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| DC 欄位 | 值 | 語言 |
|---|---|---|
| dc.contributor.advisor | 鄭淑芬(Soofin Cheng) | |
| dc.contributor.author | Chen-Yu Wu | en |
| dc.contributor.author | 吳鎮宇 | zh_TW |
| dc.date.accessioned | 2021-06-16T17:24:47Z | - |
| dc.date.available | 2012-08-17 | |
| dc.date.copyright | 2012-08-17 | |
| dc.date.issued | 2012 | |
| dc.date.submitted | 2012-08-16 | |
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| dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/63969 | - |
| dc.description.abstract | 質子交換膜燃料電池使用之燃料為氫氣，是具有高能量密度且低污染的能源。但在製備氫氣過程中殘餘0.25%~0.5%的一氧化碳會吸附在白金電極上造成電池效率降低。目前白金電極所能容忍的一氧化碳濃度約為10-100 ppm，現今最有效降低氫氣中之一氧化碳濃度的方法是使用觸媒在富氫環境下進行一氧化碳的選擇性氧化。
銅鈰氧化物對於一氧化碳之氧化具有高度轉化率以及選擇率，而介孔洞材料SBA-15具有高表面積、均勻六方角柱規則孔洞、良好的水熱穩定性之性質，使其成為極具潛力的觸媒載體。本論文利用含浸法將銅鈰氧化物負載在SBA-15介孔材料之孔道中，期望增加銅鈰氧化物之表面積，提升觸媒對一氧化碳的轉化率及選擇率。藉由改變不同的含浸順序、負載金屬比例、重量、煆燒溫度、以及不同的形態之二氧化矽載體以得到最佳化之觸媒。利用XRD、氮氣吸附儀、SEM、TEM、XANES以及H2-TPR 對觸媒進行分析。實驗的反應氣體組成成分為He : CO : O2 :H2 = 48.4 : 0.8 : 0.8 : 50，流速為每分鐘100毫升，並探討添加水氣與二氧化碳對觸媒活性的影響。由 XRD 與 TEM 發現金屬氧化物成功含浸至SBA-15 孔洞中，且形成分散性良好的小顆粒。由 TPR 發現形成較大的CeO2 顆粒有助於增加其與 CuO 顆粒的接觸介面，使得還原溫度降低。活性結果指出SBA-15載體經由900 oC煆燒處理去除表面 OH 基後，可提升其CO 轉化率及對水氣的容忍度，顯示表面的 OH 基對於反應有不利的影響。所合成之觸媒中，以0.1CuO-0.9CeO2/ 2SBA-15-p-900具有最高的活性，在140oC時可達到100 %的轉化率與70%選擇率。 | zh_TW |
| dc.description.abstract | Proton exchange membrane fuel cell (PEMFC) has been a powerful energy source due to several advantages such as high energy density, low emission of pollutants and low operation temperature. However, there are still some challenges needed to overcome. For example, the CO impurity in H2 fuel may poison the Pt electrode. During the hydrogen production by steam reforming and water-gas shift, there are still 0.25 %~0.5% CO in flowing gas, and the tolerance limit of Pt alloy anode for CO concentration is around 10-100 ppm. Therefore, it is necessary to eliminate 99% of the CO present in the H2 fuel, and the most effective way has been by preferential oxidation (PROX).
