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研究生： 周仕涵
Chou, Shih-Han
論文名稱： 以S、N改質TiO2光觸媒在可見光下處理1,2-二氯乙烷之研究
Photocatalytic Degradation of 1,2-dichloroethane Under Visible Light with S- or N-doped TiO2 Photocatalysts
指導教授： 朱信
Chu, Hsin
學位類別： 碩士
Master
系所名稱： 工學院 - 環境工程學系
Department of Environmental Engineering
論文出版年： 2010
畢業學年度： 98
語文別： 中文
論文頁數： 189
中文關鍵詞： 1,2-二氯乙烷 、光觸媒 、可見光光催化 、N改質光觸媒 、S改質光觸媒
外文關鍵詞： 1,2-dichloroethane, Titanium dioxide (TiO2), Visible light photocatalysis, N-doped catalyst, S-doped catalyst
相關次數： 點閱：130  下載：2 
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    • 1,2-二氯乙烷(1,2-dichloroethane, DCE)為工業上常用的有機溶劑，但如果在使用過程中釋放到空氣中，與人體接觸或經人體吸入，將對健康造成危害，亦造成環境污染。光催化反應具有氧化能力強、處理效率高及操作程序簡單等優點，成為具有潛能的控制空氣污染技術。
    本實驗利用溶膠凝膠法製備而成TiO2光觸媒，並以N或S改質/摻雜，期望藉由改質來提高TiO2光觸媒在可見光下降解1,2-二氯乙烷的效率。同時探討批次實驗中，不同改質/摻雜物質對光觸媒光催化活性的影響，並藉由各種輔助實驗，如UV-Visible、XRD、BET、XPS等精密儀器來研究光觸媒吸光度、晶相變化、粒徑分佈、化學鍵結等物化性質，藉以探討與1,2-二氯乙烷降解效率之關連性。
    研究結果顯示，經由N或S改質TiO2光觸媒(N/TiO2、S/TiO2)能使吸收波長往可見光波長位移且光觸媒能隙(band gap)能有效下降；在XRD分析結果得知，當鍛燒溫度為500°C時自製TiO2光觸媒晶相大部分為anatase，另有部分rutile晶相產生。經過N、S改質/摻雜的TiO2光觸媒，anatase晶相比例明顯增加，而經S改質的TiO2粒徑明顯變小。
    在日光照射下之光催化實驗中，光觸媒塗佈量為0.6 g，改質TiO2光觸媒處理1,2-二氯乙烷的轉化率分析可發現，經過改質後的TiO2其轉化效率皆大幅提升，以S/Ti = 10 mol%之光觸媒表現最佳，平均降解速率為55.3 nmol/min/g，其次是N/Ti = 20 mol%，為43.2 nmol/min/g。結果顯示，S的含量越高，在光催化實驗中活性越好。
    從結果得知，N改質的TiO2光觸媒所含的rutile比例越高，其光催化活性則越差。

    1,2-dichloroethane is widely used as organic solvents in industrial processes. While 1,2-dichloroethane evaporates, it will cause environmental pollution and harm to human health. Photocatalytic reaction with its fast oxidation rate, high decomposition rate, and simple procedures now has become one of novel technologies to degrade organic solvents and has been applied widely in relative researches.
    In this study, TiO2 was prepared by sol-gel method and doped with N or S (N/TiO2 or S/TiO2). The photocatalytic decomposition rate of 1,2-dichloroethane under visible light condition was expected to increase via doping. Additionally, the physical and chemical properties of the photocatalysts such as adsorbance spectrum, crystallinity, particle size, and chemical bonding, measured by UV-Visible, XRD, BET and XPS, respectively, were obtained for a better understanding to the reaction of 1,2-dichloroethane decomposition rate.
    The UV-Visible spectra analysis indicates that the adsorbance wavelength of N/TiO2 or S/TiO2 became closer to the visble light, resulting in the narrower band gap. The XRD pattern of TiO2 which was calcined at 500°C shows the coexistence of the crystal forms of anatase and rutile. By doping with N or S, the content of anatase obviously increased; moreover, the particle size of S/TiO2 was smaller than pure TiO2.
    The photocatalytic degradation of 1,2-dichloroethane under fluorescent light was further studied using N/TiO2 and S/TiO2. The experimental results showed 1,2-dichloroethane conversion increased in N/TiO2 and S/TiO2 photocatalysts. It was found that S/TiO2 = 10 mol% achieved the greatest performance, and the average 1,2-dichloroethane conversion rate is 55.3 nmol/min/g. Following is N/TiO2 = 20 mol%, the average 1,2-dichloroethane conversion rate is 43.2 nmol/min/g. The higher S doping content, the better the photocatalytic decomposition efficiency. On the other hand, for N/TiO2 photocatalysts, the higher content of rutile, the worse the 1,2-dichloroethane decomposition efficiency.

