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研究生： 徐承昱
Hsu, Cheng-Yu
論文名稱： 合成中孔洞金屬氧化物顆粒狀觸媒在甲醇蒸氣重組反應及溫室氣體去除之研究
A Study on the Synthesis of Mesoporous Metal Oxide Granular Catalysts for Methanol-Steam Reforming and Removal of Greenhouse Gases
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： 97
中文關鍵詞： 非貴金屬觸媒 、海藻酸鈉造粒 、甲醇蒸汽重組 、一氧化二氮催化分解 、產氫
外文關鍵詞： non-noble metal catalyst, sodium alginate granulation, methanol-steam reforming, hydrogen production, catalytic decomposition of nitrous oxide
相關次數： 點閱：155  下載：0 
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    • 本論文主要研究非貴金屬觸媒之合成與造粒，共分為兩大部分，第一部分以造粒法直接合成-鋁酸銅鎳應用於甲醇蒸汽重組反應中，主要目的為再生能源-氫氣之產生。第二部分以異相成核法合成氫氧化鐵/氧化鋅之濾餅，並經造粒後獲得氧化銅/氧化鐵/四氧化三鐵/鐵酸鋅之觸媒，應用於一氧化二氮分解反應中，進而處理半導體製程中排放之尾氣。
    本實驗第一部分探討了在鋁酸銅鎳造粒觸媒製程中，載體與海藻酸鈉比例、離子交換溶液之濃度、離子交換時間及溫度等參數，優化造粒之機械強度以及提升活性金屬在造粒中之比例，因此在甲醇蒸汽重組反應中有良好之甲醇轉化率及氫氣產率，且材料在反應後可經由煅燒過程除去積碳，恢復相當程度之觸媒活性。將造粒觸媒與過去本實驗室粉末觸媒相比，造粒觸媒則具有較少之粉塵汙染、反應器背壓、一氧化碳排放等優勢。此外，本實驗亦採用低成本之工業級硝酸銅、硝酸鎳及活性氧化鋁，將製程成功放大至公斤級，驗證了材料在工業應用之可行性。
    第二部分以氧化鋅作為載體，利用其具有豐富氧空缺之優勢，可助於斷裂一氧化二氮中之氮氧鍵結，再由異相成核法擔載活性金屬鐵、鋁，水熱過程促使氫氧化物結構重組，使活性金屬在載體上分散性提高，後續滴入銅鎳離子溶液進行造粒，並且針對異相成核進料時間、水洗方式以及離子交換溶液進行研究。研究重心一方面為提升機械強度和觸媒活性以符合商用標準，另一方面則為簡化製程、節省成本，最終成功放大量至一次產出數公斤之造粒，且同時在一氧化二氮分解反應中維持良好之分解率以及低副產物之生成，目前亦成功於半導體尾氣處理計畫中使用。
    第二部分後段則將載體更換為氧化鋁及單水鋁石，鋁載體有高比表面積與熱穩定性之優勢，其中又以活性氧化鋁造粒具有較佳之機械強度與催化活性，在一氧化二氮分解反應中有較低之反應溫度，具有後續開發之潛力。

    As industrial development continues to flourish, environmental pollution has become a significant issue. The development of clean alternative energy sources and the reduction of greenhouse gas emissions are two major research trends. Therefore, the goal of this study is to synthesize a low-cost, highly efficient non-noble metal catalyst to produce renewable energy - hydrogen and to remove greenhouse gases-nitrous oxide.
    In the first part of the experiment, active metals-copper and nickel were loaded onto active alumina using the sodium alginate granulation method to synthesize low-cost copper-nickel aluminate granular catalyst. The catalyst was applied in the methanol-steam reforming reaction at a temperature of 250°C, the methanol conversion rate and hydrogen selectivity were close to theoretical values, and low emissions of by-product carbon monoxide were produced. In the future, this catalyst can be used in hydrogen fuel cells.
    In the second part of the experiment, iron and aluminum were loaded onto zinc oxide using deposition–precipitation method, followed by granulation with a copper-nickel ion solution to obtain a copper oxide/zinc oxide/iron oxide/zinc ferrite catalyst. This catalyst was used in the catalytic decomposition of nitrogen oxide at 500°C, and the nitrous oxide decomposition rate of over 95% under a high flow rates and nitrous oxide concentration. Subsequently, this catalyst can be used for exhaust gas treatment in semiconductor manufacturing processes.

