臺灣博碩士論文加值系統

本研究旨在以疏水性的正己烷(n-Hexane)及親水性的乙酸乙酯(Ethyl acetate, EA)蒸氣為目標污染物，進行系列氣相光催化分解實驗，藉以測試自製薄膜光觸媒於去除揮發性有機物之可行性，並探討rGO摻雜比例對TiO2光催化活性之影響。另外，本研究分析目標污染物於不同環境參數(反應溫度、環境濕度)下的光催化分解速率，藉以探討反應物之親疏水性與其光化分解速率上的關聯性。在光觸媒製備上，本研究分別以聚偏氟乙烯(Polyvinylidene difluoride, PVDF)及聚碸(Polysulfone, PSF)為載體，經由水熱合成法(Hydro-thermal method)製備不同重量比例還原氧化石墨烯(reduced Graphene Oxide, rGO)之二氧化鈦(TiO2)，再利用浸漬沉澱法(Immersion precipitation method)製備成二氧化鈦/聚偏氟乙烯 (TiO2/PVDF)與二氧化鈦/聚碸 (TiO2/PSF)薄膜光觸媒。
實驗結果顯示：正己烷蒸氣與乙酸乙酯蒸氣的光催化分解反應，皆遵循擬一階反應動力關係。經由EDX分析結果顯示，T-PVDF薄膜表面的TiO2較T-PSF來的高，使得T-PVDF整體有較快的光催化活性，基於此選用PVDF做為改質rGO/ TiO2的固定化材料。在正己烷光催化分解方面，在所設定之環境溫度範圍內(35 ~ 75℃)，隨著反應溫度上升，分解速率呈現先增、後減的反應趨勢，並以45℃實有最高的分解速率(k = 0.264 hr-1)；另外在環境濕度範圍內(Dry ~ 30 g/m3)，則以乾燥條件下，正己烷有較快的分解速率，水氣會干擾正己烷的光催化分解；另外，就rGO觸媒改質之摻雜比例而言，以摻雜7%rGO時，對於正己烷有最快的光催化分解速率(k = 0.282 hr-1)。
其次，針對乙酸乙酯蒸氣光催化分解反應方面，其反應趨勢與正己烷相類似。在反應溫度影響上，其光催化分解速率，隨反應溫度上升逐漸增加，並在75℃時，有最高反應速率；在濕度影響方面，則以濕度濃度為10 g/m3時有較快的反應速率，而此時反應溫度則以55℃時有最快反應速率，雖然適度濕度環境中，有助於乙酸乙酯蒸氣光催化分解，但當水氣含量過高時，仍會干擾乙酸乙酯蒸氣光催化分解；在摻雜rGO的效應上，並未有明顯提升光催化分解效果，但在反應濕度20~30 g/m3環境下，使仍TiO2保有一定的光催化活性；整體而言，乙酸乙酯蒸氣光催化分解，以未摻雜rGO時、反應溫度55℃時、10 g/m3濕度條件下，有最快的分解速率(0.271 hr-1)。
綜合比較正己烷與乙酸乙酯蒸氣的光催化分解速率，在乾燥條件時，它們的反應速率大致相同，其可能原因與其親疏水性以及化學鍵結構有關。親水性的乙酸乙酯較易被吸附於TiO2表面的活性位置，有利於後續光催化分解反應的進行。此外，正己烷與乙酸乙酯本身的化學鍵結構強弱，得使後續分解反應的中間產物有所不同，使觸媒在表面反應速率有些許差異；對於摻雜rGO而言，推測有助於提升對疏水性之正己烷的吸附；最終，對於氣相光催化分解反應整體而言，光催化反應速率的限制步驟，仍取決於反應物與光觸媒間的親和性有關。

Gas-phase photocatalysis of both ethyl acetate and n-hexane, with a similar molecular weight but with different hydrophilicity, were investigated by using TiO2-based thin-films as photocatalysts in this study. Series of photocatalytic degradation experiments for both target compounds were performed in a batch photocatalytic reactor under illumination of near-UV light. Two types of thin-film photocatalyst, including pure TiO2 or reduced graphene oxide (rGO) doped TiO2 composting with commercial polymer substrates, polyvinylidene difluoride (PVDF) or polysulfone (PSF), were applied. Some experimental parameters including reaction temperature, water vapor content, types of deposition substrates, and the amount of doped rGO were tested for investigating their effects on photocatalytic degradation rates of target pollutants. The contribution of hydrophilicities of organic compounds to their degradation rate was discussed, too.
