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研究生： 魏伯諭
Wei, Po-Yu
論文名稱： 多壁奈米碳管／環氧樹脂碳化複合材料對二價銅離子吸附能力研究
Cu(II) adsorption by carbonized multi-walled carbon nanotubes/epoxy composites
指導教授： 徐文光
Hsu, Wen-Kuang
口試委員: 郭信甫
黃淑娟
學位類別： 碩士
Master
系所名稱： 工學院 - 材料科學工程學系
Materials Science and Engineering
論文出版年： 2012
畢業學年度： 100
語文別： 中文
論文頁數： 94
中文關鍵詞： 多壁奈米碳管 、環氧樹脂 、吸附 、二價銅離子 、電容去離子法
外文關鍵詞： Carbon nanotubes, Epoxy, Adsorption, Cu(II), Capacitive deionization
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    • 　　本研究以簡單的方式製作多壁奈米碳管複合物，成功地去除溶液中的二價銅離子(Cu2+)，同時解決奈米碳管難以回收的缺點。
    　　三種比例之多壁奈米碳管(MWCNTs)混合環氧樹脂(Epoxy resin)後再經碳化(Carbonization)和酸化(Acidification)改質步驟，用來吸附溶液中二價銅離子。吸附實驗分為兩部分：以粉末狀樣品做吸附；另一部分是使用薄板狀樣品以電容去離子技術(capacitive deionization, CDI)去除溶液中Cu(II)。同時量測樣品各種性質，探討比表面積、平均孔徑、電阻率、石墨化程度、表面形貌和官能基與吸附效率之間的關係。
    　　結果顯示，樣品經過酸化步驟，樣品電阻率大幅下降；比表面積下降；平均孔徑提升；極性官能基增加，使樣品由疏水性轉為親水性。粉末狀樣品以Langmuir等溫吸附模型估算其最大吸附容量為19.49 mg•g-1，而吸附現象較符合Freundlich模型。粉末樣品經過酸洗可重複利用。薄片樣品在施加1.2 V偏壓下，吸附容量可提升約3.5倍。溶液濃度低時，Cu(II)之去除機制為電雙層吸附及官能基離子交換；高濃度時，機制為電解硫酸銅溶液。經過再生步驟之薄板狀樣品，去除Cu(II)能力皆相近，但僅為初次使用之樣品的80 %左右。

    Carbonized multi-walled carbon nanotubes/epxoy composites are made to absorb Cu2+ in aqueous solution and CNTs are found retrievable after repeated experiments.
    Carbonized composites, consisting of multi-walled carbon nanotubes and epoxy resin in different ratios, are used to remove copper ions in the solution after carbonization and acidification processes. Adsorptive experiments are divided into two parts; first, the samples powdered and are used as Adsorbents; second, samples are made as thin films and ionic absorption is carried out using CDI technology. Samples are also characterized in order to establish the relationship between sample structure and chemical treatments.
    Results show that acidification decreases resistivity of powdered samples and specific surface area whereas porosity and density of functional groups increase. Accordingly, samples change from hydrophobic into hydrophilic property and the maximum adsorption capacity of Cu(II) calculated by Langmuir model reaches 19.49 mg•g-1, fit better with Freundlich model than that of Langmuir model. Samples can be reused through regeneration procedure. In CDI adsorption experiment, the adsorption capacity of film samples increases by three-fold at applied 1.2 V between electrodes. The adsorption mechanism is found as a result of combined electrosorption and ion exchange at low concentration situation. At high concentration, adsorption of copper(II) sulfate proceeds through electrolysis and amount of removed ions from solution decreases to 80 % at the 1st run. Absorption curves become stabilized after the 1st regeneration process.

    摘要 I Abstract II 總目錄 IV 圖目錄 VIII 表目錄 XI 第一章 前言及研究動機 1 第二章 文獻回顧 3 2.1奈米碳管 (Carbon nanotubes, CNTs) 3 2.1.1 奈米碳管簡介及結構 3 2.1.2 奈米碳管的電性 5 2.1.3 奈米碳管去除水中重金屬離子之應用 8 2.1.4 奈米碳管的吸附機制 11 2.1.5 影響奈米碳管吸附金屬離子的因素 12 2.1.5.1 pH值 12 2.1.5.2 官能基 13 2.1.5.3 吸附劑劑量 14 2.1.5.4 離子強度 14 2.1.5.5 接觸時間和起始離子濃度 15 2.1.5.6 溫度 16 2.2 電容去離子技術 (Capacitive deionization, CDI) 22 2.2.1 簡介 22 2.2.2 奈米碳管於電容去離子技術之應用 24 2.3 環氧樹脂 (Epoxy resins) 26 2.3.1 簡介 26 2.3.2 奈米碳管及環氧樹脂複合材的熱性質 27 2.4 吸附理論 29 2.4.1 吸附類型 29 2.4.2 離子交換 (Ion exchange) 30 2.4.3 等溫吸附曲線 (Adsorption isotherm) 31 2.4.4 等溫吸附模型 34 2.4.4.1 Freundlich等溫吸附模型 34 2.4.4.2 Langmuir等溫吸附模型 35 第三章 實驗方法 37 3.1 實驗材料及儀器 37 3.2 實驗流程 39 3.3 實驗步驟 40 3.3.1 樣品製備 40 3.3.2 樣品測量 43 3.3.2.1 電阻率量測 43 3.3.2.2 比表面積及孔隙量測 (ASAP) 45 3.3.2.3 場發射掃描式電子顯微鏡 (FE-SEM) 45 3.3.2.4 拉曼光譜 (Raman Spectroscopy) 46 3.3.2.5 傅立葉轉換紅外線光譜 (FT-IR) 47 3.3.2.6 Boehm滴定法 48 3.3.2.7 感應耦合電漿原子發射光譜 (ICP-AES) 49 3.3.3 吸附實驗 50 3.3.3.1 Cu(II)溶液配製方式 50 3.3.3.2 粉末樣品吸附實驗 50 3.3.3.3 電容去離子實驗 51 第四章 結果與討論 55 4.1 碳化及酸化後樣品分析 55 4.1.1 電阻率分析 55 4.1.2 拉曼光譜分析 56 4.1.3 場發射掃描式電子顯微鏡分析 58 4.1.4 比表面積及孔隙分析 61 4.1.5 傅立葉轉換紅外線光譜分析 63 4.1.6 Boehm滴定法結果分析 66 4.2 樣品吸附能力分析 67 4.2.1 粉末樣品吸附能力分析 67 4.2.1.1 靜態吸附與動態吸附之比較 67 4.2.1.2 粉末樣品之等溫吸附模型 69 4.2.1.3 粉末樣品再生實驗 71 4.2.2 電容去離子實驗結果分析 73 4.2.2.1 有無施加偏壓對吸附容量之影響 73 4.2.2.2 吸附時間對吸附容量之影響 73 4.2.2.3 溶液起始濃度對吸附容量之影響 76 4.2.2.4 電容去離子再生實驗 78 第五章 結論 80 參考文獻 83

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