed (Fridell et al., 1998)………………………….16
Figure 2-4. Figure 2-4 proposed by Hohne et al. (2001) is a graph which schematically represents the time dependence of nitrogen oxide sorption and desorption when the storage catalyst is operated according to the process of the invention……..........................18
Figure 2-5.1A / F window with three-way catalysts .
(Koberstein and Wannemacher, 1987)………………………..20
Figure 2-6.1The graph shows a relationship between cerium content and NOx removal rate on a catalyst (Iizuka et al., 2000)…..….......24
Figure 2-7.1The graph shows a relationship between strontium content and NOx removal rate of a catalyst (Iizuka et al., 2000)…………..27
Figure 2-8.1The graph shows a relationship between platinum content and NOx removal rate on a catalyst (Iizuka et al., 2000).................29
Figure 2-9. A graph of a honeycomb support (Suzuki et al., 1998)………..32
Figure 3-1. De-NOx catalysts prepared by incipient-wetness impregnation method………………………………………………………...35
Figure 3-2.1De-NOx catalysts prepared by precipitation method…….........36
Figure 3-3.1Micromeritics ASAP 2000……………………………….........41
Figure 3-4.1The schematic diagram of the De-NOx reaction apparatus…...42
Figure 3-5.1The diagram of the De-NOx reactor…………………………..43
Figure 3-6 The inlet O2 content for cycle test……………………………...44
Figure 4-1. SEM micrographs of (A)Pt2.5Ce30.5Ba33.4Al100 and (B) Pt2.5Ce22.5Ba41.7Al100………………………………………….47
Figure 4-2. SEM micrographs of (A)Pt2.5Ce30.5Sr33.4Al100 and (B)
Pt2.5Ce22.5Sr41.7Al100………………………………....................48
Figure 4-3. SEM micrographs of (A) Pt2.5La30.5Ba33.4Al100 and (B) Pt2.5La22.5Ba41.7Al100………………………………………….49
Figure 4-4. SEM micrographs of (A) Pt2.5La30.5Sr33.4Al10 and (B) Pt2.5La22.5Sr41.7Al100………..……………………………........50
Figure 4-5. Shematic showing extremes of micro-macropore distribution (Nortier and Soustelle, 1987)…………..................................51
Figure 4-6. TEM micrographs of (A) Pt2.5Ce30.5Ba33.4Al100 and (B) Pt2.5Ce22.5Ba41.7Al100………………….………………………53
Figure 4-7. TEM micrographs of (A) Pt2.5Ce30.5Sr33.4Al100 and (B) Pt2.5Ce22.5Sr41.7Al100…………………………………………..54
Figure 4-8. TEM micrographs of (A) Pt2.5La30.5Ba33.4Al100 and (B) Pt2.5La22.5Ba41.7Al100………………………………..………...55
Figure 4-9. TEM micrographs of (A) Pt2.5La30.5Sr33.4Al100 and (B) Pt2.5La22.5Sr41.7Al100…………………………………………..56
Figure 4-10. NO storage and conversion of (A) Pt2.5Ce30.5Ba33.4Al100 and (B) Pt2.5Ce22.5Ba41.7Al100 for cycle test in 400℃…………………..68
Figure 4-11. The NO storage vs. reaction temperatures of (A) Pt2.5Ce30.5Ba33.4Al100 and (B) Pt2.5Ce22.5Ba41.7Al100……..........69
Figure 4-12. NO storage and conversion for duration of 30 min of (A) Pt2.5Ce30.5Ba33.4Al100 and (B) Pt2.5Ce22.5Ba41.7Al100…….…….70
Figure 4-13. NO storage and conversion of (A) Pt2.5Ce30.5Sr33.4Al100 and (B) Pt2.5Ce22.5Sr41.7Al100 for cycle test in 400℃………………….72
Figure 4-14. The NO storage vs. reaction temperatures of (A) Pt2.5Ce30.5Sr33.4Al100 and (B) Pt2.5Ce22.5Sr41.7Al100………........73
Figure 4-15. NO storage and conversion for duration of 30 min of (A) Pt2.5Ce30.5Sr33.4Al100 and (B) Pt2.5Ce22.5Sr41.7Al100………........74