Copper and cerium mixed oxide has been found as a promising catalyst for PROX duo to its high conversion and relative cheap price. Mesoporous silica SBA-15 with uniform 2 D hexagonal arrays of pores and high surface area is a promising support to increase CuO/CeO2 surface area and dispersion. Various amounts of copper oxide were impregnated onto SBA-15.The catalysts were characterized by XRD, N2 sorption isotherm, SEM, TEM, XANES, TPR. The activities of the catalysts were tested in PROX reaction under 0.8 % CO, 0.8 % O2, 50 % H2, and 48.4 % He with a total flow rate of 100 mL/min. XRD patterns showed that copper oxide formed small particles and well dispersed when the mixed oxide was supported on SBA-15. TPR showed that the formation of large CeO2 can enhance the reducibility of catalyst, The reason may due to the particle size of cerium oxide in the high surface silica support is too small, and it would lower the interface of CuO contact with CeO2 .CuO-CeO2 supported on SBA-15 dehydrated at 900oC gave higher catalytic activity than that supported on 500oC calcined SBA-15, probably due to hydroxyl groups on the surface hinder the active site. The activities of the catalysts were significantly decreased in the presence of H2O, especially the silica supported catalysts. This negative effect may be attributed to the hydrophilic surfaces of silica. Among the supported catalysts, 0.1CuO-0.9CeO2/ 2SBA-15-p-900 catalyst could reach 100% CO conversion at 140oC with O2 selectivity around 70%. | en |
| dc.description.provenance | Made available in DSpace on 2021-06-16T17:24:47Z (GMT). No. of bitstreams: 1 ntu-101-R99223165-1.pdf: 3210538 bytes, checksum: 53d477893332e3847ee33ebad80626e3 (MD5) Previous issue date: 2012 | en |
| dc.description.tableofcontents | 目錄
中文摘要 ii ABSTRACT iii 目錄 iv 圖目錄 vi 表目錄 ix 第1章 緒論 1 1.1 質子交換膜燃料電池 1 1.2 氫氣製備 3 1.2.1 蒸氣重組 (Steam reforming) 3 1.2.2 水氣轉移反應 ( Water gas shift reaction, WGSR ) 4 1.2.3 移除氫氣中之微量一氧化碳 6 1.3 選擇性氧化 (Preferential Oxidation) 8 1.3.1 惰性金屬觸媒( Pt、Pd、Ru、Rh) 8 1.3.2 金觸媒 9 1.3.3 過渡金屬觸媒 10 1.4 介孔材料的簡介 13 1.5 研究目標 18 第2章 實驗部分 19 2.1 實驗藥品 19 2.2 觸媒之製備 20 2.2.1 銅鈰氧化物之製備 20 2.2.2 銅鈰氧化物負載於SBA-15 載體觸媒製備 20 2.3 鑑定觸媒材料的儀器 22 2.4 催化反應 26 2.5 產物鑑定 28 第3章 觸媒之鑑定 29 3.1 不同二氧化矽載體的比較 29 3.2 銅鈰氧化物觸媒負載於SBA-15 32 3.2.1 改變含浸溶劑 32 3.2.2 改變銅鈰氧化物的負載量 35 3.2.3 改變銅鈰氧化物的比例 37 3.2.4 改變銅與鈰的負載順序 40 3.2.5 改變煆燒溫度 41 3.2.6 改變二氧化矽載體 43 3.3 Cu K-edge X光吸收光譜 46 3.4 觸媒氧化還原性質 50 第4章 催化反應 56 4.1 觸媒製備對催化活性的影響 56 4.1.1 溶劑的影響 56 4.1.2 負載量的影響 58 4.1.3 負載比例的影響 60 4.1.4 負載順序的影響 62 4.1.5 煆燒溫度的影響 64 4.1.6 不同二氧化矽載體的影響 67 4.1.7 水氣與二氧化碳的影響 70 4.1.8 水氣對不同二氧化矽載體之觸媒的影響 72 第5章 結論 74 第6章 參考文獻 75 圖目錄 Fig. 1 1. The component of fuel cell 2 Fig. 1 2. Illustration of an ATR reactor [6] 4 Fig. 1 3. M4IS mesoporous structure (a) MCM-41，(b) MCM-48，(c)MCM-50[52]. 13 Fig. 1 4. A schematic description of the effect of Zr(IV) ions on the evolution of mesostructures and morphologies of SBA-15 materials [52]。 14 Fig. 1 5. Left: Powder XRD patterns of (A) calcined MCM-41 silica; (B) calcined MCM-41 after heating in boiling water for 6 hours; and (C) calcined SBA-15 after heating in boiling water for 24 hours. Right: SEM photos of as-synthesized hexagonal mesoporous silica SBA-15 [54]。 15 Fig. 1 6. (C) SEM image and (D, E) TEM images of calcined SBA-15 with platelet morphology and short mesochannels [57]。 16 Fig. 1 7. A schematic description of the effect of Zr(IV) ions on the evolution of mesostructures and morphologies of SBA-15 materials [57]。 17 Fig. 2 1. Powder X-ray diffraction. 22 Fig. 2 2. Equipment of BL17C X-ray absorption at NSRRC. 25 Fig. 2 3. Catalytic reaction system. 