臺灣博碩士論文加值系統

本研究探討應用自製rGO/TiO2-PVDF複合薄膜光觸媒，去除水中藥物和個人保健品 (pharmaceuticals and personal care products, PPCPs)的可行性。研究中分別針對親水性的磺胺甲基噁唑(sulfamethoxazole, SMX)及疏水性的卡馬西平(carbamazepine, CBZ)，進行液相光催化分解實驗。分別探討rGO摻雜比例、水溶液酸鹼值、以及污染物親疏水性等，對於相關污染物分解速率的影響；另外，研究中也藉由SME、XRD、EDX及接觸角分析等測量儀器，測定薄膜光觸媒表面形貌、晶相、化學元素及親疏水性等性質，藉以探討薄膜光觸媒性質與污染物光催化分解速率間的關聯性。針對薄膜光觸媒的製備，此研究中先利用水熱合成法(Hydro-thermal method)，製備複合還原氧化石墨烯(Reduced Graphene Oxide, rGO)之二氧化鈦(TiO2)，之後再以聚偏氟乙烯(PVDF)為載體，利用浸漬-沉澱法(Immersion precipitation method)製備成rGO/TiO2-PVDF薄膜光觸媒，此薄膜光觸媒可兼顧光催化活性與實務應用需求。
研究結果顯示：本研究證實所製備的rGO/TiO2-PVDF複合薄膜光觸媒，可在近紫外光(λ= 365 nm)照射下，快速地催化分解SMX及CBZ；SMX及CBZ的光催化分解反應，遵循擬一階反應動力關係，並以在酸性水環境中，有較快的分解速率。其可能與相關污染物在酸性環境中，較易被光觸媒所吸附，並進一步分解所致；另外，就rGO觸媒改質之摻雜比例而言，以摻雜5% rGO時有較快的光催化分解速率 (kSMX = 0.552 hr-1、kCBZ = 0.534 hr-1)，其作用應主要在於改變電子-電洞再結合速率。
綜合比較兩種PPCPs的光催化分解速率，以具親水性的SMX，略高於疏水性的CBZ。高親水性的污染物因與二氧化鈦結合性較佳，分解速率也較快。本研究也據以推論此類光催化分解反應的速率限制步驟，應主要在於反應物被光觸媒吸附的速率。而且但當水溶液酸鹼環境改變時，不僅改變反應物親疏水性，反應物在水中以分子狀或離子狀分布情形，以及二氧化鈦表面的電性等，也皆隨之改變，成為一複雜的競爭吸附行為。液相光催化反應在水分子包覆干擾下，反應物的親疏水性，不是決定整體光催化分解反應之單一因子，其仍需視反應物與光觸媒間的吸附情形，以及當時觸媒的催化活性來決定。

This study prepared rGO/TiO2-PVDF composite thin-film photocatalysts to remove sulfamethoxazole (SMX) and carbamazepine (CBZ), two commonly using pharmaceuticals and personal care products (PPCPs) but with different hydrophilic/hydrophobic characteristics. The rGO/TiO2-PVDF composite thin-film photocatalysts were prepared by mixing reduced graphene oxide/ titanium dioxide (rGO/TiO2) composite photocatalyst and polyvinylidene fluoride (PVDF) powder in a dimethylacetamide and acetone mixture solution, and then forming thin-film photocatalysts through an immersion precipitation process. The doping effects of rGO, pH levels of solution, and hydrophilic/hydrophobic properties of PPCPs on their degradation rates were investigated. For investigating the relationships of the photocatalytic degradation reaction rates of both PPCPs with the activities of photocatalysts, in addition to degradation rates of SMX and CBZ, several catalyst properties including its surface morphology, crystalline structures, elemental distribution, and contact angles were measured.