Figure 4-16. NO storage and conversion of (A) Pt2.5La30.5Ba33.4Al100 and (B) Pt2.5La22.5Ba41.7Al100 for cycle test in 400℃…………………76
Figure 4-17. The NO storage vs. reaction temperatures of (A) Pt2.5La30.5Ba33.4Al100 and (B) Pt2.5La22.5Ba41.7Al100…………..77
Figure 4-18. NO storage and conversion for duration of 30 min of (A) Pt2.5La30.5Ba33.4Al100 and (B) Pt2.5La22.5Ba41.7Al100……………78
Figure 4-19. NO storage and conversion of (A) Pt2.5La30.5Sr33.4Al100 and (B) Pt2.5La22.5Sr41.7Al100 for cycle test in 400℃…………………..80
Figure 4-20. The NO storage vs. reaction temperatures of (A) Pt2.5La30.5Sr33.4Al100 and (B) Pt2.5La22.5Sr41.7Al100……………81
Figure 4-21. NO storage and conversion for duration of 30 min of (A) Pt2.5La30.5Sr33.4Al100 and (B) Pt2.5La22.5Sr41.7Al100……………..82
Figure 4-22. NO storage for duration of 30 min of Pt2.5Ce30.5Sr33.4Al100 (-●-) and Pt2.5Ce30.5Ba33.4Al100 (--○--)…………………………..83
Figure 4-23. NO storage for duration of 30 min of Pt2.5Ce30.5Sr33.4Al100 (-●-) and Pt2.5Ba33.4Al100 (--○--)……………………..................83
Figure 4-24. NO storage for duration of 30 min of Pt2.5Ce30.5Ba33.4Al100 (-●-) and Pt2.5La30.5Ba33.4Al100 (--○--)…………………………84
Figure 4-25. NO storage and conversion for duration of 30 min of (A) Pt2.5Ti24K30Al100(R) and (B) Pt2.5Ti24Ba32Al100(R)…………...85
Figure 4-26 The relationship between barium content and NOx storage (%)…………………………………………………………….86
Appendix: Synthesis and Characterization of Nano-Sized Zeolites
Figure 2-1. XRD pattern of ZSM-5 synthesized after van Grieken (2000); crystallization time: 2 days (Reding et al., 2003)……………102
Figure 2-2. SEM image of ZSM-5 synthesized after van Grieken (2000); crystallization time: 2 days (Reding et al., 2003)………........102
Figure 2-3. XRD spectra of as-synthesized samples obtained at different reaction time. (a) t = 6 h, (b) t = 12 h, (c) t = 18 h, (d) t = 20 h, (e) t = 22 h, (f) t = 24 h, (g) t = 48 h, (h) t = 72 h, (i) t = 96 h, (j) t = 108 h and (k) t = 120 h (van Grieken et al., 2000)…………………………………………………….…..103
Figure 2-4. (a) Nitrogen adsorption-desorption isotherms at 77 K of calcined samples obtained at different synthesis time and (b) their corresponding pore size distribution (van Grieken et al., 2000)…………………………………………………………106
Figure 2-5. Preparation protocol for colloidal suspensions of template removal zeolite nanocrystals (Wang et al., 2000)……….…...107
Figure 2-6. SEM images of silicalite nanocrystals prepared without polymer network barrier: (a) after drying, (b) after calcinations (Wang et al., 2000)……………………………………………………..109
Figure 2-7. Confined space synthesis. The zeolite is crystallized within the pore system of mesoporous carbon matrix. The crystal size L1, is always smaller than the pore diameter, L2 (Jacobsen et al., 2000)…………………………………………………………109
Figure 3-1. The preparation method of ZSM-5…………………………...112
Figure 3-2. The preparation method of silicalite-1………………………..113
Figure 4-1. The XRD patterns of silicalite-1 prepared at various synthesis temperatures. (A) 80TMAS-2; reacted at 80℃; (B) 120TMAS-2; reacted at 120℃; (C) 170TMAS-2; reacted at 170℃……….118