The experimental results demonstrate that prepared TiO2-based thin-film photocatalysts can effectively decompose both ethyl acetate and n-hexane vapor in a short reaction time. Their photocatalytic degradation reactions follow pseudo first-order reaction kinetics. Owing to more photocatalysts that can participate in the reaction, the photocatalyst using PVDF as the composing substrate has higher photocatalytic activities than by using PSF as the composing substrate. For the effects of reaction temperatures (35 ~ 75 ℃) on reaction rates for both target compounds, ethyl acetate had the highest reaction rate at 75℃ but n-hexane peaked its degradation rate at 45℃. For the effects of humidity (dry ~ 30 g/m3) on their degradation rates, the presence of water vapor could interfere the photocatalytic degradation rate of n-hexane, even though the highest degradation rate for ethyl acetate was observed as water vapor concentration equal to 10 g/m3. In addition, for the doping effects of rGO on the photocatalyst activity, higher degradation rates were observed for n-hexane while TiO2 co-doped with more rGO, but less changes in the degradation rate of ethyl acetate after co-doped with rGO.
Comparing both photocatalytic decomposition rates of ethyl acetate and n-hexane vapor, their reaction rates are near each other in dry conditions. In humid conditions, on the other hand, the degradation rate of n-hexane is inhibited due to the presence of water vapor but the degradation rate of ethyl acetate is less affected, which should be caused by these two reactants having different hydrophilicity. Ethyl acetate is more hydrophilic than n-hexane, and it is easier to be adsorbed by TiO2, even in humid environment. This study confirmed that the adsorption of reactants onto photocatalyst is a critical mechanism for the photocatalysis of many organic vapors and the photocatalytic reaction rates can be enhanced by modifying affinity between them. Doping with suitable amount of rGO may be a potential catalyst modification method.

摘要 i
Abstract iii
致謝 v
目錄 vi
圖目錄 ix
表目錄 xv
第一章 緒論 1
1-1 研究緣起 1
1-2 研究目的 4
第二章 文獻回顧 5
2-1 正己烷與乙酸乙酯流佈與危害 5
2-1-1 正己烷蒸氣在環境中的流佈 6
2-1-2 乙酸乙酯蒸氣在環境中的流佈 6