Some important results were achieved by this study. The experimental results demonstrated fast degradation of both SMX and CBZ by the prepared rGO/TiO2-PVDF photocatalyst under the illumination of near-UV light (λ= 365 nm). The degradation reactions of them basically followed the pseudo first-order reaction kinetics and higher degradation rates were detected in more acidic conditions due to more adsorption of reactants by the photocatalysts. For the doping effects of rGO, TiO2 had the highest activity by co-doping with 5% rGO, which resulted in both SMX and CBZ having the highest degradation rate constants of kSMX 0.552 hr-1 and kcbz 0.534 hr-1, respectively. It is expected that the doped rGO can reduce the recombination rates of electron-hole pairs and enhance photocatalytic activity of TiO2.
The experimental results also showed that the SMX generally had higher degradation rate than CBZ, which might be because that the former one was more hydrophilic. SMX is more easily absorbed by TiO2, since TiO2 is a hydrophilic substance under illumination of suitable light energy. Accordingly, this study proposed that the adsorption rates of reactants onto photocatalysts would be the rate determining step for the photocatalytic reaction. But the affinity potential of reactants for photocatalysts would not be the only factor to determine the overall reaction rate when solution pH levels change, because that hydrophilicity and intrinsic activities of photocatalysts may be also altered at the same time.

摘要 I
目錄 VI
圖目錄 VIII
表目錄 XI
第一章 緒論 1
1-1 研究背景 1
1-2 研究目的 4
第二章 文獻回顧 5
2-1 二氧化鈦光觸媒特性及光催化分解反應 5
2-1-1 二氧化鈦特性 5
2-1-2光催化反應反應原理 6
2-1-3 光催化反應機制 7
2-2影響光催化分解反應速率因子 11
2-3 藥物及個人保健用品(PPCPs)特性與現況 13
2-3-1 Carbamazepine (CBZ)特性與環境中的流佈 18
2-3-2 Sulfamethoxazole(SMX)特性與環境中的流佈 19
2-4 PPCPs去除技術 20
