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研究生： 陳嘉宏
Chia-Hong Chen
論文名稱： 利用迷你乳化聚合法製備二甲基丙烯酸乙二酯與甲基丙烯酸甲酯共聚物微凝膠之合成與特性研究
Synthesis and characterization of Ethylene glycol dimethacrylate and Methyl methacrylate copolymer based Microgel particles via a miniemulsion techniq
指導教授： 陳崇賢
Chorng-Shyan Chern
口試委員: 黃延吉
Yan-Jyi Huang
許榮木
Jung-Mu Hsu
學位類別： 碩士
Master
系所名稱： 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年： 2015
畢業學年度： 103
語文別： 中文
論文頁數： 109
中文關鍵詞： 迷你乳化聚合反應 、微凝膠
外文關鍵詞： Miniemulsionspolymerization, Microgels
相關次數： 點閱：179  下載：3 
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  •  上一筆

    • 本實驗主要是使用甲基丙烯酸甲酯(MMA)與二甲基丙烯酸乙二酯(EGDMA)作為單體，利用迷你乳化聚合法進行共聚合反應，合成出微凝膠(Microgrls)的高分子產品。除了改變反應溫度外，也與MMA單體自聚合、EGDMA單體自聚合反應做比較。
    利用總體轉化率、單體轉化率，膠體粒徑來探討單體與成核粒子間的成核機制；利用DSC、TGA、FTIR、NMR、GPC來探討微凝膠產品的高分子結構與性質分析；最後將微凝膠產品溶在溶劑中，觀察是否會對溶劑流變性質產生改變。
    另外實驗中也利用奧斯華老化效應、膏化線和相分離來探討乳液的安定性。

    The object of this study was to prepare Microgels latex by
    miniemusion copolymerization with MMA and EGDMA monomer.
    In addition to changing the reaction temperature, but also compare to P-MMA and P-EGDMA.
    In addition, overall conversion, monomer conversion, colloid diameter were used to investigate the relationship between monomers and particle nucleation mechanism. DSC, TGA, FTIR, NMR,TEM,GPC used to investigate the Structure of Microgels and properties of Microgels. Finally , Microgels were dissolved at solvent ,and figured out the changing of the rheological property.
    Besides ,Ostwald Ripening Effect, creaming line , Phase separation were used to discuss latex stability.

    摘要 I ABSTRACT II 致謝 III 目錄 IV 圖目錄 IX 表目錄 XII 第一章緒論 1 1-1簡介 1 1-1-1乳液之簡介 1 1-1-2 微凝膠(Microgels)之簡介 2 1-2 研究目的 2 第二章 文獻回顧 4 2-1 乳液的安定性 4 2-1-1奧斯瓦老化效應和滲透壓效應( Osmotic Pressure Effect ) 7 2-1-2 凝聚( Flocculation )與合併( Coalescence ) 8 2-1-3 膏化現象 9 2-2 迷你乳化聚合反應 10 2-3 乳化聚合反應之成核機制 13 2-3-1微胞成核 ( Micellar nucleation ) 14 2-3-2 均質成核理論 ( Homogeneous nucleation ) 15 2-3-4 單體液滴成核( Monomer droplet nucleation ) 18 2-4 微凝膠 ( MICROGELS ) 19 2-4-1微凝膠的分類 19 2-4-2 製備微凝膠 20 2-4-3微凝膠的特性及應用 21 第三章 實驗設備與方法 22 3-1 實驗藥品 22 3-2 實驗儀器 24 3-2-1 乳化聚合反應儀器 24 3-2-2迷你乳液製備儀器 25 3-2-3其他儀器 25 3-2-3測量儀器 26 3-3 實驗方法 27 3-3-1 批次迷你乳化聚合反應 27 3-3-2 總體轉化率的測定 33 3-3-3單體轉化率的測定 34 3-3-4反應速率計算 37 3-3-5迷你乳液奧斯華老化效應測定 38 3-4性質鑑定及分析 41 3-4-1性質鑑定流程 41 3-4-2利用DLS量測不同轉化率的粒子粒徑 42 3-4-3 反應前單體液滴計算 42 3-4-4乳漿高分子產品粒子數計算 43 3-4-5利用GPC 量測乳液產品的分子量以及分子量分布指數(PDI) 43 3-4-6利用TGA測量熱裂解溫度Td 43 3-4-7利用DSC量測玻璃轉移溫度Tg 44 3-4-8利用1H-NMR 量測高分子結構組成與單體雙鍵轉移的量 44 3-4-9利用FTIR尋找是否有未反應的C=C雙鍵 45 3-4-10測量聚合Microgels高分子是否改變溶劑流變性質 46 3-4-11測量膏化線 46 3-4-12判定相分離 47 3-4-13利用未反應之殘留單體再活化 47 3-4-14改變起始劑使否會對乳液產生影響 47 第四章 結果與討論 48 4-1乳液的安定性 48 4-1-1 奧斯瓦老化效應 48 4-1-2 膏化線與相分離 48 4-2總體轉化率 50 4-2-1 單體含量改變對總體轉化率的影響 50 圖 4-2-1 反應溫度70 ℃下迷你乳液的轉化率對時間作圖 51 4-2-2溫度改變對總體轉化率的影響 51 4-3 反應期間粒徑變化 53 4-3-1 含量改變對粒徑的影響 53 4-3-2 溫度改變對粒徑的影響 55 4-4 單體轉化率 56 4-5數目平均分子量與分子量分布(PDI) 62 4-6 TGA 與 DSC 66 4-7 NMR與FTIR 71 4-8 未反應單體實驗再乳化 80 4-9改變起始劑使否會對乳液產生影響 81 4-10 測量聚合MICROGELS高分子是否改變溶劑流變性質 82 第五章 結論 84 文獻 85 附表 91

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