博碩士論文 93324034 詳細資訊



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姓名 陳世文(Shr-Wen Chen)  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 奈米非晶態CoNiB雙金屬觸媒的製備與氫化探討
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摘要(中) 本研究採化學還原法製備CoNiB觸媒，並引入水溶性高分子PVP，製備PVP-CoNiB觸媒。藉液相丁醛氫化模式反應有系統探討CoNiB及PVP-CoNiB觸媒製備變因，以ICP、BET、TEM、XRD、DSC、XPS瞭解其物理性質，藉糠醛(含呋喃環外羰基及環內烯基鍵)、巴豆醛(含共軛烯基-羰基鍵)及檸檬醛(含共軛烯基-羰基鍵及一孤立烯基鍵)的選擇性氫化反應瞭解雙金屬觸媒之催化特性，並與活性及選擇性都優於倫尼金屬之NiB與CoB觸媒比較。
CoNiB與PVP-CoNiB觸媒最佳製備條件為以醋酸鹽類為前驅鹽，金屬莫耳比例Co/Ni = 5/5，硼氫化鈉水溶液進料速率2.6 ml/min，水溶性高分子PVP添加莫耳比例為PVP/Metal = 2~5 。
CoNiB雙金屬觸媒粒徑及粒徑分佈(3.8~5.6 nm)都比NiB(15~50 nm)及CoB(5.5~9.4 nm)觸媒小，添加PVP高分子穩定劑能讓PVP-CoNiB觸媒的粒徑更小更均一。CoNiB雙金屬觸媒整體組成中金屬對硼之元素比值，與NiB及CoB單金屬觸媒比值相近，引入高分子PVP並不影響PVP-CoNiB組成中金屬對硼之元素比值。CoNiB與PVP-CoNiB雙金屬觸媒組成分佈均勻，表面Co/Ni比例與整體組成相近。觸媒經不同溫度熱處理之XRD分析與DSC晶化分析發現，CoNiB並非為CoB與NiB的物理混合物。CoNiB、PVP-CoNiB皆為非晶態觸媒，PVP-CoNiB觸媒熱穩定性最佳，CoNiB觸媒與CoB觸媒次之，NiB觸媒最差。
以最佳比例之CoNiB(5/5)觸媒於丁醛、巴豆醛、糠醛及檸檬醛等液相氫化反應，活性皆優於NiB、CoB觸媒，且引入高分子PVP，以莫耳比PVP/Me = 2~5即達保護觸媒效果，避免顆粒聚集成長，製
得顆粒更小更均一的PVP-CoNiB觸媒，活性優於CoNiB觸媒。
丁醛與糠醛氫化反應，皆屬單一官能基C=O鍵的氫化。CoNiB觸媒活性為NiB及CoB觸媒的2~3倍，PVP-CoNiB觸媒又為CoNiB觸媒的1.7~2倍。糠醛氫化反應中，PVP-CoNiB觸媒對糠醇選擇率更高於CoNiB觸媒，幾無開環產物。
巴豆醛及檸檬醛選擇性氫化反應，皆屬共軛C=C/C=O鍵的選擇性氫化。於相同反應條件下，CoB觸媒活性不佳，CoNiB及PVP-CoNiB觸媒的催化特性較偏向NiB觸媒，都優先選擇氫化共軛C=C/C=O中的C=C鍵成丁醛及香茅醛，CoNiB觸媒活性為NiB觸媒的2倍，PVP-CoNiB觸媒又為CoNiB觸媒的1.6~1.8倍以上。
檸檬醛氫化反應，反應溶劑影響觸媒活性也影響產物的產率，以環己烷為溶劑，對香茅醛產率較高，但活性不佳；以甲醇或乙醇為溶劑，活性較佳，但對香茅醛產率較低。若以香茅醛為主要產物，則以乙醇為溶劑，在低溫(30℃)下進行反應可獲得香茅醛最大產率(86%)；若以香茅醛與香茅醇為主要產物，則以甲醇為溶劑，在短時間內即可獲得最大香茅醛與香茅醇產率(97%)。
摘要(英) The PVP-stabilized CoNiB catalysts were prepared using the chemical reduction method with NaBH4, dissolving the water-soluble polymer of polyvinylpyrrolidone (PVP) in the precursor salt solution as a protective reagent. The PVP-CoNiB catalysts were characterized and examined for their catalysis on the hydrogenation of furfural, crotonaldehyde and citral. PVP polymer could adsorb on the nano-particles of CoNiB via a weak coordination bonding and stabilize it; the molecular weight of PVP about 10,000 was suitable, and the optimal quantity of PVP (PVP/Ni+Co) in the salt solution for preparing catalysts was around 2~10. The PVP-CoNiB samples were characterized by XRD as an amorphous structure and by TEM with a particle size distribution in the range of 3–5 nm. On catalysis, the PVP-CoNiB catalyst was significantly more active and slightly more selective than NiB for hydrogenating furfural to furfuryl alcohol and crotonaldehyde to butyraldehyde. A good yield of citronellal about 87% could be obtained by reducing citral in ethanol at a low reaction temperature of 30oC over the PVP-CoNiB catalyst.
關鍵字(中) ★ 觸媒 關鍵字(英) ★ catalyst
論文目次 第一章 緒論 1
第二章 文獻回顧 3
2-1 金屬-硼奈米合金觸媒 3
2-1-1 物理性質 4
2-1-2 催化特性 13
2-1-2(a) NiB催化性質 13
2-1-2(b) CoB催化性質 14
2-1-2(c) CoNiB催化性質 16
2-2 PVP穩定化金屬奈米微粒 17
2-3 PVP穩定化雙金屬奈米微粒 22
2-4 不飽和醛選擇性氫化反應 23
2-4-1 糠醛 23
2-4-2 巴豆醛 25
2-4-3 檸檬醛 28
第三章 實驗方法與設備 31
3-1 觸媒製備 31
3-1-1 CoNiB觸媒與PVP-CoNiB觸媒之製備 31
3-2 觸媒性質鑑定 33
3-2-1 元素組成分析 33
3-2-2 X-射線繞射分析 33
3-2-3 比表面積測定 34
3-2-4 示差掃描熱量測定 34
3-2-5 X-射線光電子光譜 35
3-2-5 穿透式電子顯微鏡 36
3-3 反應活性測定 36
3-4 實驗藥品及氣體 40
第四章 結果與討論 43
4-1-1 CoNiB觸媒製備 43
4-1-2 PVP-CoNiB觸媒之製 43
4-1-3 CoNiB觸媒與PVP-CoNiB觸媒之ICP組成分析 48
4-1-4 CoNiB觸媒與PVP-CoNiB觸媒之BET鑑定 48
4-1-5 CoNiB與PVP-CoNiB觸媒之TEM顯微影像分析 48
4-1-6 CoNiB及PVP-CoNiB觸媒之X-射線繞射分析 53
4-1-7 CoNiB觸媒與PVP-CoNiB觸媒之DSC熱穩定分析 53
4-1-8 CoNiB觸媒與PVP-CoNiB觸媒之表面分析 58
4-2 奈米非晶態CoNiB與PVP-CoNiB觸媒催化性質的探討 65
4-2-1 丁醛與糠醛氫化 65
4-2-2 巴豆醛選擇性氫化 70
4-2-3 檸檬醛選擇性氫化 75
第六章 結論 87
總結 89
參考文獻 90
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指導教授 陳吟足(Yin-Zu Chen) 審核日期 2006-7-12
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