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研究生： 李韙丞
Li, Wei-Cheng
論文名稱： 合成活性碳/中孔洞氧化矽與氧化鈷/氧化鋁之粒狀複合材料應用於氨氣吸附與低溫燃燒觸媒
Synthesis Activated Carbon/Mesoporous Silica and Cobalt Oxide/Alumina Oxide as Granular Composite Material, Applied for Ammonia Adsorption and Low-temperature Catalytic Combustion.
指導教授： 林弘萍
Lin, Hong-Ping
學位類別： 碩士
Master
系所名稱： 理學院 - 化學系
Department of Chemistry
論文出版年： 2023
畢業學年度： 111
語文別： 中文
論文頁數： 152
中文關鍵詞： 氨氣吸附 、低溫催化燃燒反應 、溶膠-凝膠法 、海藻酸鹽 、鈷/氧化鋁催化反應
外文關鍵詞： NH3 Adsorption, Low-temperature Catalytic Combustion, Sol-gel Method, Alginate, Co/ Al2O3 catalyst
相關次數： 點閱：196  下載：0 
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    • 近年來，各國政府對於尾氣的不當處理與排放對環境造成的危害越加關注，特別是碳排放和氨氣等廢棄物。本研究成功引入造粒技術合成了氨氣吸附材料和低溫燃燒催化材料。在氨氣吸附材料的合成方面，透過使用炭化的菱殼炭作為孔洞材料，物理混合的孔洞氧化矽以及海藻酸鈉水溶液，滴入檸檬酸與氯化鈣水溶液形成粒狀材料。這個簡單的製程成功合成了具有高達17.9 mg NH3(g) /g材料的吸附效果之粒狀材料，並且該材料於合成過程中是使用低濃度有機酸進行合成，相較於傳統酸改質法或重金屬所合成之金屬有機框架材料(MOF)結構，具有更高的安全性與環境保護性。在低溫燃燒催化反應材料合成方面，本研究使用鈷作為活性金屬，取代傳統催化觸媒中的貴金屬，實現了更低的成本效益。透過使用異相成核法將過渡金屬離子沉積於金屬氧化物載體的表面，相較於傳統所使用的NaBH4或水熱閥等方法，本研究則是使用低濃度之NaOH或K2CO3進行常壓水熱反應，使製程更加簡便且安全。此方法所合成的觸媒在低溫下仍具有優異的催化活性，即使在高空間流速的條件下依然能夠保持高轉化率，對於氫氣和甲烷等氣體的轉化效率都可以達到99% 以上，為低碳能源的使用提供了新的選擇。綜合上述，本研究發展之氨氣吸附與低溫催化燃燒材料在吸附與催化反應上都有不錯的表現性，而粒狀材料相較於粉末材料則是具有更低的氣體背壓以及更高的替換方便性，且具備可直接應用於產業中等相關優勢，期望對於工業的使用上提供了一種新型的選擇與開發方向。

    In recent years, there has been increasing global concern among governments regarding the improper treatment and emissions of exhaust gases, particularly the environmental hazards posed by carbon emissions and waste gases like ammonia. This study has successfully induced granulation technology to synthesize ammonia adsorbent materials and low-temperature combustion catalyst materials. Regarding the synthesis of ammonia adsorbent materials, a simple yet effective process was employed. WSCB was used as a porous material, physically combined with porous silica and sodium alginate solution. This mixture was then dripped into citric acid and calcium chloride solution to form granular materials. The resulting granular materials exhibited impressive adsorption capacity, reaching up to 17.9 mg NH3(g)/g of material. Importantly, the synthesis process employed low-concentration organic acids, enhancing safety and environmental friendliness compared to traditional methods involving acid modification or heavy metal-synthesized MOF structures. In the synthesis of low-temperature combustion catalyst materials, cobalt was utilized as an active metal, replacing the expensive noble metals, commonly found in traditional catalysts. This substitution significantly reduced production costs. The study employed a heterogeneous nucleation method to deposit transition metal ions onto the surface of metal oxide carriers. Unlike traditional methods using NaBH4 or hydrothermal valves, this research utilized low-concentration NaOH or K2CO3 for a simplified and safer conventional pressure hydrothermal reaction. The resulting catalyst exhibited excellent catalytic activity at low temperatures, maintaining high conversion rates even under high space velocities. It achieved conversion efficiencies of over 99% for gases such as hydrogen and methane, presenting a promising option for the utilization of low-carbon energy.