27 Fig. 2 4 The product distribution analyzed by GC 28 Fig. 3 1. Small angle XRD patterns (a) and N2 adsorption-desorption isotherms (b) of different silica supports. 30 Fig. 3 2. Solid state 29Si-NMR of different type silica supports. 30 Fig. 3 3. SEM images of SBA-15 and SBA-15-p. 31 Fig. 3 4. TEM images of SBA-15 and SBA-15-p. 32 Fig. 3 5. Small (a) and wide (b) angle XRD patterns of Cu and Ce oxide impregnated SBA-15 using different solvents (Ethanol、Water ) 0.1CuO-0.9CeO2/1SBA-15-p. 33 Fig. 3 6. N2 adsorption-desorption isotherms of Cu and Ce oxide impregnated SBA-15 using different solvents (Ethanol、Water ) 0.1CuO-0.9CeO2/1SBA-15-p. 34 Fig. 3 7. TEM images of Cu and Ce oxide impregnated SBA-15 using different solvents (Ethanol、Water ) 0.1CuO-0.9CeO2/1SBA-15-p. 35 Fig. 3 8. Small (a) and wide (b) angle XRD patterns of SBA-15-p impregnated with different amounts of metal oxide. 36 Fig. 3 9. N2 adsorption-desorption isotherms of SBA-15-p impregnated with different amounts of metal oxide. 37 Fig. 3 10. Small (a) and wide (b) angle XRD patterns of SBA-15-p impregnated with metal oxide of different Cu to Ce ratios. 38 Fig. 3 11. N2 adsorption-desorption isotherms of SBA-15-p impregnated with metal oxide of different Cu to Ce ratios. 39 Fig. 3 12. Small (a) and wide (b) angle XRD patterns of metal oxide impregnated SBA-15-p by different loading sequences. 40 Fig. 3 13. N2 adsorption-desorption isotherms of metal oxide impregnated SBA-15-p by different loading sequences. 41 Fig. 3 14. Small (a) and wide (b) angle XRD patterns of CuO and CeO2 impregnated SBA-15-p after calcination at different temperatures. 42 Fig. 3 15. N2 adsorption-desorption isotherms of CuO and CeO2 impregnated SBA-15-p after calcination at different temperatures. 43 Fig. 3 16. Small (a) and wide (b) angle XRD patterns of CuO and CeO2 impregnated onto different silica supports. 44 Fig. 3 17. N2 adsorption-desorption isotherms of different silica supports (a) and CuO and CeO2 impregnated onto different silica supports (b). 45 Fig. 3 18. Cu K-edge XANES spectra and EXAFS Fourier transform spectra in r-space of (a) Cu2O, (b) CuO, (c) 0.1CuO-0.9CeO2/3SBA-15-p, (d) 0.1CuO-0.9CeO2/2SBA-15-p, (e) 0.1CuO-0.9CeO2/1SBA-15-p 47 Fig. 3 19. Cu K-edge XANES spectra and EXAFS Fourier transform spectra in r-spacing of (a) Cu2O, (b) CuO, (c) 0.1CuO-0.9CeO2/2SBA-15-p-d500, (d) 0.1CuO-0.9CeO2/2SBA-15-p-d400, (e) 0.1CuO-0.9CeO2/2SBA-15-p-d300. 48 Fig. 3 20. Cu K-edge XANES spectra and EXAFS Fourier transform spectra in r-space of (a) Cu2O, (b) CuO, (c) 0.1CuO-0.9CeO2/2SBA-15-p, (d) 0.1CuO-0.9CeO2/2silica gel-made, (e) 0.1CuO-0.9CeO2/2silicagel. 49 Fig. 3 21. Cu K-edge XANES spectra and EXAFS Fourier transform spectra in r-space of (a) Cu2O, (b) CuO, (c) 0.1CuO-0.9CeO2/2SBA-15-p, (d) 0.9CeO2/0.1CuO/2 SBA-15-p, (e) 0.1CuO/0.9CeO2/2 SBA-15-p. 50 Fig. 3 22. H2-TPR profiles of 0.1CuO-0.9CeO2/1SBA-15-p catalysts with different 51 Fig. 3 23. H2-TPR profiles of 0.1CuO-0.9CeO2/XSBA-15-p catalysts with different loading amount. 51 Fig. 3 24. H2-TPR profiles of 0.1CuO-0.9CeO2/2SBA-15-p-dT catalysts after calcination at different temperatures. 52 Fig. 3 25. H2-TPR profiles of 0.1CuO-0.9CeO2/2supports catalysts with different supports. 53 Fig. 3 26. H2-TPR profiles of CuO and CeO2 catalysts with different supports 55 Fig. 4 1. CO conversion, selectivity and O2 conversion over 0.1CuO-0.9CeO2/1SBA-15-p prepared using different solvents. 57 Fig. 4 2. CO conversion, selectivity and O2 conversion over SBA-15-p loaded with different amounts of CuO and CeO2 oxide. 59 Fig. 4 3. CO conversion, selectivity and O2 conversion over SBA-15-p loaded with CuO and CeO2 oxide of different CuO/CeO2 ratio. 