    摘要 A Abstract C 目錄 I 表目錄 IV 圖目錄 V 第一章 前言 1 1-1 研究動機 1 1-2 研究目的 5 第二章 文獻回顧 7 2-1 VOCs的特性及影響 7 2-1.1 VOCs的定義及來源 7 2-1.2 含氯揮發性有機物(Cl−VOCs)的使用狀況 9 2-2 1,2-二氯乙烷的特性與處理方法 14 2-2.1 1,2-二氯乙烷的特性 14 2-2.2 1,2-二氯乙烷之處理方法 18 2-3 光觸媒 19 2.3.1 光觸媒之物理意義 19 2.3.2 能隙(Band gap) 20 2-4 光催化原理 23 2-5 二氧化鈦的基本特性 28 2-6 光觸媒的製備 30 2-6.1 含浸法(Impregnation) 30 2-6.2 溶膠-凝膠法(Sol-gel) 30 2-6.3 物理氣相沉積法(Physical Vapor Deposition) 32 2-6.4 化學氣相沉積法(Chemical Vapor Deposition, CVD) 33 2-6.5 真空濺鍍法(Sputtering) 33 2-6.6 綜合比較 34 2-7 二氧化鈦的改質 35 2-7.1 添加金屬原子 36 2-7.2 添加金屬離子 38 2-7.3 添加非金屬元素 40 2-7.4 表面敏化 45 2-7.5 加入其它種半導體 46 2-8 二氧化鈦光觸媒塗佈方法 48 2-8.1 浸漬塗佈方法 48 2-8.2 旋轉塗佈法 49 2-9 光觸媒降解VOCs之反應動力 51 2-9.1 柱流式反應器基礎理論 51 2-9.2 微分型反應器 53 2-9.3 觸媒異相反應模式 54 第三章 研究方法與實驗設備 61 3-1 研究方法 61 3-2 預備實驗 63 3-2.1 光觸媒之製備 63 3-2.2 光觸媒膜之製備 65 3-2.3 檢量線的製作 67 3-2.4 光催化之背景實驗 68 3-3 實驗材料與設備 69 3-3.1 試藥與氣體 69 3-3.2 實驗系統裝置 71 3-3.3 分析儀器操作條件與原理 77 第四章 結果與討論 86 4-1 自製TiO2光觸媒之特性分析 86 4-1.1 熱重分析 86 4-1.2 X-射線繞射分析 88 4-1.3 FTIR及TG-IR分析 90 4-1.4 TiO2光觸媒之TEM分析 93 4-1.5 TiO2光觸媒之SEM、Mapping、EDS分析 94 4-1.6 TiO2光觸媒之XPS分析 98 4-1.7 TiO2光觸媒之BET比表面積極孔洞分佈分析 100 4-2 自製N/TiO2光觸媒之特性分析 102 4-2.1 熱重分析 102 4-2.2 X-射線繞射分析 105 4-2.3 FTIR及TG-IR分析 109 4-2.4 UV-Visible分析 110 4-2.5 N/TiO2光觸媒之TEM分析 112 4-2.6 N/TiO2光觸媒之SEM、Mapping、EDS分析 113 4-2.7 N/TiO2光觸媒之XPS分析 118 4-2.8 BET比表面積及孔洞分佈分析 121 4-3 自製S/TiO2光觸媒之特性分析 124 4-3.1 熱重分析 124 4-3.2 X-射線繞射分析 127 4-3.3 FTIR及TG-IR分析 131 4-3.4 UV-Visible分析 132 4-3.5 S/TiO2光觸媒之TEM分析 134 4-3.6 S/TiO2光觸媒之SEM、Mapping、EDS分析 136 4-3.7 S/TiO2光觸媒之XPS分析 141 4-3.8 BET比表面積及孔洞分佈分析 145 4-3.9 S/TiO2光觸媒之EA分析 148 4-4 光觸媒在可見光下降解1,2-二氯乙烷之光催化實驗 149 4-4.1 自製TiO2光觸媒降解1,2-二氯乙烷之實驗 149 4-4.2 以不同N/Ti比例光觸媒降解1,2-二氯乙烷之實驗 150 4-4.3 以不同S/Ti比例光觸媒降解1,2-二氯乙烷之實驗 152 4-5 自製S/TiO2光觸媒之動力分析 154 4-5.1 Langmuir-Hinshelwood Model 154 4-5.2 Mars & van Krevelen Model 164 第五章 結論與建議 168 5-1 結論 168 5-2 建議 171 參考文獻 172 附錄 185

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