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完整後設資料紀錄
DC 欄位 | 值 | 語言 |
---|---|---|
dc.contributor.advisor | 林江珍(Jiang-Jen Lin) | |
dc.contributor.author | Jau-Yu Chiou | en |
dc.contributor.author | 邱昭諭 | zh_TW |
dc.date.accessioned | 2021-06-16T07:09:07Z | - |
dc.date.available | 2014-07-11 | |
dc.date.copyright | 2014-07-11 | |
dc.date.issued | 2014 | |
dc.date.submitted | 2014-07-08 | |
dc.identifier.citation | Chapter 1
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dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/57878 | - |
dc.description.abstract | 本論文探討黏土插層/脫層機制形成“黏土/高分子混成材料”之策略性研究與黏土含磷之難燃性衍生奈米複合材料與應用,研究內容主要分敘如下。
黏土插層/脫層機制形成黏土/高分子混成材料之策略性研究,係藉由聚醚胺(polyoxyalkylene-amines) 插層劑之親/疏水性質與末端基差異性,探討對層狀黏土有機化改質機制之影響。研究中發現在相同分子量之線性疏水鏈段聚醚胺 (polyoxypropylene-amines, POP-amines),一端末端基為甲基之 POP-M-amines,與雙端皆為胺基之 POP-D-amines 相比具有最大層間距擴張。由動態實驗發現,POP-M-amines進行黏土插層具有特殊之第二步插層現象,有別於一般插層劑經離子交換進入黏土層間(第一步插層)所觀察到有機量關鍵性插層 (critical intercalation);第二步插層,黏土之層間距與插層劑量成正比。此階段式插層現象,除了可達到天然黏土脫層型態外,進一步地,可利用此特殊插層機制,將有機化黏土做為奈米容器,把材料儲存於黏土層間之奈米空間,如原油吸附與回收、藥物釋放及相變化 (PCM) 材料 (如paraffin wax) 之包覆等。 高分子/黏土 (Polymer layered silicate, PLS) 奈米複合材具有優秀的機械性質、熱穩定性質與生物相容性質。關鍵技術在於親水性之黏土與疏水性高分子間之相容性。本研究,黏土含磷之難燃性衍生奈米複合材料與應用,係以合成 Phosphazene-poly(oxypropylene)-amines (HCP-D400) 為始,並依三種改質方式製得 HCP-D400/NSP、HCP-D400/MMT及HCP-D400/Na+-MMT 有機化黏土,並具有 lower critical aggregate temperature (LCAT) 之特殊性質。經由SEM-EDX、XRD 及 TEM 分析,發現 HCP-D400 與脫層之奈米矽片(NSP) 以物理摻混方式製備之 HCP-D400/NSP 於環氧樹酯中分散效果最佳。更進一步分析複合材料之熱穩定性,當添加 10wt% HCP-D400/NSP 於環氧樹酯,T¬¬10wt% 由 350 oC 增加至 447 oC,T¬¬10wt% 由 500 oC 增加至757 oC ,有效提升環氧樹酯熱裂解溫度 127 oC (T10wt%)與 257 oC (T¬¬80wt%)。限氧指數 (limit oxygen index, LOI) 則提升 7% 至 27%。研究中發現HCP-D400不僅可使奈米矽片均勻分散於環氧樹酯中,進一步的與奈米矽片產生協同作用 (synergistic effect),提升高分子材料之熱穩定性質。 | zh_TW |
dc.description.abstract | Layered silicate clays are natural crystallites and are well recognized for their organic intercalation for nanocomposite applications. In this study, a new mechanism is revealed by selection of hydrophobic polyetheramines with a poly(oxypropylene) (POP) backbone and a methyl terminus as the intercalation agent. Specifically, the monoamine with a molecular weight of 2000 g/mol widened the basal spacing of the layered sodium montmorillonite up to 74 A and further expansion to 84 A, 96 A, and 100 A by a second intercalation different from the ionic exchange reaction. Kinetic studies indicated that the first stage of intercalation occurred after a critical concentration of a monoamine, while the second stage had no critical concentration behavior. This two-step method shows the potentials for synthesizing suitable organoclay nanostructures for encapsulating phase change materials (PCM) and oil recovery from the spilt ocean. The exploration of the in-depth understanding of clay confinement chemistry leads the strategic design of new materials and oil recovery process.
