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系統識別號 U0002-1107201313260300
中文論文名稱 二苯亞甲基山梨醇與醇系統有機膠之結構與性質研究
英文論文名稱 Studies on the structure-property of the organogels composed of dibenzylidene sorbitol and alcohol system
校院名稱 淡江大學
系所名稱(中) 化學工程與材料工程學系碩士班
系所名稱(英) Department of Chemical and Materials Engineering
學年度 101
學期 2
出版年 102
研究生中文姓名 李易晉
研究生英文姓名 Yi-Chin Lee
學號 600401177
學位類別 碩士
語文別 中文
口試日期 2013-06-28
論文頁數 115頁
口試委員 指導教授-賴偉淇
委員-童世煌
委員-楊大毅
中文關鍵字 自組裝  二苯亞甲基山梨醇  有機膠 
英文關鍵字 self-assemble  DBS  organogel 
學科別分類
中文摘要 本研究以二苯亞甲基山梨醇(DBS)之衍生物與醇類極性溶劑所形成有機膠分別形成兩個系統,一方面改變溶劑極性基團與分子量,另一方面改變二苯亞甲基山梨醇分子上的基團作探討;討論其有機膠之結構型態、流變性質、熱性質、分子間作用力。
由結構與型態中可觀察到DBS形成之馬爾他十字類似球晶外觀,並由SEM與TEM中觀察到DBS與其衍生物自組裝所形成網狀纖維之外觀,DBS有機膠可由SAXS觀察到可能為層狀堆積。由流變性質與熱性質可發現,因PEG溶劑鏈長較長末端基影響相對明顯;長碳鏈與OH末端基使DBS不易自組裝,形成之有機膠強度較弱且有機膠相變化較慢。IR與UV分析可知道雖小分子溶劑OH末端基較多,但分子無長碳鏈阻礙有助於DBS的自組裝。在DBS與其衍生物系統中,由流變性質與熱性質可得知DBS衍生物分子上的碳基團對於自組裝型成立體障礙,阻礙PEG的OH末端基團影響使其較易自組裝並使有機膠易相變化,但不易形成整齊的結構。IR分析可得知1wt%DBS有機膠雖有較強的氫鍵,但形成的纖維強度不足以成膠。藉由UV與文獻推測出DBS苯環為T-shape堆疊而DMDBS為邊對平面之堆疊模式。
英文摘要 We study the organogels of structure, rheology and thermal Properties in two systems by 1,3:2,4 -Dibenzylidene sorbitol(DBS) and alcohol systems. One system is the difference between molecular weight and different end groups of alcohol solvents and another is the structure difference between DBS and its derivers.
By POM analysis, we found the spherulite-like structure and the 3-D network of DBS by TEM and SEM. We also found the DBS organogels aggregate as lamellar type by SAXS. By rheology and thermal Properties analysis, we found the long carbon chains of PEG make the OH end groups more influential ;the long carbon chains of PEG and the OH end groups made DBS cannot self-assemble easily result in weaker organogels and slower phase transition . By IR and UV analysis we found though small molecular weight solvents have more OH end groups, DBS still self-assemble easily in these solvents without long carbon chains barrier.
By rheology and thermal properties analysis, we found the alkyl groups steric resistance of DBS derivers keep the molecules away from PEG OH end groups then made organogelaters self-assemble and phase transition easily. By IR analysis we found though 1wt% DBS organogel has stronger hydrogen bond, the fibers of DBS were too weak to form gel. By UV analysis, we can simulate DBS phenyl rings stack as T-shape (point to face) and DMDBS stack as face to edge structure.
