臺灣博碩士論文加值系統

惡臭問題已成為社會環境問題，其中二甲基硫（DMS, C2H6S）的臭味閾值約於0.6-40 ppb，對眼睛、皮膚和呼吸系統具有刺激性。DMS排放的人為來源主要來自造紙廠、廢水處理廠、釀酒廠和畜牧場。
在降解DMS的許多方法中，光觸媒氧化是一種成本較低，耗能低和對環境友善的技術。二氧化鈦（TiO2）是目前被廣泛應用於光催化的半導體，然而其較寬之帶隙（3.2 eV）使其大部分的吸收波長落於紫外光範圍，且其光生電子空穴對會有較高複合率，限制其光催化效率。
本研究將透過摻雜硫、氮和石墨烯改質二氧化鈦，以溶熱法製作成複合奈米材料，期望能改善二氧化鈦本身吸收可見光之限制。TGA的結果可驗證還原氧化石墨烯的製備成功。由TEM結果可知二氧化鈦複合光觸媒為顆粒狀。從UV-visible光譜的結果可得知摻雜硫、氮和石墨烯於二氧化鈦中可增加可見光的吸收強度。XPS，FTIR和Raman光譜顯示在二氧化鈦複合光觸媒合成時，通過引入含氧官能基團產生了新的化學缺陷和鍵結，進一步提高了光催化效果。由XRD，SEM和BET結果顯示，在摻雜還原氧化石墨烯後，二氧化鈦複合光觸媒的晶體尺寸減小。二氧化鈦顆粒會附著在還原氧化石墨烯表面上或夾在還原氧化石墨烯層之間，促進了比表面積的增加。雖然還原氧化石墨烯可以提高光催化效率，但過量的摻雜可能會造成光遮蔽現象導致光催化活性降低。本研究中，0.1wt％還原氧化石墨烯是最佳摻雜量，在PL實驗中也應證了其為電子電洞對再結合率最低之材料。
在操作參數實驗中，相對濕度的增加會導致DMS的轉代率降低，這可能是由於水蒸氣和DMS的競爭吸附。溫度的增加會導致轉代率增加，可能是因為光催化反應的動力增加和光催化劑表面上吸附的水的減少。增加DMS的進流濃度會導致轉化率降低，可能是因為DMS分子之間發生競爭吸附。停留時間減少導致轉化率降低，可能是由於羥基自由基和DMS之間發生的碰撞頻率降低。Langmuir-Hinshelwood模型4最適合本研究之反應動力，代表水蒸氣和DMS具有競爭性吸附。根據FTIR分析結果，發現DMS降解會產生SO2，CO2，DMDS，DMSO，DMSO2、CO和MSA等之反應路徑。

Malodour issues have become a socio-environmental concern. Dimethyl sulfide (DMS, C2H6S) is an odorous pollutant with low odor threshold value of 0.6–40 ppb and is an irritant to the eyes, skin, and respiratory system. Anthropogenic sources of DMS emissions mainly come from paper pulping, wastewater treatment processes, distillery and livestock farm.
Among many methods in DMS degradation, photocatalytic oxidation is a suitable technology with advantages of cheaper cost, low energy consumption and environmental friendliness. Titanium dioxide (TiO2) is most widely used in photocatalytic applications. However, the wide band gap (3.2 eV) restricts its efficiency by causing its mainly absorption within the UV range of the spectrum and higher recombination rate of photogenerated electron-hole pairs.
To improve the performance of the photocatalysts, sulfur, nitrogen and graphene were chosen to dope into TiO2 by solvothermal method. The results of TGA confirms the successful preparation of reduced graphene oxide. Their particle morphologies of the photocatalysts are shown in TEM result. The UV-visible absorption spectrum indicates that the doping process can improve visible light absorption intensity and reduce the band gap. The XPS, FTIR and Raman spectra show that new chemical defect and bonding are produced by introducing oxygen-containing functional groups when synthesis of the reduced graphene oxide (rGO)/S0.05N0.1TiO2 composite, further enhance the photocatalytic effect. The XRD, SEM and BET results show that the decreasing crystallite size of rGO/S0.05N0.1TiO2 is formed after introducing the graphene sheets. The TiO2 particles are attached to the rGO surface and interpose between the rGO layers. Although rGO can enhance the photocatalytic efficiency, excess rGO could shield the light. In this study, 0.1 wt% rGO is the best doping amount. In PL analysis, it also shows the lowest recombination rate.
In operating parameters tests, the increasing relative humidity results in decreasing conversion rate. It may be due to the competitive adsorption of water vapor and DMS. The conversion rate increases with an increase of operating temperature due to the increasing kinetics of photocatalytic reaction and the reduction of water adsorbed on the photocatalyst surface. Increasing the influent concentration of DMS results in a decrease in the conversion because of the competitive adsorption occurs between the DMS molecules. The decreasing residence time leads to lower conversion. It may be due to the decreasing collision frequency between the hydroxyl radicals and DMS. Langmuir-Hinshelwood model 4 is best suited to the kinetics of this study, the water vapor and DMS have competitive adsorption. According to the FTIR analysis, DMS degradation has been found to generate SO2, CO2, DMDS, DMSO, DMSO2, CO, and MSA through various reaction pathways.