We further synthesized the phosphazene-amine adduct of hexachlorocyclophosphazene (HCP) and poly(oxypropylene)-diamines of 400 g/mol molecular weight (D400) by amine/chloride substitution and triethylamine removal of HCl. Subsequently, the adduct HCP-D400 was physically mixed with exfoliated silicate platelets (SP) to prepare the HCP-D400/silicate hybrids (HCP-D400/SP). The HCP-D400/MMT (HCP-D400 intercalated Na+-MMT) and HCP-D400/Na+-MMT (HCP-D400 physically mixed with Na+-MMT) were also prepared for comparison with HCP-D400/SP. A more homogeneous silicate distribution HCP-D400/SP than the HCP-D400/MMT counterparts in epoxy nanocomposites was revealed by SEM-EDX, XRD, and TEM analyses. The epoxy nanocomposite with 10 wt% of HCP-D400/SP, HCP-D400/MMT, and HCP-D400 had a degradation temperature at 80 % weight loss (T80 wt%) of 757 oC, 712 oC, and 519 oC, respectively, in comparison with the 500 oC of the pristine epoxy system. Anti-flame test confirmed that the HCP-D400/SP epoxy nanocomposite had a higher limit oxygen index (LOI) of 27.0 % than the HCP-D400/MMT counterpart (24.0 %). The degree of exfoliating the layered clay into random silicate platelets is the predominant factor for the thermal stability enhancement. It is also demonstrated that the co-presence of phosphazene-amines and silicate platelets has a synergistic effect in improving the thermal behavior of the nanocomposites. | en |
dc.description.provenance | Made available in DSpace on 2021-06-16T07:09:07Z (GMT). No. of bitstreams: 1 ntu-103-D97549011-1.pdf: 6111836 bytes, checksum: ecb92c994f2c73b1a889663a4adde3ac (MD5) Previous issue date: 2014 | en |
dc.description.tableofcontents | Index
謝辭 i 中文摘要 iii Abstract iv Index vi List of Figures ix List of Tables xiv List of Schemes xv Chapter 1 Introduction of Intercalation and Exfoliation Mechanism of Clays and Applications of Clay Nanocomposites 1 1.1 Classification of nanomaterials 1 1.2 Natural nanomaterials with a layered structure 4 1.3 Mechanistic aspects of organic modification through the intercalation and exfoliation of clay 6 1.3.1 Covalent bonding between silicates and monomers 7 1.3.1.1 Sol-gel reaction 8 1.3.1.2 Atom transfer radical polymerization 9 1.3.2 Non-covalent bonding involving ionic exchange reaction 10 1.3.2.1 Ionic exchange reaction mechanism 11 1.3.2.2 Hydrogen bonding mechanism 20 1.3.2.3 Combined ionic exchange and hydrogen bonding mechanism 20 1.3.2.4 Chelation mechanism by amido acids/carboxylic acids 22 1.3.2.5 Mechanochemical intercalation mechanism 24 1.4 Clay/polymer nanocomposites 26 1.5 Flame retardant of polymer–layer silicate nanocomposites 28 1.6 References 29 Chapter 2 A Stepwise Mechanism for Intercalating Hydrophobic Organics into Multilayered Clay Nanostructures 37 2.1 Introduction 38 2.2 Experimental 40 2.2.1 Materials 40 2.2.2 Intercalation of Na+-MMT by amine-salts 41 2.2.3 Characterization and measurements 42 2.3 Results and Discussion 43 2.3.1 General intercalation of poly(oxyalkylene)-amines into the layers of MMT 43 2.3.2 Hydrophobic effect from the methyl termini of the POP-monoamines 46 2.3.3 The effect of a methyl versus an amino terminus 47 2.3.4 A stepwise mechanism by POP-M2000 to expand the layered clay 50 2.3.5 Encapsulating organics in the second stage of intercalation 51 2.4 Conclusion 54 2.5 References 55 Chapter 3 Fine Dispersion of Phosphazene-Amines and Silicate Platelets in Epoxy Nanocomposites and the Synergistic Fire-Retarding Effect 59 3.1 Introduction 60 3.2 Experimental 63 3.2.1 Materials 63 3.2.2 General procedures for the amine substitution of hexachlorocyclophosphazene 63 3.2.3 Exfoliation of layered silicate Na+-MMT into random nanoscale silicate platelets (NSP) suspended in water 64 3.2.4 Intercalation of Na+-MMT by HCP-D400-amine salts 65 3.2.5 The preparation of physically blended HCP-D400/Clay hybrids 65 3.2.6 Preparation of HCP-D400/clay epoxy nanocomposites 66 3.2.7 Characterization and instruments 66 3.3 Results and Discussion 68 3.3.1 Characterization of phosphazene-amine HCP-D400 68 3.3.2 Preparation and characterization of HCP-D400/NSP hybrids 68 3.3.3 Physical blending of HCP-D400/NSP in epoxy nanocomposites 71 3.3.4 Surface morphologies of the epoxy nanocomposites 74 3.3.5 Thermal stability and synergistic behavior of phosphazene and silicate platelet in epoxies 76 3.4 Conclusion 79 3.5 References 80 Chapter 4 Summary 83 Curriculum Vitae…. 87 | |
dc.language.iso | en | |
dc.title | 黏土插層/脫層機制之策略性研究與黏土/磷難燃性奈米複合材料之應用 | zh_TW |
dc.title | Intercalation Strategies of Synthesizing Clay/Polymer Hybrids and Clay/Phosphazene Nanocomposites for Fire-Retarding and the Synergistic Effect | en |
dc.type | Thesis | |
dc.date.schoolyear | 102-2 | |
dc.description.degree | 博士 | |
dc.contributor.oralexamcommittee | 謝國煌(Kou-Huang Hsieh),邱文英(Wen-Yin Chiu),蔣見超(Raymond Chien-Chao Tsiang),戴憲弘(Shenghong A. Dai),郭炳林(Ping-Lin Kuo) | |
dc.subject.keyword | 黏土插層/脫層機制,階段式插層,奈米容器,奈米複合材,熱穩定性, | zh_TW |
dc.subject.keyword | intercalation mechanism,stepwise intercalation,phosphazene-amines,flame retardant,nanocomposites, | en |
dc.relation.page | 89 | |
dc.rights.note | 有償授權 | |
dc.date.accepted | 2014-07-08 | |
dc.contributor.author-college | 工學院 | zh_TW |
dc.contributor.author-dept | 高分子科學與工程學研究所 | zh_TW |
顯示於系所單位: | 高分子科學與工程學研究所 |
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