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研究生： 施育仁
Shih, Yu-Jen
論文名稱： 以水熱法製備具膨潤性奈米雲母及其有機插層之研究
Swelling and organo-intercalation of hydrothermally Li-treated sericite
指導教授： 申永輝
Shen, Yun-Hwei
學位類別： 博士
Doctor
系所名稱： 工學院 - 資源工程學系
Department of Resources Engineering
論文出版年： 2009
畢業學年度： 97
語文別： 中文
論文頁數： 169
中文關鍵詞： 陽離子交換容量 、混層構造 、雲母礦物 、水熱法 、界面活性劑
外文關鍵詞： hydrothermal reaction, cationic surfactants, mica, cation exchange capacity, mixed-layer clay
相關次數： 點閱：104  下載：6 
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    • 本研究以開發雲母礦物膨潤特性的初衷，將內容概分兩大方向，一是採用水熱法之高溫高壓環境進行絹雲母膨潤改質實驗，二是藉陽離子型界面活性劑以離子交換機制吸附插層膨潤雲母，證明其層內空間以有機改性且擴張之能力，作為高電荷雲母跨進奈米領域的前驅。
    在以添加高濃度硝酸鋰進行水熱反應改質絹雲母之研究結果發現，預先脫結晶水可大幅提升水熱反應使層間含鉀轉化成含鋰膨潤程度，以反應溫度170 ℃持溫48小時，K+置換達50 %以上，陽離子交換容量(CEC)從原始3~5 meq/100 g提升至70 meq/100 g，並隨升高反應溫度至270 ℃或增加反應次數，使產品CEC值最終接近原礦電荷理論值120 meq/100 g。熱分析及紅外光光譜(FT-IR)證明改質雲母層間含水現象，並且脫結晶水扭曲結構得以恢復，然原礦中葉蠟石不受水熱反應影響。X光粉末繞射(XRD)顯示晶面間距從原始含K層10 膨脹為含Li層12 ，另外在低角度出現22 及其次階11 晶面是雲母過渡到飽和含Li+相前所形成K、Li層交疊之混層構造。元素分析顯示經水熱反應後層間含K+、Li+總量未明顯改變，並有正比於改質程度的Li+進入結構，此證實雲母能在維持其高電荷量同時達到含水膨潤，並且結構中含Li+模型為取代結晶水之H+的-OLi。
    在以陽離子型界面活性劑插層具膨潤性雲母之研究結果顯示，TMA、DP與CTA等三種界劑對雲母吸附量隨分子量依序增加，晶面間距從改質飽和Li+層之12 分別擴張為含界劑層之13.7 、25.7 與35 。而混層樣品晶面則呈現以含K層與含界劑層相互疊合之形式。FT-IR分析界劑分子以相當1倍CEC值之劑量為分界，變換層間極性環境及DP與CTA碳鏈捲曲/伸張(gauche/trans)之相轉換，並在呈伸張狀態(all-trans) 時以約60°傾角支架層內空間。在電子顯微鏡觀察下，膨潤雲母之飽和Li+相與混層相分別以原始厚度約1 nm矽酸鹽層以及夾非膨潤含K+層約2 nm單位層進行晶面拓展。

    The objective of this study is to explore the swelling capability of mica. Modified mica has been prepared by a two-step process. The first step is mica sheet alteration, which allows interlayer K+ were replaced by hydrated Li+ under hydrothermal-assisted conditions. The second step is the intercalation of cationic surfactants into interlayer space of Li-mica.
    In the study of mica alteration, the thermal-dehydroxylation of mica prior to hydrothermal-Li-treatment leads to a higher exchangeability of interlayer K+ of modified mica. About 50 % of interlayer K+ were removed rapidly in a hydrothermal Li+ solution at 170 ℃ after 48 hours. The CEC value of modified mica increases from 3~5 meq/100 g to 70 meq/100 g. When repeating the hydrothermal-Li-treatment or increasing the reaction temperature to 270 ℃, the CEC value of modified mica increased to the theoretical charge of mica sample, i.e. 120 meq/100 g. Results of thermal and FT-IR analysis suggested the structure distortion of mica caused by dehydroxylation was reconstructed after hydrothermal-Li-treatment. The d-spacing of modified mica obtained by XRD indicated the formation of a mixed-layer 22  phase as mica transited from the K-layer of 10  spacing to the Li-layer of fully hydrated 12  spacing. The invariance of total amounts of interlayer charges before and after hydrothermal-Li-treatment implied that the mica’s high layer charge has not been changed. In addition it is found that a trace amount of Li+ diffused into mica’s lattice and substituted the hydroxyl H+ by transforming into –OLi.