2-5 CBZ及SMX之光催化分解反應 22
2-5-1 CBZ 22
2-5-2 SMX 24
2-6 薄膜光觸媒製備技術 26
2-6-1 固定化光觸媒製備 26
2-6-2 聚偏氟乙烯(PVDF)薄膜製備 28
2-7 石墨烯 29
第三章 研究材料及方法 35
3-1 研究架構與流程 35
3-1-1 研究概述 35
3-1-2 研究架構 35
3-2 實驗材料與設備 37
3-2-1 實驗材料 37
3-2-2 實驗儀器設備 38
3-3 實驗方法與分析 39
3-3-1 薄膜光觸媒之製備 39
3-3-2 異相光催化反應系統 41
3-3-3 CBZ及SMX濃度檢測 45
3-4 光觸媒表面特性分析儀器 46
3-4-1 掃描式墊子顯微鏡(scanning electron microscope，SEM) 46
3-4-2 X光繞射分析儀(X-ray Diffractometer，XRD) 47
3-4-3 接觸角測試 48
第四章 結果與討論 49
4-1 薄膜光觸媒之分析 49
4-1-1薄膜光觸媒形貌分析(SEM) 49
4-1-2光觸媒表面結晶與化學組成(EDX) 56
4-1-3薄膜光觸媒晶相特徵分析(XRD) 63
4-1-4薄膜光觸媒接觸角分析 66
4-2 CBZ及SMX應用於複合薄膜光觸媒光催化分解反應 71
4-2-1 SMX及CBZ分解反應速率關係 71
4-2-2水溶液pH值影響 74
4-2-3還原氧化石墨烯摻雜比例影響 85
4-3薄膜光觸媒吸附實驗 89
4-4 有機物親疏水性特性與光催化分解效率之關聯性 96
4-5薄膜光觸媒反應機制 102
第五章 結論與建議 109
5-1 結論 109
5-2 建議事項 110
參考文獻 111
附錄A.污染物光催化分解反應濃度隨時間變化一覽表 1
附錄B.吸附實驗反應濃度隨時間變化一覽表 6

 
圖目錄
圖 2 1銳鈦礦、金紅石和板鈦礦的晶體結構[Mohamad et al., 2015] 6
圖 2 2異相光催化反應是示意圖[Herrmann et al., 1999] 9
圖 2 3不同接觸角水滴圖 11
圖 2 4不同國家地表水樣中NSAID濃度[Ebele et al., 2017] 15
圖 2 5光催化降解途徑[Hu et al., 2019] 23
圖 2 6 SMX分解途徑[Wang et al., 2011] 25
圖 2 7石墨烯結構圖[Tiwari et al., 2018] 30
圖 2 8氧化石墨烯結構圖[Tiwari et al., 2018] 30
圖 2 9還原氧化石墨烯結構圖[Tiwari et al., 2018] 31
圖 3 1研究架構流程 36
圖 3 2反應器示意圖 42
圖 3 3 CBZ檢量線 43
圖 3 4 SMX檢量線 44
圖 3 5 HPLC HITACH-CM500系列 45
圖 3 6掃描式墊子顯微鏡(成功大學) 46
圖 3 7多功能X光繞射儀 (成功大學) 47
圖 3 8自動接觸角分析儀 48
圖 4 1 P-25 TiO2粉末表面形貌 50
圖 4 2 GO表面形貌 50
圖 4 3 rGO表面形貌 50
圖 4 4 PVDF表面形貌 51
圖 4 5 TP平面形貌 51
圖 4 6 TP剖面形貌 52
圖 4 7 TP-rGO3平面形貌 52
圖 4 8 TP-rGO3剖面形貌 53
圖 4 9 TP-rGO5平面形貌 53
圖 4 10 TP-rGO5剖面形貌 53
圖 4 11 TP-rGO7平面形貌 54
圖 4 12 TP-rGO7剖面形貌 54
圖 4 13 TP-rGO10平面形貌 54
圖 4 14 TP-rGO10剖面形貌 55
圖 4 15 TP-rGO12平面形貌 55
圖 4 16 TP-rGO12剖面形貌 55
圖 4 17 TP Mapping元素分析結果 57
圖 4 18 TP-rGO Mapping元素分析結果 58
圖 4 19 TiO2表面元素分析結果 59
圖 4 20 GO表面元素分析結果 59
圖 4 21 rGO表面元素分析結果 59
圖 4 22 PVDF表面元素分析結果 60
圖 4 23 TP表面元素分析結果 60