Figure 4-2. SEM images of silicalite-1 prepared at various synthesis temperatures. (A) 80TMAS-2; reacted at 80℃; (B) 120TMAS-2; reacted at 120℃; (C) 170TMAS-2; reacted at 170℃……….119
Figure 4-3. TEM images of silicalite-1 prepared at various synthesis temperatures. (A) 80TMAS-2; reacted at 80℃; (B) 120TMAS-2; reacted at 120℃; (C) 170TMAS-2; reacted at 170℃……….120
Figure 4-4. The XRD patterns of ZSM-5 prepared at various synthesis temperatures. (A) 80TMAR60-2; reacted at 80℃; (B) 120TMAR60-2; reacted at 120℃; (C) 170TMAR60-2; reacted at 170℃……………………………………………………...122
Figure 4-5. SEM images of ZSM-5 prepared at various synthesis temperatures. (A) 80TMAR60-2; reacted at 80℃; (B) 120TMAR60-2; reacted at 120℃; (C) 170TMAR60-2; reacted at 170℃……………………………………………………...123
Figure 4-6. TEM images of ZSM-5 prepared at various reaction temperatures. (A) 80TMAR60-2; reacted at 80℃; (B) 120TMAR60-2; reacted at 120℃; (C) 170TMAR60-2; reacted at 170℃……………………………………………………...124
Figure 4-7. The XRD patterns of ZSM-5 prepared with different
templates. (A) 170TMAS-2; prepared with TMA;
(B) 170TPAS-2; prepared with TPA…………………………127
Figure 4-8. SEM images of ZSM-5 prepared with different templates. (A) 170TMAS-2; prepared with TMA; (B) 170TPAS-2; prepared with TPA……………………………………………………..128
Figure 4-9. The XRD patterns of silicalite-1 prepared at various synthesis times. (A) 170TPAS-1; synthesized for 1 d; (B) 170TPAS-2; synthesized for 2 d; (C) 170TPAS-3; synthesized for 3 d; (D) 170TPAS-4; synthesized for 4 d……………………………..131
Figure 4-10. SEM images of silicalite-1 prepared with various synthesis times. (A) 170TPAS-1; synthesized for 1 d; (B) 170TPAS-2; synthesized for 2 d; (C)170TPAS-3; synthesized for 3 d; (D)170TPAS-4; synthesized for 4 d……………………........132
Figure 4-11. TEM images of silicalite-1 prepared with various synthesis times. (A) 170TPAS-1; synthesized for 1 d; (B) 170TPAS-2; synthesized for 2 d; (C)170TPAS-3; synthesized for 3 d; (D)170TPAS-4; synthesized for 4 d…………………………133
Figure 4-12. The N2 sorption of silicalite-1 prepared with various synthesis
times. (A) 170TPAS-1; synthesized for 1 d; (B) 170TPAS-2;
synthesized for 2 d; (C)170TPAS-3; synthesized for 3 d; (D)170TPAS-4; synthesized for 4 d. The isotherms are offset vertically by 100 cm3/g, STP for clarity…………………….134
Figure 4-13. The XRD patterns of the samples synthesized with various SiO2/Al2O3 molar ratios. (A) 170TPAS-2; synthesized in the absence of aluminum; (B) 170TPAR60-2; SiO2/Al2O3 ratio of 60; (C) 170TPAR-30; SiO2/Al2O3 ratio of 30…………….....137
Figure 4-14. SEM images of the samples synthesized with various
SiO2/Al2O3 molar ratios. (A) 170TPAS-2; synthesized in the
absence of aluminum; (B) 170TPAR60-2; SiO2/Al2O3 ratio of
60; (C) 170TPAR-30; SiO2/Al2O3 ratio of 30…………….....138
Figure 4-15. TEM images of the samples synthesized with various
SiO2/Al2O3molar ratios. (A) 170TPAS-2; synthesized in the
absence of aluminum; (B) 170TPAR60-2; SiO2/Al2O3 ratio of
60; (C) 170TPAR-30; SiO2/Al2O3 ratio of 30…………….....139
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指導教授 陳郁文(Yu-Wen Chen) 審核日期 2003-6-30
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