    In the study of organo-intercalation, XRD results revealed that the d-spacing of fully modified mica expanded to 13.7 , 25.7 , and 37  after intercalated with TMA, DP, and CTA, respectively. For the mica with mixed-layer phase a large increase in d-spacing was obtained after intercalated with surfactants. Presumbly the formation of superstructure of unexpanded K-layer and organo-layer caused this artifical expansion. The configuration and aggregation state of intercalated surfactants were monitored by FT-IR analysis using frequency shifts in CH2 stretching and scissoring vibrations. Conformations of the alkyl chains of intercalated surfactant transferred from “gauche” to “trans” state at a surfactant loading of 1.0 CEC equivalence, and hydrophilic state of interlayer inversed simultaneously. The paraffin-like arrangement of intercalated surfactant with the chains tilted an average angle of 60° with respect the surface was found at satuated loading of surfactant. TEM micrographs demonstrated that after intercalation mica sheets were delaminated to single-layers with thickness of 1 nm for fully hydrated mica, and 2 nm for mica containing mixed-layer phase.

    總目錄 摘要 I Abstract II 總目錄 III 表目錄 VI 圖目錄 VII 1-1 研究背景 1 1-2 研究動機 7 1-3 研究目的 8 第二章 理論基礎 9 2-1 層狀矽酸鹽礦物(Phyllosilicates) 9 2-1-1 以結構組成份定義與分類 9 2-1-2 雲母多型體構造(Polytypism in micas) 15 2-1-3 黏土礦物離子交換行為(Cation Exchange Capacity, CEC) 16 2-1-4 雲母改質之候選陽離子 17 2-1-5 黏土-水界面化學模型 18 2-2 黏土礦物之脫結晶水行為(Dehydroxylation) 21 2-2-1 八面體層Al-OH bonding 21 2-2-2 四面體層Si-O bonding 22 2-3 黏土構造之紅外光光譜分析(IR Spectra) 26 2-3-1 晶格振動(Lattice Vibrations) 26 2-3-2 結晶水伸縮振動(Hydroxyl Vibrations) 27 第三章 水熱法製備具膨潤性雲母微粒 31 3-1 實驗方法與步驟 31 3-1-1 實驗材料 31 3-1-2 實驗架構流程 31 3-1-3 實驗步驟 31 1. 樣品處理： 31 2. 脫結晶水熱處理： 32 3. 水熱反應實驗： 32 3-1-4 性質分析 32 1. 元素分析及鉀離子置換量 32 2. 陽離子交換容量(Cation Exchange Capacity, CEC) 33 3. 水熱產物鑑定及結構分析(XRD) 33 4. 紅外光光譜分析(IR specta) 33 5. 熱差/熱重分析(DTA/TG) 33 6. 微觀影像分析 33 3-2 結果與討論 36 3-2-1 絹雲母含結晶水之探討 36 1. 熱重熱差分析(TG/DTA) 36 2. X光粉末繞射分析(XRD) 37 3. 紅外光光譜分析(IR Spectra) 37 3-2-2 絹雲母添加硝酸鋰(LiNO3)之水熱反應 45 1. 不同熱處理溫度預脫結晶水之影響 45 2. 黏土混層概念(Mixed-layer clays) 46 3. K釋出效率與陽離子交換能力 46 4. 水熱改質後雲母中K+及Li+含量變化 48 5. 改質雲母含水膨潤及晶格結構重整 49 6. 水熱溶液固含量與Li濃度之影響 58 7. 水熱反應溫度之影響 58 8. 水熱反應持續時間之影響 60 3-2-3 雲母風化(Mica Weathering)與鉀離子抑制行為 73 1. 於水熱反應時添加NaTPB之效果 74 2. 增加水熱次數之效果 75 3. 白雲母水熱改質實驗 76 3-2-4 雲母層間含水對其矽氧層Si-O鍵結的影響 83 3-2-5 水熱反應後雲母含晶格Li離子之行為 83 3-2-6 改質雲母之熱分析 90 3-2-7 絹雲母水熱反應前後之化學成分變化 90 3-2-8絹雲母水熱反應前後之微觀影像 91 3-2-9 絹雲母之純化 97 1. 原礦之沉降分級 97 2. 水熱改質樣品之沉降分級 100 3-3 結論 106 第四章 以陽離子界面活性劑插層製備有機雲母 108 4-1 實驗方法與步驟 108 4-1-1 實驗材料 108 1. 經水熱改質雲母樣品 108 2. 陽離子型界面活性劑: TMA, DP, CTAB 108 4-1-2 實驗流程 108 4-1-3 實驗步驟 109 4-1-4 性質分析 109 1. 有機插層雲母之界劑吸附量 109 2. 微觀影像分析 109 4-2 結果與討論 113 4-2-1 膨潤雲母對陽離子界劑之吸附行為 113 4-2-2 膨潤雲母插層實驗 114 1. TMA (Tetramethylammonium, 四甲基銨) 114 2. DP (Dodecylpyridinium, 十二烷基啶) 115 3. CTA (Cetyltrimethylammonium, 十六烷基三甲基銨) 116 4-2-3 長碳鏈界劑分子於雲母層間之形態 127 4-2-4 紅外光光譜分析(IR spectra) 130 1. C-H彎曲振動波段(δ-band)區域(1380-1500 cm-1) 130 2. C-H伸縮振動波段(ν-band)區域(2800-3050 cm-1) 131 3. 界劑碳鏈於雲母層間之構造(Trans- vs. Gauche-conformers) 132 4. 經界劑插層雲母之結晶水(~3630 cm-1) 133 5. 經界劑插層雲母之層間水狀態(1640, 3300~3500 cm-1) 133 4-2-5 改質雲母有機插層之微觀影像 144 1. SEM電子顯微分析 144 2. TEM 電子顯微分析 144 4-3結論 153 總結論 154 未來研究建議 155 References 156 表目錄 Table 1.1. Applied sciences of intercalated clays. 5 Table 1.2. The various preparation methods of swelling micas. 6 Table 2.1. Classification of phyllosilicates related to clay minerals. 