    摘要 i SUMMARY ii 致謝 viii 目錄 x 圖目錄 xiii 表目錄 xix 第一章 緒論 1 1.1 淨零排放 (Net Zero) 1 1.2 工業產氫法介紹 1 1.2.1 甲醇蒸汽重組反應 (MSR) 2 1.2.2 甲醇部分氧化反應 (POM) 2 1.2.3 甲醇氧化性蒸汽重組反應 (ATRM) 3 1.2.4 應用於甲醇蒸汽重組反應之非貴金屬觸媒介紹 3 1.3 一氧化二氮去除法介紹 4 1.3.1 熱分解 (Thermal decomposition) 5 1.3.2 直接催化分解 (Direct catalytic decomposition (de N2O)) 5 1.3.3 選擇性催化還原 (Selective catalytic reduction (SCR)) 5 1.4 孔洞材料簡介 6 1.5 觸媒載體簡介 7 1.5.1 氧化鋁簡介 7 1.5.1.1 氧化鋁製備法 9 1.5.2 氧化鋅簡介 10 1.6 氧空缺簡介 11 1.7 水熱法簡介 13 1.7.1 溶解-析出機制 (Dissolution-precipitation) 14 1.7.2 原位生長機制 (In-situ growth process) 14 1.8 複合金屬氧化物材料合成 15 1.8.1 共沉澱法(Co–precipitation) 15 1.8.2 異相成核法(Deposition–precipitation) 15 1.8.3 含浸法(Impregnation) 15 1.8.4 離子交換法(Ion exchange) 15 1.9 褐藻酸鈉造粒技術簡介 16 第二章 合成與鑑定 18 2.1 實驗藥品 18 2.2 實驗步驟與流程示意圖 19 2.2.1 鋁酸銅鎳觸媒之合成及造粒 19 2.2.2 以 30 公升級加熱槽合成鋁酸銅鎳造粒觸媒 20 2.2.3 氫氧化鐵/氧化鋁粉體之合成 21 2.2.4 氫氧化鐵/氧化鋅粉體之合成 22 2.2.5 以 300 公升級加熱槽合成氫氧化鐵/氧化鋅粉體 23 2.2.6 異相成核濾餅之造粒 24 2.3 儀器設備 25 2.3.1 X-射線粉末繞射光譜 (Powder X-Ray Diffraction；PXRD) 25 2.3.2 氮氣等溫吸附/脫附測量 (N2 Adsorption / Desorption Isotherm) 26 2.3.3 熱重量分析儀 (Thermogravimetric Analysis；TGA) 31 2.3.4 能量散射X-射線譜 (Energy-dispersive X-ray Spectroscopy；EDX) 32 2.3.5 X光光電子能譜儀 (X-ray photoelectron spectroscopy；XPS) 32 2.3.6 掃描式電子顯微鏡 (Scanning Electron Microscope；SEM) 33 2.3.7 氫氣程序升溫還原(H2 temperature programmed reduction ; H2-TPR) 34 2.3.8 機械強度測量 34 第三章 鋁酸銅鎳造粒觸媒應用於甲醇蒸汽重組反應 35 3.1 研究動機 35 3.2 甲醇蒸汽重組催化測試設備及參數 36 3.3 以造粒法合成鋁酸銅鎳觸媒 37 3.3.1 不同活性氧化鋁/褐藻酸鈉比例之探討 38 3.3.2 離子交換溫度之探討 40 3.3.3 離子交換時間之探討 42 3.3.4 浸泡金屬溶液濃度之探討 44 3.4 鋁酸銅鎳造粒觸媒用於甲醇蒸汽重組反應 46 3.5 以 30 公升級加熱槽合成鋁酸銅鎳造粒觸媒並用於甲醇蒸汽重組反應 50 3.6 甲醇蒸汽重組反應後之鋁酸銅鎳造粒觸媒分析及再活化 53 3.7 鋁酸銅鎳造粒觸媒並用於甲醇蒸汽重組反應之反應機制探討 59 第四章 氧化銅/氧化鋅/四氧化三鐵/鐵酸鋅造粒觸媒應用於笑氣分解反應 61 4.1 研究動機 61 4.2 一氧化二氮催化測試設備 62 4.3 氧化銅/氧化鋅/四氧化三鐵/鐵酸鋅造粒觸媒 63 4.3.1 以異相成核法合成造粒觸媒 63 4.3.2 進料時間之探討 64 4.3.3 晶相之探討 67 4.3.4 水洗對造粒之影響 70 4.3.5 離子交換溶液之水來源探討 76 4.3.6 離子交換溶液之選擇 79 4.3.7 以 300 公升級加熱槽合成氧化銅/氧化鋅/四氧化三鐵/鐵酸鋅造粒觸媒並應用於笑氣分解反應 83 4.4 氧化銅/三氧化二鐵/氧化鋁造粒觸媒 87 4.4.1 不同鋁來源之探討 87 4.4.2 氧化銅/三氧化二鐵/氧化鋁造粒觸媒應用於一氧化二氮分解反應 89 第五章 總結 91 參考文獻 92

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