圖 4 24 TP-rGO3表面元素分析結果 60
圖 4 25 TP-rGO5表面元素分析結果 61
圖 4 26 TP-rGO7表面元素分析結果 61
圖 4 27 TP-rGO10表面元素分析結果 61
圖 4 28 TP-rGO12表面元素分析結果 62
圖 4 29 PVDF、TiO2、rGO、GO XRD之掃描結果 64
圖 4 30 TP及TP-rGO系列薄膜XRD之掃描結果 65
圖 4 31 TP及TP-rGO3接觸角分析 66
圖 4 32 TP-rGO5及TP-rGO7接觸角分析 67
圖 4 33 TP-rGO10及TP-rGO12接觸角分析 67
圖 4 34接觸角角度與摻雜rGO比例 68
圖 4 35 TP及TP-rGO3接觸角分析(UV) 68
圖 4 36 TP-rGO5及TP-rGO7接觸角分析(UV) 69
圖 4 37 TP-rGO10及TP-rGO12接觸角分析(UV) (X) 69
圖 4 38面積擴散速率與摻雜rGO比例(UV) 70
圖 4 39 SMX光催化分解趨勢圖 72
圖 4 40 SMX濃度與時間趨勢圖 72
圖 4 41 CBZ光催化分解趨勢圖 73
圖 4 42 SMX濃度與時間趨勢圖 73
圖 4 43 TP薄膜在不同pH下，SMX殘餘濃度與反應時間之趨勢圖 76
圖 4 44 TP薄膜在不同pH下，CBZ殘餘濃度與反應時間之趨勢圖 76
圖 4 45 TP-rGO3薄膜在不同pH下，SMX殘餘濃度與反應時間之趨勢圖 77
圖 4 46 TP-rGO3薄膜在不同pH下，CBZ殘餘濃度與反應時間之趨勢圖 77
圖 4 47 TP-rGO5薄膜在不同pH下，SMX殘餘濃度與反應時間之趨勢圖 78
圖 4 48 TP-rGO5薄膜在不同pH下，CBZ殘餘濃度與反應時間之趨勢圖 78
圖 4 49 TP-rGO7薄膜在不同pH下，SMX殘餘濃度與反應時間之趨勢圖 79
圖 4 50 TP-rGO7薄膜在不同pH下，CBZ殘餘濃度與反應時間之趨勢圖 79
圖 4 51 TP-rGO10薄膜在不同pH下，SMX殘餘濃度與反應時間之趨勢圖 80
圖 4 52 TP-rGO10薄膜在不同pH下，CBZ殘餘濃度與反應時間之趨勢圖 80
圖 4 53 TP-rGO12薄膜在不同pH下，SMX殘餘濃度與反應時間之趨勢圖 81
圖 4 54 TP-rGO12薄膜在不同pH下，CBZ殘餘濃度與反應時間之趨勢圖 81
圖 4 55 TP、TP-rGO系列薄膜光觸媒於不同pH值與反應速率常數圖 82
圖 4 56 TP、TP-rGO系列薄膜光觸媒於不同pH值與反應速率常數圖 83
圖 4 57不同pH值下還原氧化石墨烯與反應速率常數關係圖 84
圖 4 58不同pH值下還原氧化石墨烯與反應速率常數關係圖 84
圖 4 59 TP、TP-rGO系列薄膜光觸媒於不同pH值與反應速率常數圖 87
圖 4 60 TP、TP-rGO系列薄膜光觸媒於不同pH值與反應速率常數圖 87
圖 4 61系列薄膜光觸媒在不同pH與反應速率常數關係圖 88
圖 4 62系列薄膜光觸媒在不同pH與反應速率常數關係圖 88
圖 4 63 TP SMX暗吸附實驗 90
圖 4 64 TP CBZ暗吸附實驗 90
圖 4 65 TP-rGO3 SMX暗吸附實驗 91
圖 4 66 TP-rGO3 CBZ暗吸附實驗 91
圖 4 67 TP-rGO5 SMX暗吸附實驗 92
圖 4 68 TP-rGO5 CBZ暗吸附實驗 92
圖 4 69 TP-rGO7 SMX暗吸附實驗 93
圖 4 70 TP-rGO7 CBZ暗吸附實驗 93
圖 4 71 TP-rGO10 SMX暗吸附實驗 94
圖 4 72 TP-rGO10 CBZ暗吸附實驗 94
圖 4 73 TP-rGO12 SMX暗吸附實驗 95
圖 4 74 TP-rGO12 CBZ暗吸附實驗 95
圖 4 75在pH 3條件下SMX與CBZ反應速率與還原氧化石墨烯關係圖 97
圖 4 76在pH 5條件下SMX與CBZ反應速率與還原氧化石墨烯關係圖 98
圖 4 77在pH 7條件下SMX與CBZ反應速率與還原氧化石墨烯關係圖 99
圖 4 78在pH 9條件下SMX與CBZ反應速率與還原氧化石墨烯關係圖 100