2-1-3 正己烷蒸氣污染特性與危害 7
2-1-4 乙酸乙酯蒸氣污染特性與危害 9
2-2 揮發性有機蒸氣控制技術 11
2-2-1 揮發性有機污染物控制技術 11
2-2-1-1 正己烷蒸氣的控制技術 12
2-2-1-2 乙酸乙酯蒸氣的控制技術 13
2-3 半導體金屬氧化物(SMO)光催化分解反應 14
2-3-1 SMO種類與特性 14
2-3-2 SMO光催化反應原理 16
2-4 光催化分解反應機制與反應動力模式 17
2-4-1 影響光催化反應速率因素 17
2-4-1-1 反應溫度 17
2-4-1-2 水氣含量 19
2-4-1-3 光源 20
2-4-1-4 反應物特性(親疏水性) 22
2-4-2 異相光催化反應機制與反應動力 24
2-4-2-1單分子反應 26
2-4-2-2單分子競爭反應 26
2-4-2-3雙分子競爭反應 27
2-4-2-4雙分子無競爭反應 28
2-5 光催化劑改質與固定化處理 29
2-5-1 摻雜石墨烯之二氧化鈦光觸媒 29
2-5-1-1 石墨烯及石墨烯衍生物特性與應用 29
2-5-1-2 半導體金屬氧化物摻雜石墨烯製備 32
2-5-2 薄膜光觸媒製備 38
2-5-2-1 薄膜光觸媒之製備技術 38
2-5-2-2 複合聚偏氟乙烯之二氧化鈦薄膜製備 39
2-5-2-3 複合聚碸之二氧化鈦薄膜製備 46
第三章 實驗材料與方法 52
3-1 研究架構與規劃 52
3-1-1 研究概要 52
3-1-2 研究流程 53
3-2 實驗材料與儀器 54
3-2-1 實驗材料 54
3-2-2 實驗儀器與設備 55
3-3 實驗方法與分析 56
3-3-1 薄膜光觸媒之製備 56
3-3-1-1 氧化石墨烯製備 56
3-3-1-2 rGO/TiO2光觸媒製備 57
3-3-1-3 TrGO-PVDF薄膜光觸媒製備 58
3-3-1-4 T-PSF薄膜光觸媒製備 59
3-3-2 氣相光催化反應系統 64
3-3-2-1 光催化反應器 64
3-3-2-2 反應器氣密性測試 66
3-3-2-3 光催化反應實驗 67
3-3-2-4 檢量線配置 68
3-3-3 正己烷蒸氣濃度定量 69
3-3-4 乙酸乙酯蒸氣濃度定量 70
3-4 複合材料表面特性分析 71
3-4-1 掃描式電子顯微鏡 (Scanning Electoron Microscope, SEM) 71
3-4-2 X光繞射分析儀 (X-ray Diffractometer, XRD) 73
3-4-3 接觸角分析儀 (Contact Angle Meter) 75
第四章 結果與討論 76
4-1 複合薄膜光觸媒特性分析 76
4-1-1 薄膜光觸媒表面形貌分析(SEM) 76
4-1-1-1 TiO2-PVDF薄膜光觸媒形貌分析 78
4-1-1-2 TiO2/rGO-PVDF薄膜光觸媒形貌分析 81
4-1-1-3 TiO2-PSF薄膜光觸媒形貌分析 85
4-1-2 薄膜光觸媒表面化學成分分析(EDX) 88
4-1-3 薄膜光觸媒晶相特徵分析(XRD) 98
4-1-4 薄膜光觸媒材料親疏水性分析(Contact Angle Meter) 102
4-2 正己烷蒸氣與乙酸乙酯蒸氣之光催化分解反應 105
4-2-1 反應溫度對正己烷蒸氣與乙酸乙酯蒸氣分解速率之影響 110
4-2-2 環境濕度對正己烷蒸氣與乙酸乙酯蒸氣分解速率之影響 116
4-3 固定化材料PVDF與PSF對VOCS蒸氣光催化分解速率之影響 130
4-3-1 環境溫度對正己烷蒸氣與乙酸乙酯蒸氣分解速率之影響 130
4-3-2 環境濕度對正己烷蒸氣與乙酸乙酯蒸氣分解速率之影響 136
4-4 摻雜還原氧化石墨烯複合薄膜之VOCS蒸氣光催化分解反應 150
4-4-1 摻雜rGO比例對VOCs蒸氣光催化分解速率影響 150
4-4-2 溫度、濕度及rGO比例對VOCs蒸氣光催化分解速率影響 164
4-5 揮發性有機物親水特性對其光催化分解速率之影響 174
4-5-1 正己烷與乙酸乙酯光催化分解速率比較 174
4-5-2 異丙醇、乙酸乙酯、苯以及正己烷光催化分解速率彙整比較 176
4-6 VOCS光催化去除效能比較 183
4-7 薄膜光觸媒分解VOCS蒸氣之反應機制 186
4-7-1 VOCs光催化分解路徑 186
4-7-2 VOCs光催化分解反應機制 190
4-7-2-1 T-PSF、T-PVDF及改質之TrGO-PVDF系列薄膜光觸媒影響 190
4-7-2-2 反應溫度之影響 192
4-7-2-3 環境濕度之影響 194
第五章 結論與建議 196
5-1 結論 196
5-2 建議事項 197
參考文獻 198
附錄A. 正己烷於各操作參數下之光催化分解實驗結果 A-1
附錄B. 乙酸乙酯於各操作參數下之光催化分解實驗結果 B-1
附錄C. 近紫外光燈管-波長光譜圖 C-1
附錄D. 不同溫度下-絕對濕度與相對濕度關係表 D-1

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