    摘要 i 致謝 vii 目錄 x 表目錄 xv 圖目錄 xvii 第一章 緒論 1 1.1 研究背景及前言 1 1.1.1 氨氣簡介 1 1.1.2 低碳能源簡介 2 1.1.3 空氣汙染物的處理方式 5 1.2 研究目的與方法 6 第二章 文獻回顧 8 2.1 氨氣(NH3)/銨(NH4+)之相關處理材料 8 2.1.1 吸附材料設計與應用 8 2.1.1.1 沸石(Zeolite) 10 2.1.1.2 生物炭(Biochar) 11 2.1.1.3 活性碳(Activated Carbon) 11 2.1.1.4 有機金屬框架(MOFs) 12 2.1.1.5 材料整理與比較(Comparison of adsorbent materials) 13 2.1.2 吸附機制討論 14 2.1.2.1 吸附位點 15 2.1.2.2 水氣存在之影響 17 2.2 中孔洞氧化矽合成方式 18 2.2.1 軟模板法合成 19 2.2.2 無模板法合成 23 2.3 催化材料合成技術之整理 24 2.3.1 觸媒載體之介紹 24 2.3.2 金屬塗佈之方式介紹 25 2.3.3 鍛燒溫度(混合晶相問題) 27 2.4 造粒技術整合 28 2.4.1 海藻酸鈉特性簡介 29 2.4.2 作用機制簡介 30 2.4.3 陽離子對於凝膠化反應之影響 31 2.4.3.1環境pH值對於凝膠化反應之影響 31 2.4.3.2濃度對於凝膠化反應之影響 32 2.4.4 粉末顆粒對於造粒強度之影響 33 2.4.5 溫度對於交聯機制之影響 34 第三章 實驗方法、儀器及藥品 36 3.1 實驗藥品 36 3.2 實驗儀器 38 3.2.1 掃描式電子顯微鏡(Scattering Electron Microscope, SEM) 38 3.2.2 能量色散X射線譜(Energy-Dispersive X-ray Spectroscopy, EDS) 39 3.2.3 穿透電子顯微鏡(Transmission Electron Microscope, TEM) 40 3.2.4 熱重分析儀(Thermogravimetric Analysis , TGA) 41 3.2.5 氮氣等溫吸附-脫附儀(Nitrogen Adsorption-Desorption Isotherms) 42 3.2.6 紫外光可見光/近紅外光光譜儀(UV-VIS/NIR Spectrophotometer) 52 3.2.7 X-射線繞射儀(X-Ray Diffractometer, XRD) 53 3.2.8 元素分析儀(Elemental Analysis, EA) 53 3.2.9 程序升温還原(Temperature-Programmed Reduction, TPR) 54 3.3 實驗方法 55 3.3.1 利用無模板法合成中孔洞氧化矽 55 3.3.2 利用軟模板法合成中孔洞氧化矽 56 3.3.3 碳/多孔洞氧化矽複合材料之造粒合成 57 3.3.4 利用異相成核法合成Co(OH)2/Al2O3之濾餅 58 3.3.5 利用異相成核法合成CoCO3/Al2O3之濾餅 59 3.3.6 利用造粒法合成Co3O4/Al2O3造粒 60 第四章 粒狀氨氣吸附材料合成與機制討論 61 4.1 研究動機與目的 61 4.2 粒狀氨氣吸附材料與原料之合成 62 4.2.1 碳源使用與分析 62 4.2.2 中孔洞氧化矽合成 65 4.2.2.1 無模板法合成 65 4.2.2.2 軟模板法合成 69 4.2.3 粒狀材料之製程優化 72 4.2.3.1 酸性溶液造粒 73 4.2.3.2 中孔洞氧化矽的置入 76 4.3 吸附結果之討論 79 4.3.1 不同環境造粒之吸附表現 80 4.3.1.1 不同環境造粒之氨氣吸附表現 80 4.3.1.2 材料之水氣吸附表現 81 4.3.2 不同碳材之吸附表現 83 4.3.3 使用不同氧化矽作為前驅物探討氧化矽對於NH3吸附之影響 85 4.3.3.1不同比表面積之氧化矽對於NH3吸附之影響 86 4.3.3.2 使用矽凝膠取代多孔洞氧化矽作為氧化矽來源 89 4.3.4 材料含有海藻酸鈉量對於氨氣捕捉量之影響 92 4.3.5 氣體濃度與流量控制條件對於氨氣捕捉效率之影響 93 4.4 吸附機制之討論 94 4.4.1 材料前驅物之吸附熱力學討論 (Adsorption Thermodynamics) 96 4.4.1.1 Langmuir等溫吸附模型 96 4.4.1.2 Freundlich等溫吸附模型 97 4.4.2 活性碳之吸附熱力學模型擬合 98 4.4.3 多孔洞氧化矽之吸附熱力學模型擬合 100 4.5 章節結論 101 4.6 未來發展之方向與期許 102 第五章 低溫燃燒催化反應 103 5.1 研究動機與目的 103 5.2 粒狀金屬氧化物之催化材料合成與催化結果 103 5.2.1 金屬之選擇 104 5.2.2 載體之選擇 106 5.2.3 沉澱析出法製程改善 109 5.2.3.1 沉澱析出速率之調整 109 5.2.3.2 水熱因素之影響 112 5.2.3.3 沉澱劑之改變 114 5.2.4 金屬離子置換法 119 5.2.5 金屬-載體交互作用之討論 121 5.2.5.1 金屬比例 122 5.2.5.2 鍛燒溫度之改變 124 5.2.6 大量製程之設計 127 5.3 催化結果之討論 130 5.3.1 H2低溫燃燒催化結果與最佳參數之討論 130 5.3.2 CH4低溫燃燒催化結果與最佳參數之討論 131 5.4 章節結論 132 5.5未來發展之方向與期許 133 第六章 總結論 134 參考文獻 136

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