14 Table 2.2. Hydration enthalpies and Misono softness parameters for metal cations in aqueous solutions. 20 Table 3.1. Assignments of structural infrared vibrations (cm-1) before and after dehydroxylation. 44 Table 3.2. Assignments of structural infrared vibrations (cm-1) of hydrothermally treated sericite. 57 Table 3.3. Chemical composition of original and hydrothermally treated sericite. 94 Table 3.4. Mass and K+ distribution of various hydrodynamically classified original ore. 99 Table 3.5. Mass, CEC, and Li-K content distribution for hydrodynamically classified (±2 µm) sericite. 104 Table 4.1. Properties of altered micas used for organo-intercalation. 110 Table 4.2. Properties of organic cations. 110 Table 4.3. Band positions and assignments for cationic sufactants. 141 圖目錄 Fig. 1.1. Conceptual scheme of Nylon 6-clay hybrid. 2 Fig. 2.1. (a) Single silica tetrahedron and (b) sheet structure of silica tetrahedrons in a hexagonal network. 12 Fig. 2.2. (a) Single octahedral unit and (b) the sheet structure of the octahedral units. 12 Fig. 2.3. Sheet structure of 1:1 type kaolinite. 12 Fig. 2.4. Sheet structure of 2:1 type muscovite. 13 Fig. 2.5. Distance between the planes of atom centers in mica structure. 15 Fig. 2.6. (a) Definition of OI and OII sites of octahedral cation above a tetrahedral net relative to a fixed set of hexagonal axes for a 2:1 layer. (b) Six possible directions of interlayer shift when octahedral cation OI and OII sites are occupied. (c) Three possible stacking polytypes in micas. 19 Fig. 2.7. Models of inner- and outer-sphere surface complexes of interlayer cations. 20 Fig. 2.8. Dioctahdedral sheet structure of mica projected on (001) (a) before and (b) after dehydroxylation. 24 Fig. 2.9. A section of single ditrigonal ring formed by TO4 polyhedra perpendicular to the z direction. Apical oxygen atoms, labeled O(1) and O(2) are part of T(1) and T(2) respectively and those labeled O(4), O(5) and O(6) are basal oxygen atoms. O(3) is the part of hydroxyl groups. 25 Fig. 2.10. Typical infrared diagram of clay minerals. 29 Fig. 2.11. Vibrations of the ideal hexagonal Si2O5 layer. 29 Fig. 2.12. IR spectra of sericite ore (symbol P: pyrophyllite phase), muscovite and pyrophyllite. 30 Fig. 2.13. Orientation of structural hydroxyls in (a): trioctahedral and (b): dioctahedral layer silicates. 30 Fig. 3.1. XRD patterns of natural (a) sericite ore, (b) muscovite and (c) pyrophyllite. 34 Fig. 3.2. Flow sheet of hydrothermally treated sericite. 35 Fig. 3.3. TG/DTA curves of sericite ore. 39 Fig. 3.4. DTA/TG curves of muscovite. 39 Fig. 3.5. Al polyhedron in dioctahedral sheet of a partially dehydroxylated muscovite. 40 Fig. 3.6. XRD patterns of sericite ore heated at various temperature (symbol S* and P* are dehydroxylate sericite and pyrophyllite phase, respectively). 41 Fig. 3.7. IR spectra of sericite ore heated at various temperature. 42 Fig. 3.8. IR spectra of muscovite (after ball milling 18h) and pyrophyllite before and after dehydroxylation. 43 Fig. 3.9. Effect of dehydroxylation temperature on the XRD patterns of Li-hydrothermally treated sericite. 52 Fig. 3.10. Schemes of (a) K+ occupied interlayer, (b) Li+ occupied interlayer, (c) K+ and Li+ homogeneously mixed in interlayer, and (d) regular K+-Li+ mixed-layer superstructure. 54 Fig. 3.11. (a) Exchangeability of K+, CEC values, and (b) K-Li contents of hydrothermally treated sericite as a function of dehydroxylation temperature. 54 Fig. 3.12. Possible positions of diffused Li+ into dioctahedral structure upon heating. 