氮改質煅燒牡蠣殼提升水中亞甲基藍染料 吸附和光催化降解之研究

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吳佩珊(PEI-SHAN WU) 查詢紙本館藏

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論文名稱

氮改質煅燒牡蠣殼提升水中亞甲基藍染料吸附和光催化降解之研究
(Nitrogen-doped Calcined Oyster Shells as Adsorbents and Photocatalysts for the Removal of Methylene Blue Dye in Water)

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至系統瀏覽論文 (2027-1-31以後開放)

摘要(中)

本研究的目的是以亞甲基藍(Methylene blue, MB)染料作為目標污染物，牡蠣殼煅燒製備的生物氧化鈣(biogenic calcium oxide)作為光觸媒，進行 MB 的吸附和光催化氧化降解研究。首先以高溫煅燒(Calcined)鹼洗後的牡蠣殼(uncalcined oyster shell, UOS)，製備成氧化鈣(heated oyster shell, HOS)，再加入 2%(w/w)、5%(w/w)、 10%(w/w)尿素(urea)以溶膠凝膠(sol-gel method)進行表面改質，再將此粉體於高溫爐中以 600°C 煅燒 2 小時，合成氮摻雜氧化鈣(2%N-HOS、5%N-HOS、10%N-HOS)。從 BET 比表面分析得知，比表面積從 2.9370 m2 g-1(UOS)提高至 72.3785 m2 g-1(HOS) 和 71.4240 m2 g-1(2%N-HOS)。XRD 及 EDS 結果證明氮元素成功參雜在 HOS 表面; 以 UV-vis 量測及 Talc plot 計算氮參雜氧化鈣粉體能隙值介在 4.37 - 4.45eV。
在光催化過程添加過氧化氫(hydrogen peroxide, H2O2)，可以提高有機污染物的降解效率，因為它還有多種優點，包括提高氫氧自由基(hydroxyl radical, •OH)量、防止電子-電洞再結合。本研究探討在紫外光線(ultraviolet light, UV)、可見光(visible light, vis)及暗反應下，添加過氧化氫，氧化鈣對亞甲基藍(Methylene blue, MB)染料之光催化降解效率。由可見光光催化實驗結果顯示，氮摻雜氧化鈣因帶隙距縮短，可有效利用長波長能量小的可見光波段，故在 MB 濃度 10 mg L-1、添加 0.84 g L-1 的 2%N- HOS、H2O2 (0.23%)(將 H2O2 溶液添加在亞甲基藍染料中，經計算得出濃度約為 0.23%)、反應溫度為 60°C下，在反應時間在 120 min，2%N-HOS 具有最佳的光降解效率，去除率達 99.8%。由氧化鈣及氮摻雜氧化鈣在添加過氧化氫對 MB 之動力實驗結果顯示，反應遵循一階動力學模式，表示反應時間對降解 MB 為正相關。

摘要(英)

The primary objective of this research is to investigate the adsorption and photocatalytic oxidation degradation of Methylene Blue dye using nitrogen-doped calcium oxide (N-HOS) as the photocatalyst. The procedure involves the initial conversion of oyster shells through calcination and alkali washing to produce heated oyster shell (HOS). Subsequently, surface modification is accomplished by introducing urea in varying proportions (2% (w/w), 5% (w/w), and 10% (w/w)) via the sol-gel method. The resulting powder undergoes high- temperature annealing at 600°C for 2 hours, resulting in the synthesis of nitrogen-doped calcium oxide (2%N-HOS, 5%N-HOS, 10%N-HOS). BET surface area analysis illustrates a substantial augmentation in surface area, progressing from 2.9370 m2 g-1 (UOS) to 72.3785 m2 g-1 (HOS) and 71.4240 m2 g-1 (2%N-HOS). Further substantiating this, XRD and EDS analyses confirm the successful integration of nitrogen onto the HOS surface. The evaluation of energy bandgap values, conducted through UV-visible measurements and Tauc plots revealed a bandgap energy of 4.5 eV for calcium oxide, whereas the bandgap of nitrogen- doped calcium oxide ranged from 4.37 to 4.45 eV. Nitrogen doping effectively reduced the bandgap, thereby enhancing light absorption capabilities.
To intensify the concentration of hydroxyl radicals (•OH) during photocatalytic reactions, hydrogen peroxide (H2O2) is introduced into the aqueous solution. Subsequent assessments encompass the investigation of the photocatalytic degradation efficiency of Methylene Blue (MB) under different conditions, encompassing ultraviolet light (UV), visible light (vis), and dark adsorption. The experiments pertaining to visible light photocatalysis underscore the multifaceted attributes of nitrogen-doped calcium oxide, highlighting its competence in MB adsorption and visible light photocatalysis. Specifically,
II
under conditions characterized by a 10 mg L-1 MB concentration, 0.84 g L-1 of 2%N-HOS, and 0.23% H2O2 (calculated concentration), executed at a reaction temperature of 60°C, and sustained for a duration of 120 minutes, 2%N-HOS emerges as the most proficient photocatalyst, delivering a remarkable removal efficiency of 99.8%.

