臺灣博碩士論文加值系統

二氧化鈦光催化程序具高效率、低能耗及無二次污染等優點，廣泛應用於處理揮發性有機物；惟其應用有製備過程繁瑣、顆粒不均、反應後二氧化鈦粉體不易回收及光源利用性低等限制。因此，本研究旨在利用石化廢觸媒為氧化鋁載體，透過超臨界流體法製備複合材料（TiO2/Al2O3），瞭解不同製備參數(前驅物材料、製備溫度、製備時間、鍛燒溫度)合成複合材料之表面結構及型態，並進行光催化降解甲苯實驗，進一步探討反應溫溼度等操作參數對甲苯降解率之影響，藉以評估本研究開發複合材料分解甲苯蒸氣之應用性。
綜合光觸媒特性及光觸媒催化效率結果，以1 M 異丙基鈦之異丙醇溶液為前驅物及0.5 wt.%界面活性劑，於超臨界製備條件下(50℃、140 bar、2小時及無鍛燒)，可得到單一銳鈦礦晶相的奈米級晶粒(~6 nm)，並具有高比表面積及高孔體積特性。二氧化鈦光觸媒於近紫外光催化反應下，有明顯分解甲苯蒸氣之效果，光催化反應遵循一階反應動力模式，於甲苯進流濃度為60 ppm下，光催化反應速率為0.0046 min-1。複合材料之光催化降解60 ppm甲苯研究中，甲苯降解率隨溫度提高有先升後降的趨勢，55℃及9.6 RH%有最佳分解速率0.0096 min-1。此外，以本研究製備二氧化鈦進行甲苯蒸氣光催化分解研究中，發現光催化過程中副產物為苯甲酸、一氧化碳、丙酮等，此結果與甲苯光催化反應途徑之相關文獻相符。綜合言之，複合材料因兼具吸附及光催化作用，相較於二氧化鈦光觸媒，有較佳的光催化活性，整體甲苯降解率由50.5%提高至66.4%，顯示多孔性氧化鋁載體有助於光催化效率提升。

The titanium dioxide (TiO2) photocatalytic process has the advantages of high efficiency, low energy consumption, and no secondary pollution which is widely used for treating VOCs. However, limitations such as complicated preparation process, uneven-sized particles, difficulty of recovering TiO2 powder after reaction, and low light source utilization have been identified. Accordingly, this research aims to study the treatment of toluene by TiO2/Al2O3 composites prepared with a supercritical fluid deposition process. The effects of the preparation parameters (precursor, temperature, time, and calcination temperature) on the properties and photocatalytic activity of products were investigated. The influence of operating parameters (reaction temperature and humidity) on the degradation rate of toluene was also examined.
According to the results of catalyst characterization and their photocatalytic degradation, optimization process was carried out using 1 M isopropyl titanium isopropanol solution with the addition of 0.5 wt.% surfactant, under supercritical preparation conditions at 50◦C and 140 bar for 2 hours withthout calcination. The anatase TiO2 crystalline structure (around 6 nm in diameter) with high specific surface area and large pore volume can be obtained from the optimization process. It was found that the photocatalytic degradation follows the first-order reaction kinetic model, the obtained photocatalytic reaction rate of TiO2 was 0.0046 min-1 at a toluene inflow concentration of 60 ppm. As for photocatalytic degradation of 60 ppm toluene by TiO2/Al2O3 composites, the optimum decomposition rate was 0.0096 min-1 at 55◦C and 9.6 RH%. The by-products (benzoic acid, carbon oxide, acetone, etc.) formed during photocatalytic process are generally consistent with the related literature of its photocatalytic reaction pathway. In summary, TiO2/Al2O3 composited photocatalyst displayed better photocatalytic activity than pure TiO2 due to its high porosity of support. The overall toluene degradation can be enhanced from 50.5% to 66.4% by TiO2/Al2O3 composited photocatalyst.

摘要 I
Abstract II
誌謝 IV
目錄 V
圖目錄 VIII
表目錄 XI
第一章 前言 1
1.1 研究動機 2
1.2 研究目的 3
第二章 文獻回顧 4
2.1 光觸媒及光催化反應機制 4
2.1.1 光觸媒特性及應用 4
2.1.2 光催化反應原理 6
2.1.3 光催化反應動力模式 7
2.2 二氧化鈦光觸媒 9
2.2.1 二氧化鈦物化特性及應用 9
2.2.2 二氧化鈦之光催化特性 13
2.2.3 二氧化鈦製備方式 14
2.2.4 影響二氧化鈦光催化反應速率因子 16
2.3 超臨界流體 23
2.3.1 超臨界流體簡介 23
2.3.2 超臨界流體應用 28
2.3.3 超臨界流體製備奈米材料 30
2.3.4 超臨界流體製備光觸媒相關文獻 34
2.3.5 超臨界流體參數對於光觸媒特性影響 36
第三章 研究材料、設備與方法 40
3.1 研究概要與流程 40
3.1.1 研究概要 40
3.1.2 研究流程 41
3.2 實驗材料與器材 42
3.2.1 實驗材料 42
3.2.2 實驗設備 43
3.3 觸媒製備 44
3.3.1 超臨界流體設備裝置 44
3.3.2 製備方法 45
3.4 甲苯光催化實驗 47
3.5 觸媒特性分析 52
3.5.1 表面型態鑑定 52
3.5.2 晶相特徵分析 54
3.5.3 比表面積分析 56
第四章 結果與討論 58
4.1 複合材料製備 58
4.1.1 廢棄觸媒特性分析 58
4.1.2 田口式實驗設計 58
4.2 製備溫度對二氧化鈦光催化特性之影響 62
4.2.1 表面型態鑑定（SEM、TEM） 62
4.2.2 晶相特徵分析（XRD） 66
4.2.3 比表面積分析（BET） 68
4.2.4 甲苯之光催化降解 69
4.3 製備時間對二氧化鈦光催化特性之影響 72
4.3.1 表面型態鑑定（SEM、TEM） 72
4.3.2 晶相特徵分析（XRD） 76
4.3.3 比表面積分析（BET） 78
4.3.4 甲苯之光催化降解 79
4.4 鍛燒溫度對二氧化鈦光催化特性之影響 82
4.4.1 表面型態鑑定（SEM、TEM） 82
4.4.2 晶相特徵分析（XRD） 86
4.4.3 比表面積分析（BET） 89
4.4.4 甲苯光催化反應 90
4.5 複合材料之甲苯光催化降解 92
4.5.1 光催化反應溫度之影響 93
4.5.2 光催化反應濕度之影響 96
4.6 甲苯光催化降解之中間產物與反應途徑 99
第五章 結論及未來展望 103
5.1 結論…... 103
5.2 建議…… 104
第六章 參考文獻 105

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