55 Fig. 3.13. IR spectra of hydrothermally treated sericite: effect of dehydroxylation temperature. 56 Fig. 3.14. IR spectra of Li-SAz montmorillonite: (A) OH, H2O stretching and (B) H2O bending regions. From the top to bottom: spectra of unheated sample, and the samples heated for 5, 10, 15, 20, 60 min at 50 ℃... 57 Fig. 3.15. Effect of solid loading on (a) XRD, (b) K-exchangeability, and CEC values of hydrothermally treated sericite. 61 Fig. 3.16. Effect of Li-concentration on (a) XRD, (b) K-exchangeability, and CEC values of hydrothermally treated sericite. 62 Fig. 3.17. Effect of solid loading on the IR spectra of hydrothermally treated sericite. 63 Fig. 3.18. Effect of Li-concentration on the IR spectra of hydrothermally treated sericite. 64 Fig. 3.19. Effect of hydrothermal temperature on the XRD patterns of hydrothermally treated sericite (without dehydroxylation). 65 Fig. 3.20. Effect of hydrothermal temperature on the XRD patterns of hydrothermally treated sericite (with dehydroxylation). 66 Fig. 3.21. (a) Exchangeability of potassium, CEC values, and K-Li contents of specimens Li-treated (15 M for 48 h) from (b) original and (c) dehydroxylated sericite at 90~270 ℃. 67 Fig. 3.22. Effect of hydrothermal temperature on the IR spectra of hydrothermally treated sericite (without dehydroxylation). 68 Fig. 3.23. Effect of hydrothermal temperature on the IR spectra of hydrothermally treated sericite (with dehydroxylation). 69 Fig. 3.24. Effect of hydrothermal duration on the XRD pattern of hydrothermally treated sericite (with dehydroxylation). 70 Fig. 3.25. (a) Exchangeability of potassium, CEC values, and (b) K-Li contents of 800 ℃ preheat sericite after Li-treatment (15 M at 170 ℃) for various duration of hydrothermal heating. 71 Fig. 3.26. Effect of hydrothermal duration on the IR spectra of hydrothermally treated sericite (with dehydroxylation). 72 Fig. 3.27. Formation of mixed-layer phyllosilicates as the weathering front is proceeding around the edge of the particle. 76 Fig. 3.28. (a) 50:50 regularly interstratified clay caused by layer weathering; (b) frayed edge or edge weathering. 77 Fig. 3.29. Potassium displacement by Na+ (1 M NaCl) from several K+-bearing silicates as a function of the solution concentration of K+. 77 Fig. 3.30. (a) XRD, (b) K-exchangeability, and CEC values of dehydroxylated sericite after hydrothermal treatment with various amounts of NaTPB addition. 78 Fig. 3.31. Effects of reaction time on (a) XRD, (b) K-exchangeability, and CEC values of hydrothermal treated sericite with 0.05 N NaTPB. 79 Fig. 3.32. Effects of repeating hydrothermal treatment on the XRD patterns of modified sericite. 80 Fig. 3.33. (a) Exchangeability of potassium, CEC values, and (b) K-Li contents of dehydroxylated sericite after repeating hydrothermal treatment. 81 Fig. 3.34. XRD patterns of original and dehydroxylate muscovite after hydrothermal treatment. 82 Fig. 3.35. Effects of repeating hydrothermal treatment on the IR spectra of sericite. 88 Fig. 3.36. IR spectra of original and dehydroxylate muscovite before and after hydrothermal treatment. 87 Fig. 3.37. The correlation between CEC values and structural Li+ content for different hydrothermally treated sericite samples. 88 Fig. 3.38. (a) XRD patterns and (b) CEC values of hydrothermally treated sericite reheated at various temperature. 89 Fig. 3.39. TGA and DTA results of hydrothermally treated sericite. 