關鍵字(中)

★ 牡蠣殼
★ 氧化鈣
★ 氮摻雜
★ 紫外/可見光催化氧化法
★ 過氧化氫
★ 亞甲基藍

關鍵字(英)

論文目次

摘要 ............................................................................................................................................ I Abstract...................................................................................................................................... II 致謝 ..........................................................................................................................................IV 目錄 ........................................................................................................................................... V 圖目錄 ................................................................................................................................... VIII 表目錄 ....................................................................................................................................... X 第壹章前言 ...............................................................................................................................1
1.1 研究緣起及背景 ..............................................................................................................1 1.2 研究目的 ..........................................................................................................................2 1.3 研究創新性 ......................................................................................................................3
第貳章文獻回顧 .......................................................................................................................4 2.1 牡蠣殼(Oyster shell) ........................................................................................................4 2.2 氧化鈣(Calcium Oxide, CaO) ..........................................................................................5 2.3 染整產業污染水體 ..........................................................................................................6 2.4 染料 ..................................................................................................................................7
2.4.1 亞甲基藍(Methylene blue, MB) .......................................................................8
2.4.2 染色原理 ...........................................................................................................9 2.5 光觸媒特性 ....................................................................................................................11 2.6 氮摻雜氧化鈣復合光觸媒 ............................................................................................11
2.6.1 摻雜非金屬氮元素 .........................................................................................12 2.6.2 以尿素作為氮元素摻雜來源 .........................................................................13 2.6.3 非金屬摻雜方法 .............................................................................................15
2.7 高級氧化處理程序 ........................................................................................................16 2.7.1 光催化氧化法(Photocatalytic Oxidation, PCO)機制.....................................16 2.7.2 氮摻雜光觸媒對光催化反應機制 .................................................................18 2.7.3 染料分子受光催化氧化反應之程序 .............................................................19 2.7.4 過氧化氫直接氧化 .........................................................................................20 2.7.5 氫氧自由基(hydroxyl radical) 氧化 ...............................................................20
2.8 影響光催化氧化程序之影響因子 ................................................................................22 2.8.1 光觸媒的特性 .................................................................................................22 2.8.2 光源強度和光照時間 .....................................................................................23 2.8.3 水溶液酸鹼值(pH 值) ..................................................................................... 23 2.8.4 添加劑 .............................................................................................................24
V
2.8.5 溫度和壓力 .....................................................................................................25 2.9 光觸媒重複試驗 ............................................................................................................25 2.10 光催化降解模式之探討 ..............................................................................................25
2.10.1 染料濃度測定(Determination of dye concentration)....................................25 2.10.2 動力學模式(Kinetic model)..........................................................................26 2.10.3 能隙(Band gap) .............................................................................................27
第參章研究架構與規劃 .........................................................................................................29 3.1 研究架構與流程 ............................................................................................................29 3.2 實驗材料 ........................................................................................................................31
3.2.1 牡蠣殼來源 .....................................................................................................31 3.3 氧化鈣製備及氮改質方法 ............................................................................................31 3.3.1 氧化鈣製備 .....................................................................................................31 3.3.2 氮摻雜氧化鈣製備 .........................................................................................31 3.4 亞甲基藍溶液配置 ........................................................................................................33 3.5 光催化降解實驗 ............................................................................................................33 3.5.1 空白背景實驗 .................................................................................................34 3.5.2 吸附實驗 .........................................................................................................36 3.5.3 光催化實驗 .....................................................................................................37 3.5.4 重複實驗 .........................................................................................................39 3.6 實驗藥品及設備 ............................................................................................................40 3.6.1 實驗藥品 .........................................................................................................40 3.6.2 實驗設備 .........................................................................................................41 3-7 材料特性分析量測儀器 ................................................................................................ 42 第肆章研究結果與討論 .........................................................................................................46 4.1 光觸媒表徵物化特性分析 ............................................................................................46 4.1.1 SEM 分析 ........................................................................................................ 46 4.1.2 EDS 分析.........................................................................................................49 4.1.3 BET 分析.........................................................................................................51 4.1.4 XRD 分析........................................................................................................53 4.1.5 FT-IR 分析 ......................................................................................................54 4.1.6 XPS 分析 ......................................................................................................... 55 4.1.7 光譜特性分析 .................................................................................................58 4.2 光觸媒對 MB 之光催化降解實驗................................................................................59 4.2.1 空白背景實驗 .................................................................................................59 4.2.2 暗反應吸附實驗 .............................................................................................60
VI

4.2.3 氧化鈣之光催化實驗 .....................................................................................61 4.2.4 不同操作變因下，對 MB 降解的研究 .........................................................65 4.2.5 氮摻雜氧化鈣對 MB 降解之研究 .................................................................73 4.2.6 光催化之降解動力學 .....................................................................................85 4.2.7 MB 在可見光光催化過程中，紫外-可見光吸收光譜及分解副產物的分析 .................................................................................................................................. 90
4.3 相關文獻之探討 ............................................................................................................98 第伍章結論與建議 ...............................................................................................................101 5.1 結論 ..............................................................................................................................101 5.2 建議 ..............................................................................................................................103 參考文獻 ................................................................................................................................105 附錄一紫外可見光光譜儀 ..................................................................................................117 附錄二學位考試委員意見回覆表 ......................................................................................118

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指導教授

林伯勳

審核日期

2024-1-23

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