摘要 II
Abstract III
致謝 V
CONTENT VII
LIST OF TABLES XI
LIST OF FIGURE XIII
CHAPTER 1 INTRODUCTION 1
1-1Motivation 1
1-2 Objectives 3
CHAPTER 2 LITERATURES SURVEY 5
2-1 Introduction of air pollutants 5
2-1.1 Reduced sulfur compounds (RSCs) 6
2-1.2 Introduction of DMS 6
2-2 Control technologies of air pollutants 9
2-3 Photocatalysis 11
2-3.1 Photocatalyst 11
2-3.2 Photocatalysis principle 12
2-3.3 Preparation method of photocatalyst 17
2-4 Titanium dioxide 20
2-4.1 Physical and chemical properties 20
2-4.2 Application of TiO2 22
2-4.3 Modification of TiO2 24
2-5 Graphene 26
2-5.1 Synthesis of graphene 27
2-5.2 Application of TiO2 coupled with graphene 31
2-6 Chemical reaction kinetics 32
2-6.1 Plug flow reactor 34
2-6.2 Langmuir-Hinshelwood (L-H) model 36
2-6.3 Arrhenius equation 38
CHAPTER 3 MATERIAL AND METHODS 40
3-1 Research scope 40
3-2 Experimental materials and equipments 42
3-2.1 Chemicals and gases 42
3-2.2 Reactor and experimental set-up 42
3-3 Experimental methods 47
3-3.1 Preparation of graphite oxide 47
3-3.2 Preparation of photocatalysts 49
3-3.3 Preparation of photocatalytst film 51
3-3.4 The stability and photolysis of simulated DMS gas system 51
3-3.5 Calibration curve 51
3-4 Characteristics of Photocatalysts 52
3-4.1 Thermogravimetric/ differential thermal analysis (TG/DTA) 52
3-4.2 X-ray powder diffraction spectroscopy (XRD) 53
3-4.3 Scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS) 54
3-4.4 Transmission electron microscopy (TEM) 54
3-4.5 Fourier transform infrared spectroscopy (FTIR) 55
3-4.6 UV-visible spectrometry 55
3-4.7 X-ray photoelectron spectroscopy (XPS) 55
3-4.8 Brunauer–Emmett–Teller (BET) 56
3-4.9 Raman spectroscopy 59
3-4.10 Photoluminescence (PL) 59
3-5 Gas Chromatography - Flame Photometric Detector (GC-FPD) 59
3-6 Kinetic study 60
3-7 Byproduct analysis by FTIR 60
CHAPTER 4 RESULTS AND DISCUSSION 61
4-1 Characteristics of photocatalysts 61
4-1.1 Elemental analysis 61
4-1.2 Scanning electron microscopy (SEM) with energy dispersive X-ray ectroscopy (EDS) 61
4-1.3 Transmission electron microscopy (TEM) 70
4-1.4 Thermogravimetric/differential thermal analysis (TG/DTA) 78
4-1.5 X-ray powder diffraction spectroscopy (XRD) 83
4-1.6 UV-visible spectrometry 88
4-1.7 Photoluminescence (PL) 90
4-1.8 Raman spectroscopy 92
4-1.9 Fourier transform infrared spectroscopy (FTIR) 95
4-1.10 X-ray photoelectron spectroscopy (XPS) 98
4-1.11 Brunauer–Emmett–Teller (BET) 111
4-2 Activity test of Photocatalysts 115
4-2.1 Comparison with commercial graphene 118
4-3 Operating parameter test of Photocatalysts 119
4-3.1 Effect of inlet DMS concentration 119
4-3.2 Effect of relative humidity 121
4-3.3 Effect of temperature 125
4-3.4 Effect of residence time 127
4-4 Kinetic Models 129
4-4.1 Langmuir-Hinshelwood Model 129
4-5 Mechanisms of photocatalytic reaction 135
4-5.1 Analysis of byproducts by FTIR 135
4-5.2 Mineralization extent analysis 142
4-5.3 Reaction pathways 143
CHAPTER 5 CONCLUSION AND SUGGESTION 148
5-1 Conclusion 148
5-2 Suggestion 149
REFERENCE 150

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