92 Fig. 3.40. TGA and DTA results of hydrothermally treated muscovite. 93 Fig. 3.41. SEM micrographs of (a) sericite ore, (b) S800HT, and (c) S800HT4. 95 Fig. 3.42. SEM micrographs of (a) wet-ground muscovite and (b) M800HT4. 96 Fig. 3.43. XRD patterns of various hydrodynamically classified sericite. 98 Fig. 3.44. The particle size distribution of original ore and pure sericite. 99 Fig. 3.45. Imagine of bottom sediment after centrifuging. 100 Fig. 3.46. XRD patterns of hydrodynamically classified sericite: (a) S800HT, (b) S800HT4. 103 Fig. 3.47. IR spectra of hydrodynamically classified sericite and dehydroxylated pyrophylllite. 104 Fig. 3.48. SEM micrographs of hydrodynamically classified sericite: (a) -2µm, and (b) +2µm fraction of S800HT4 (symbol S: sericite; P: pyrophyllite). 105 Fig. 4.1. The molecular comformation and stereoview of crystal structure of (a) TMA, (b) DP, and (c) CTA. 111 Fig. 4.2. Flow sheet for experiments of intercalating cationic surfactant into mica. 112 Fig. 4.3. Sorption isotherms of TMA, DP, and CTA on M800HT. 118 Fig. 4.4. Comparison of inter-chain spacing between of DP and CTA in mica. 118 Fig. 4.5. XRD patterns of (a) TMA, (b) DP, and (c) CTA intercalated M800HT at different surfactant loading. 119 Fig. 4.6. XRD patterns of TMA intercalated (a) S800HT (m: mixed layer), (b) S800HT4, (c) S800HT4-2µm, and (d) M800HT4. 120 Fig. 4.7. XRD patterns of DP intercalated (a) S800HT (m: mixed layer), (b) S800HT4, (c) S800HT4-2µm, and (d) M800HT4. 122 Fig. 4.8. XRD patterns of CTA intercalated (a) S800HT (m: mixed layer), (b) S800HT4, (c) S800HT4-2µm, and (d) M800HT4. 124 Fig. 4.9. XRD patterns of TMA, DP, and CTA adsorbed sericite and muscovite. 126 Fig. 4.10. Configuration of TMA pillars in mica, viewed along the [110] direction. 126 Fig. 4.11. Alkylammonium complexes formed by expansion of expendable micas with organic cations: (a) monolayer, (b) bilayer, (c) pseudotrimolecular layer, and (d) paraffin. 129 Fig. 4.12. IR spectra of TMA-intercalated micas 135 Fig. 4.13. IR spectra of DP-intercalated micas. 136 Fig. 4.14. IR spectra of CTA-intercalated micas. 137 Fig. 4.15. IR spectra of M800HT intercalated with various amounts of TMA. 138 Fig. 4.16. IR spectra of M800HT intercalated with various amounts of DP. 139 Fig. 4.17. IR spectra of M800HT intercalated with various amounts of CTA. 140 Fig. 4.18. IR spectra of original sericite ore and muscovite adsorbed with TMA, DP, and CTA molecules. 142 Fig. 4.19. CH2-stretching vibration region of (a) DP and (b) CTA molecules adsorbed onto outer-surfaces of muscovite and sericite. 142 Fig. 4.20. Different states of interlayer water in cationic surfactants intercalated mica. 143 Fig. 4.21. SEM micrographs of (a) S800HT, (b) S800HT4, (c) S800HT4-2µm, and (d) M800HT4 intercalated with TMA. 146 Fig. 4.22. SEM micrographs of (a) S800HT, (b) S800HT4, (c) S800HT4-2µm, and (d) M800HT4 intercalated with DP. 147 Fig. 4.23. SEM micrographs of (a) S800HT, (b) S800HT4, (c) S800HT4-2µm, and (d) M800HT4 intercalated with CTA. 148 Fig. 4.24. TEM micrographs of (a) M800HT and (b) M800HT4. 151 Fig. 4.25. TEM micrographs of M800HT intercalated with CTA. 150 Fig. 4.26. TEM micrographs of M800HT4 intercalated with CTA. 151 Fig. 4.27. Illustration of the arrangement of intercalated long chain molecules in the interlayer space of (a) mixed layer S800HT and M800HT; (b) fully expanded S800HT4, S800HT4-2µm and M800HT4. 152

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