61 Fig. 4 4. CO conversion, selectivity and O2 conversion over SBA-15-p impregnated CuO and CeO2 with different loading sequences. 64 Fig. 4 5. CO conversion, selectivity and O2 conversion of 0.1CuO-0.9CeO2/2SBA-15-dT catalyst calcined at different temperatures. 66 Fig. 4 6. IR spectra of 0.1CuO-0.9CeO2/2SBA-15-dT catalysts calcined at different temperatures 66 Fig. 4 7. CO conversion, selectivity and O2 conversion of 0.1CuO-0.9CeO2 impregnated onto different silica supports. 69 Fig. 4 8. CO conversion, selectivity and O2 conversion of 0.1CuO-0.9CeO2/2SBA-15-p-900 in the presence of 15% CO2 and 10% H2O in the reaction feed. 71 Fig. 4 9. CO conversion, selectivity and O2 conversion over different catalysts in the presence of 10 % H2O 73 表目錄 Table 1 1. Comparison of the catalytic performance for the selective CO methanation reported in the literature [13] 7 Table 1 2. Definition of pore size and examples of mesoporous materials[51]. 13 Table 2 1. Temperature program for product analysis. 28 Table 3 1. Textural properties of Silica supports. 31 Table 3 2. Textural properties of Cu and Ce oxide impregnated SBA-15 using different solvents (Ethanol、Water ) 0.1CuO-0.9CeO2/1SBA-15-p. 34 Table 3 3. Textural properties of SBA-15-p impregnated with different amounts of metal oxide. 37 Table 3 4. Textural properties of SBA-15-p impregnated with metal oxide of different Cu to Ce ratios. 39 Table 3 5. Textural properties of metal oxide impregnated SBA-15-p by different loading sequences. 41 Table 3 6. Textural properties of CuO and CeO2 impregnated SBA-15-p after calcination at different temperatures. 43 Table 3 7. Textural properties of CuO and CeO2 impregnated onto different silica supports. 46 Table 3 8. H2-TPD analysis of various samples. 54 Table 4 1. Catalytic Performance of 0.1CuO-0.9CeO2/1SBA-15-p prepared using different solvents 58 Table 4 2. Catalytic Performance of SBA-15-p loaded with different amounts of CuO and CeO2 oxide. 60 Table 4 3. Catalytic Performance of SBA-15-p loaded with CuO and CeO2 oxide of different CuO/CeO2 ratio 62 Table 4 4. Catalytic Performance of SBA-15-p impregnated CuO and CeO2 with different loading sequences. 64 Table 4 5. Catalytic Performance of 0.1CuO-0.9CeO2/2SBA-15-dT calcined at different temperatures 67 Table 4 6. Catalytic Performance of 0.1CuO-0.9CeO2 impregnated onto different silica supports. 69 Table 4 7. Catalytic performance of 0.1CuO-0.9CeO2/2SBA-15 in the presence of 10% H2O and 15% CO2 in the reaction feed. 71 | |
| dc.language.iso | zh-TW | |
| dc.subject | 銅鈰氧化物 | zh_TW |
| dc.subject | 選擇性氧化 | zh_TW |
| dc.subject | 質子交換膜燃料電池 | zh_TW |
| dc.subject | SBA-15 | zh_TW |
| dc.subject | PEMFC | en |
| dc.subject | SBA-15 | en |
| dc.subject | PROX | en |
| dc.subject | CeO2 | en |
| dc.subject | CuO | en |
| dc.title | 銅鈰氧化物負載在SBA-15介孔材料中及其在富氫氣氛中對一氧化碳的選擇性氧化 | zh_TW |
| dc.title | CuO/CeO2 supported on SBA-15 for Preferential Oxidation of CO in Hydrogen Rich Environment | en |
| dc.type | Thesis | |
| dc.date.schoolyear | 100-2 | |
| dc.description.degree | 碩士 | |
| dc.contributor.oralexamcommittee | 萬本儒(Ben-Zu Wan),簡淑華(Shu-Hua Chien) | |
| dc.subject.keyword | 銅鈰氧化物,選擇性氧化,質子交換膜燃料電池,SBA-15, | zh_TW |
| dc.subject.keyword | PROX,PEMFC,CuO,CeO2,SBA-15, | en |
| dc.relation.page | 77 | |
| dc.rights.note | 有償授權 | |
| dc.date.accepted | 2012-08-16 | |
| dc.contributor.author-college | 理學院 | zh_TW |
| dc.contributor.author-dept | 化學研究所 | zh_TW |
| 顯示於系所單位： | 化學系 | |
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| ntu-101-1.pdf 未授權公開取用 | 3.14 MB | Adobe PDF |
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