論文目次 總目錄

總目錄 V
圖目錄 VII
表目錄 X
第一章 緒論 1
1-1 前言 1
1-2 研究目的 2
第二章 理論背景 3
2-1 流變概念 3
2-1.1 黏彈性模型 4
2-1.2 剪切黏度 6
2-1.3動態流變性質 7
2-2 有機凝膠 8
2-2.1 凝膠 8
2-2.2 DBS有機膠 11
第三章 文獻回顧 12
3-1.1小分子有機膠 12
3-1.2 成膠劑對掌性 15
3-2.1 DBS 型膠化劑 17
3-2.2 DBS有機膠 20
第四章 實驗 25
4-1 實驗藥品 25
4-2 實驗設備 28
4-3 實驗流程 32
4-4 實驗樣品製備 34
第五章 溶劑變化對DBS有機膠性質結果與討論 36
5-1 溶劑變化對DBS有機膠流變性質影響 36
5-1.1 振幅掃描(amplitude sweep) 36
5-1.2 頻率掃描(frequency sweep) 38
5-1.3 凝膠熔解溫度 Td(gel dissolution temperature) 40
5-1.4 成膠時間(gel formation time)與成膠溫度Tf(gel formation temperature) 43
5-2溶劑變化對DBS有機膠結構與型態學影響 48
5-3 溶劑變化對DBS有機膠TGA熱重分析 63
5-4 溶劑變化分子作用力分析 67
5-4.1 分子間與分子內氫鍵作用力 67
5-4.2 苯環交互作用力 73
5-5 溶劑變化對DBS有機膠結論 78
第六章 DBS及衍生物變化對PEG400有機膠結果與討論 79
6-1 DBS及衍生物變化對PEG400有機膠流變性質 79
6-1.1 振幅掃描(amplitude sweep) 79
6-1.2 頻率掃描(frequency sweep) 81
6-1.3 凝膠熔解溫度 Td(gel dissolution temperature) 82
6-1.4成膠時間(gel formation time)與成膠溫度Tf(gel formation temperature) 84
6-2DBS及衍生物變化對PEG400有機膠結構與型態學 86
6-3DBS及衍生物變化對PEG400有機膠TGA熱重分析 96
6-4 DBS及衍生物變化對PEG400有機膠分子作用力分析 99
6-4.1 分子間與分子內氫鍵作用力 99
6-4.2 苯環交互作用力 103
6-5 DBS及衍生物變化對PEG400有機膠結論 107
第七章 參考文獻 110







圖目錄
圖2-2 DBS 結構式 11
圖3-1(a)固態纖維 (b)流體纖維 12
圖3-2 三十六烷層狀堆積示意圖 13
圖 3-3(a) 純DBS球晶 14
圖3-4 (A) (B)雙螺旋纖維SEM圖(C) (D) 雙螺旋纖維TEM圖(E) 雙螺旋纖維示意圖 16
圖3-5 DBS分子結構圖 17
圖3-6 DBS合成示意圖 17
圖3-7 DBS衍生物結構式 18
圖3-8 DBS碳位標示圖 19
圖3-9 DBS在不同末端基PEG中成膠時間與溫度 21
圖3-10 不同濃度DBS/PEG Td流變圖 21
圖3-11 不同濃度DBS與不同末端基Td流變圖 22
圖3-12 純DBS場發掃描式電子顯微鏡圖 22
圖3-13 2wt% DBS/PPG (a)25℃(b)83℃(c)105℃(d)130℃ 23
圖3-14 DBS與St、MMA有機膠 24
圖4-1 DBS與不同溶劑相圖 32
圖4-2 不同膠化劑與PEG400相圖 33
圖5-1 3wt%DBS/PEG400 振幅掃描 37
圖5-2 3wt%DBS/溶劑變化振幅掃描 37
圖5-3 3wt%DBS/PEG400 頻率掃描 39
圖5-4 3wt%DBS-溶劑變化頻率掃描 39
圖5-5 3wt%DBS/不同溶劑有機膠凝膠熔解溫度 Td 41
圖5-6 3wt%DBS/PEG400成膠時間 44
圖5-7 3wt% DBS/PEG200成膠時間 44
圖5-8 3wt% DBS/P5G成膠時間 45
圖5-9 3wt% DBS/GL成膠時間 45
圖5-10 3wt% DBS/PG成膠時間 46
圖5-11 3wt% DBS/EG成膠時間 46
圖5-12 PEG400/DBS (a)3wt%(b)4wt%(c)5wt%有機膠POM 51
圖5-13 PEG200/DBS (a)3wt%(b)4wt%(c)5wt%有機膠POM 52
圖5-14 P5G/DBS (a)3wt%(b)4wt%(c)5wt%有機膠POM 53
圖5-15 GL/DBS (a)3wt%(b)4wt%(c)5wt%有機膠POM 54
圖5-16 PG/DBS (a)3wt%(b)4wt%(c)5wt%有機膠POM 55