圖 4 79在pH 11條件下SMX與CBZ反應速率與還原氧化石墨烯關係圖 101
圖 4 80 在酸性條件下TP薄膜光觸媒與SMX反應機制 105
圖 4 81在酸性條件下 TP薄膜光觸媒與CBZ反應機制 106
圖 4 82在鹼性條件下 TP薄膜光觸媒與SMX反應機制 106
圖 4 83在鹼性條件下 TP薄膜光觸媒與CBZ反應機制 107
圖 4 84 TP-rGO薄膜光觸媒反應機制 108

 
表目錄
表 2 1 常見之PPCPs類別及藥品[Wamg et al., 2015] 14
表 2 2 不同事業單位排放廢水中新興污染物含量檢測結果 16
表 2 3環境水體中新興污染物檢測結果 17
表 2 4 CBZ之結構與基本資料[Jeones et al., 2002] 18
表 2 5 SMX之結構與基本資料[Nasuhoglu et al., 2011] 19
表 2 6固定化方法之優缺點比較 28
表 2 7還原氧化石墨烯/TiO2光觸媒對PPCPs的光催化作用 32
表 2 8製備複合材料合成技術比較 33
表 3 1薄膜光觸媒種類與代號 41
表 3 2實驗參數 42
表 4 1薄膜光觸媒接觸角分析彙整(LED) 67
表 4 2薄膜光觸媒接觸角分析彙整(UV) 70
表 4 3薄膜光觸媒在不同pH下降解SMX反應速率常數k (單位：hr-1) 82
表 4 4不同pH下系列薄膜光觸媒降解CBZ反應速率常數k(單位：hr-1) 83
表 4 5 pH 3條件下SMX與CBZ系列薄膜光觸媒反應速率常數k(單位：hr-1) 97
表 4 6 pH 5條件下SMX與CBZ系列薄膜光觸媒反應速率常數k(單位：hr-1) 98
表 4 7 pH 7條件下SMX與CBZ系列薄膜光觸媒反應速率常數k(單位：hr-1) 99
表 4 8 pH 9條件下SMX與CBZ系列薄膜光觸媒反應速率常數k(單位：hr-1) 100
表 4 9 pH 11條件下SMX與CBZ系列薄膜光觸媒反應速率常數k(單位：hr-1) 101
表 4 10 固定化光觸媒催化分解SMX文獻比較 102
表 4 11 固定化光觸媒催化分解CBZ文獻比較 103
表A 1系列薄膜光觸媒光催化分解SMX殘留時間濃度隨時間變化之彙整 A-1
表A 2系列薄膜光觸媒光催化分解SMX殘留時間濃度隨時間變化之彙整 A-1
表A 3系列薄膜光觸媒光催化分解SMX殘留時間濃度隨時間變化之彙整 A-2
表A 4系列薄膜光觸媒光催化分解SMX殘留時間濃度隨時間變化之彙整 A-2
表A 5系列薄膜光觸媒光催化分解SMX殘留時間濃度隨時間變化之彙整 A-3
表A 6系列薄膜光觸媒光催化分解CBZ殘留時間濃度隨時間變化之彙整 A-3
表A 7系列薄膜光觸媒光催化分解CBZ殘留時間濃度隨時間變化之彙整 A-4
表A 8系列薄膜光觸媒光催化分解CBZ殘留時間濃度隨時間變化之彙整 A-4
表A 9系列薄膜光觸媒光催化分解CBZ殘留時間濃度隨時間變化之彙整 A-5
表A 10系列薄膜光觸媒光催化分解CBZ殘留時間濃度隨時間變化之彙整 A-5
表B 1薄膜光觸媒吸附實驗SMX殘餘濃度隨時間變化之彙整 (pH= 3) B-1
表B 2薄膜光觸媒吸附實驗SMX殘餘濃度隨時間變化之彙整 (pH= 5) B-1
表B 3薄膜光觸媒吸附實驗SMX殘餘濃度隨時間變化之彙整 (pH= 7) B-2
表B 4薄膜光觸媒吸附實驗SMX殘餘濃度隨時間變化之彙整 (pH= 9) B-2
表B 5薄膜光觸媒吸附實驗SMX殘餘濃度隨時間變化之彙整 (pH= 11) B-3
表B 6薄膜光觸媒吸附實驗CBZ 殘餘濃度隨時間變化之彙整 (pH= 3) B-3
表B 7薄膜光觸媒吸附實驗CBZ 殘餘濃度隨時間變化之彙整 (pH= 5) B-4
表B 8薄膜光觸媒吸附實驗CBZ 殘餘濃度隨時間變化之彙整 (pH= 7) B-4
表B 9薄膜光觸媒吸附實驗CBZ 殘餘濃度隨時間變化之彙整 (pH= 9) B-5
表B 10薄膜光觸媒吸附實驗CBZ 殘餘濃度隨時間變化之彙整 (pH= 11) B-5

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