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研究生: 黃國徑
Huang, Guo-jing
論文名稱: 以濕式研磨法研製水滑石/尼龍6及水滑石/聚對苯二甲酸乙二酯奈米複合材料的研究
Preparation of LDHs/Nylon 6 and LDHs/PET nanocomposites by wet milling process
指導教授: 陳志勇
Chen, Chuh-Yung
學位類別: 碩士
Master
系所名稱: 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年: 2009
畢業學年度: 97
語文別: 中文
論文頁數: 69
中文關鍵詞: 濕式研磨法奈米複合材料水滑石
外文關鍵詞: Layered double hydroxides, Nanocomposites, Milling process
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  • 水滑石是一種容易製備的層狀材料,本文先利用共沉澱法合成硬脂酸根插層的有機化水滑石(LDH-S),並以FT-IR、XRD、ICP Mass、EA、TGA進行鑑定。再以濕式研磨分散法製備出高濃度(50%)的水滑石濃縮粒,經過XRD與SAXS的分析之後可知有機化水滑石LDH-S的層間距從原本的3.1nm增加到3.9nm以上,本研究再進一步將濕式研磨法處理過的水滑石濃縮粒與尼龍6(nylon 6)、聚對苯二甲酸乙二酯(PET)等高分子中進行分散,經過XRD、SAXS、TEM等分析發現水滑石呈現插層型態的分佈在高分子基材當中。從DSC的結果當中,發現水滑石會降低LDH-S/nylon 6與LDH-S/PET結晶的完整性,進而對結晶型態產生改變,亦降低結晶成長速率(k)。並透過氣體透過率的分析,發現水滑石的層板構造具有阻隔氣體穿透的能力。

    Layered double hydroxides (LDHs) are a class of readily synthesizable layered crystals. In this work, we synthesized organic stearate anion-modified MgAl-LDH (LDH-S) via the co-precipitation method. The organic-modified LDHs were characterized by FT-IR, XRD, ICP, and EA. The milling process was used to modify LDH-S by PL-101 or PL-102, and obtained high LDH-S concentration (50 wt%) hybrids. After the analysis of XRD and SAXS, the d-spacing was increased from 3.1nm to 3.9nm above. We blended these hybrids within polymer, such as nylon 6 & PET, to prepare LDH-S/nylon 6 and LDH-S/PET nanocomposites. The dispersion of LDH-S layers was characterized by XRD, SAXS, and TEM. It was found that intercalated nanocomposites were obtained by melt processing. The thermal property of these nanocomposites was characterized by DSC. From the DSC results, LDH-S layers affected the perfection of crystallization. As LDH-S contents increasing, the crystallization rate constant ( k ) was decreased. Also, we found that LDH-S layers in the nanocomposites can reduce the permeation of gas.

    中文摘要 英文摘要 誌謝 總目錄 表目錄 圖目錄 第一章 緒論…………………………………………………………1 1.1材料的發展與演變.…………………………………………………1 1.2研究動機………………………………………………………2 第二章 文獻回顧………………………………………………………4 2.1水滑石/高分子奈米複合材料…………………………………4 2.1.1水滑石的結構與特性…………………………………5 2.1.2水滑石的製備方法……………………………………8 2.1.3層狀無機物/有機高分子奈米複合材料的型態分類.10 2.1.4水滑石/高分子奈米複合材料的製備方法及相關文獻 …………………………………………………………12 2.2結晶動力學……………………………………………………17 第三章 實驗內容………………………………………………………21 3.1實驗藥品………………………………………………………21 3.2實驗儀器………………………………………………………22 3.3實驗步驟………………………………………………………23 3.3.1硬脂酸根插層有機化水滑石之合成…………………23 3.3.2製備助劑插層水滑石…………………………………24 3.3.3 LDH-S/Nylon 6 & LDH-S/PET奈米複合材料的製備24 3.4儀器分析方法…………………………………………………25 3.4.1 X-ray繞射分析(XRD) ………………………………25 3.4.2紅外線光譜分析(FT-IR) ……………………………25 3.4.3固態核磁共振分析(Solid-State NMR) ……………26 3.4.4感應耦合電漿質譜分析(ICP) ………………………26 3.4.5元素分析(EA) ………………………………………26 3.4.6穿透式電子顯微鏡(TEM) ……………….…………26 3.4.7微差掃描熱分析(非恆溫DSC) ………………………26 3.4.8微差掃描熱分析(恆溫DSC) …………………………27 3.5實驗流程………………………………………………………27 3.5.1實驗架構魚骨圖………………………………………27 3.5.2合成硬脂酸根插層有機水滑石LDH-S………………28 3.5.3 LDH-S/Nylon 6 & LDH-S/PET 奈米複材的製備…28 第四章 結果與討論……………………………………………………29 4.1有機水滑石的鑑定……………………………………………29 4.1.1有機水滑石之XRD鑑定………………………………29 4.1.2有機水滑石之FT-IR鑑定……………………………31 4.1.3有機水滑石之組成鑑定:ICP-Mass、EA & TGA……32 4.1.4有機水滑石的27Al NMR鑑定& TEM觀察……………33 4.2奈米複材的製備………………………………………………34 4.2.1製備助劑插層的LDH-S之結果分析…………………35 4.2.2 LDH-S/nylon 6奈米複合材料的製備………………36 4.2.2.1不同分散助劑對於水滑石在LDH-S/nylon 6複 材中分散型態的影響…………………………38 4.2.2.2 LDH-S/nylon 6奈米複材之熱分析與結晶型態 分析:恆溫 & 非恆溫DSC、POM觀察………44 4.2.3 LDH-S/PET奈米複合材料的製備……………………53 4.2.3.1 LDH-S/PET奈米複合材料的分散性質………53 4.2.3.2 LDH-S/PET奈米複合材料的熱性質與結晶性質 ………………………………………………57 第五章 結論……………………………………………………………64 參考文獻………………………………………………………………65

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