圖5-17 EG/DBS (a)3wt%(b)4wt%(c)5wt%有機膠POM 56
圖5-18 3wt%DBS/PEG400(a)未沖洗(b)以水沖洗表面SEM 57
圖5-19 3wt%DBS/EG(a)表面 (b)表面皺摺間 SEM 58
圖5-20 3wt%DBS/PEG400(a)50kx (b)100kx TEM 59
圖5-21 3wt%DBS/PEG400 SAXS圖譜 60
圖5-22 3wt%DBS/PEG200 SAXS圖譜 60
圖5-23 3wt%DBS/P5G SAXS圖譜 61
圖5-24 3wt%DBS/GL SAXS圖譜 61
圖5-25 3wt%DBS/PG SAXS圖譜 62
圖5-26 3wt%DBS/EG SAXS圖譜 62
圖5-27純DBS熱重損失圖 63
圖5-28 3wt%DBS/PEG400熱重損失圖 64
圖5-29 3wt%DBS/PEG200熱重損失圖 64
圖5-30 3wt%DBS/P5G熱重損失圖 65
圖5-31 3wt%DBS/GL熱重損失圖 65
圖5-32 3wt%DBS/PG熱重損失圖 66
圖5-33 3wt%DBS/EG熱重損失圖 66
圖5-34 純DBS FT-IR光譜 69
圖5-35 DBS/PEG400有機膠FT-IR光譜 70
圖5-36 DBS/PEG200有機膠FT-IR光譜 70
圖5-37 DBS/P5G有機膠FT-IR光譜 71
圖5-38 DBS/GL有機膠FT-IR光譜 71
圖5-39 DBS/PG有機膠FT-IR光譜 72
圖5-40 DBS/EG有機膠FT-IR光譜 72
圖5-41 苯環錯位示意圖 73
圖5-42 苯環平行位移示意圖 74
圖5-43 DBS/PEG400有機膠 UV/vis圖 76
圖5-44 DBS/PEG200有機膠 UV/vis圖 76
圖5-45 DBS/P5G有機膠 UV/vis圖 76
圖5-46 DBS/GL有機膠 UV/vis圖 77
圖5-48 DBS/EG有機膠 UV/vis圖 77
圖6-1 DBS及衍生物有機膠振幅掃描 80
圖6-2 DBS衍生物/PEG400有機膠頻率掃描 81
圖6-3 不同膠化劑/PEG400有機膠凝膠熔解溫度 Td 83
圖6-4不同膠化劑/PEG400有機膠成膠時間 85
圖6-5 純DBS再結晶外觀 88
圖6-6 純DMDBS再結晶外觀 88
圖6-7 純TBPMN再結晶外觀 89
圖6-8 3wt%DBS/ PEG400 POM 89
圖6-9 3wt%DBS/PEG400未沖洗有機膠SEM 90
圖6-10 3wt%DBS/PEG400水沖洗有機膠SEM 90
圖6-11 1wt%DMDBS/PEG400未沖洗有機膠SEM 91
圖6-12 1wt%DMDBS/PEG400水沖洗有機膠SEM 91
圖6-13 1wt%TBPMN/PEG400未沖洗有機膠SEM 92
圖6-14 1wt%TBPMN/PEG400水沖洗有機膠SEM 92
圖6-15 3wt%DBS/PEG400有機膠TEM 93
圖6-16 1wt%DMDBS/PEG400有機膠TEM 94
圖6-17 1wt%TBPMN/PEG400有機膠TEM 95
圖6-18純膠化劑粉末熱重損失圖 97
圖6-19 DBS有機膠熱重損失圖 97
圖6-20 DMDBS有機膠熱重損失圖 98
圖6-21 TBPMN有機膠熱重損失圖 98
圖6-22 純膠化劑FT-IR光譜 101
圖6-23 DBS與有機膠FT-IR光譜 101
圖6-24 DMDBS與有機膠FT-IR光譜 102
圖6-25 TBPMN與有機膠FT-IR光譜 102
圖6-26 (a)苯環堆疊(b)甲苯堆疊(c)受束縛苯環堆疊式意圖 103
圖6-27苯環平行位移示意圖 104
圖6-28 DMDBS苯環堆疊示意圖 105
圖6-29 DBS/PEG400有機膠 UV/vis圖 106
圖6-30 DMDBS/PEG400有機膠 UV/vis圖 106
圖6-31 TBPMN/PEG400有機膠 UV/vis圖 106
圖6-32 DBS堆疊式意圖 108
圖6-33 DMDBS堆疊式意圖 109
圖6-34 TBPMN堆疊式意圖 109



表目錄

表5-1 DBS/不同溶劑有機膠凝膠熔解溫度 Td比較表 42
表5-2 不同溶劑基團比較表 42
表5-3 不同溶劑有機膠之成膠時間與成膠溫度Tf 47
表6-1不同膠化劑有機膠凝膠熔溫度Td比較表 83
表6-2不同膠化劑有機膠之成膠時間與成膠溫度Tg 85
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