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研究生： 江啟宏
Chi-Hung Chiang
論文名稱： 合成新的含側羥基聚醯亞胺及其性質研究
Synthesis and Characterization of New Polyimides with Hydroxyl Groups
指導教授： 陳燿騰
Yaw-Terng Cherm
口試委員: 王健珍
none
陳原振
none
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： 2005
畢業學年度： 93
語文別： 中文
論文頁數： 84
中文關鍵詞： 聚醯亞胺
外文關鍵詞： Polyimide
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    • 以1,1-bis(4-(2-hydroxy-4-aminophenoxy)phenyl)-1-phenyl-2,2,2-
    trifluoroethane含側羥基二胺單體和數種芳香族二酸酐經溶液聚縮合合成含側羥基的聚醯亞胺，進一步研究此系列聚醯亞胺的固有黏度、溶解度、熱性質與機械性質。
    首先，以含側羥基之二胺單體與芳香族酸酐所合成的聚醯亞胺的固有黏度範圍在0.48∼0.83 dL/g之間，且具有好的溶解度，這些聚醯亞胺可溶於N,N'-Dimethylformamide (NMP)、o-Chlorophenol、m-cresol、 N,N'-Dimethylacetamide (DMAc)、Tetrahydrofuran與cyclohexanone等溶劑中，經differential scanning calorimeter (DSC)與 dynamic mechanical analysis (DMA)測試所合成之聚醯亞胺的玻璃轉移溫度分別介於261∼315℃與284∼333℃之間，經thermogravimetic analyzer (TGA)測試所合成之聚醯亞胺的熱安定性，其10％熱重量損失，於空氣下介於465∼486℃之間，於氮氣下介於438∼449℃之間，於氮氣下700℃燃燒殘餘率介於48∼61％之間，經抗張強度測試所合成之聚醯亞胺的機械性質，其抗張強度介於92∼155 MPa之間，斷裂伸長率介於7.6∼17.5％之間。

    A series of new polyimides, containing pendant hydroxyl groups were prepared via the solution polycondensation of various aromatic dianhydri-
    de with 1,1-bis(4-(2-hydroxy-4-aminophenoxy)phenyl)-1-phenyl-2,2,2-
    fluoroethane. The inherent viscosities, solubility properties, thermal properties and dynamic mechanical properties of the polyimides were investigated.
    First, the polyimides derived from 1,1-bis(4-(2-hydroxy-4-aminophen-
    oxy)phenyl)-1-phenyl-2,2,2-trifluoroethane, had inherent viscosities of 0.48∼0.83 dL/g. The obtained polyimides were readily soluble in N,N'-Dimethylformamide (NMP) , N,N'-Dimethylacetamide (DMAc), m-cresol, o-chlorophenol, Tetrahydrofuran (THF) and cyclohexanone. The differential scanning calorimeter (DSC) and dynamic mechanical analysis (DMA) reveals that the glass transition temperatures ranged on 261∼315℃ and 284∼333℃, respectively. In addition, the temperatures of 10％ weight loss in air and nitrogen ranged on 465∼486℃ and 438∼449℃, respectively. The polymer films had tensile strengths of 92∼155 MPa, and elongation to breakage values of 7.6∼17.5％.

    摘要 .I Abstract II 目錄 ….III Scheme索引 ..V Table索引 .VI 附圖索引 .VII 第一章 緒論….. 1 1-1 前言..1 1-2 聚醯亞胺簡介.. 1 1-3 聚醯亞胺的合成方法..3 1-4 聚醯亞胺的改質及其應用..8 1-5 側羥基聚醯亞胺的應用與文獻回顧.13 1-6 擬進行之研究….19 第二章 實驗..22 2-1 實驗藥品…22 2-2 實驗程序...26 2-2-1 單體製備.26 2-2-2 聚醯亞胺的合成…….30 2-3 單體鑑定及聚合物之物性與化性分析..32 第三章 結果與討論....35 3-1 製備1,1-bis(4-(2-hydroxy-4-aminophenoxy)phenyl)-1-phenyl- 2,2,2-trifluoroethane單體…35 3-2 聚醯亞胺的合成..36 3-3 聚醯亞胺的物性分析.37 第四章 結論....41 參考文獻….43 作者簡介.71 Scheme索引 Scheme 1 1,1-bis(4-(2-hydroxy-4-aminophenoxy)phenyl)-1-phenyl-2,2, 2- trifluoroethane合成步驟……………………………….27 Scheme 2 合成聚醯亞胺之反應式…………………………………..31 Table索引 Table 1 The Inherent Viscosities of Soluble Polyimides……………...36 Table 2 Solubility of Polyimides……………………………………...37 Table 3 Thermal Properties of Polyimides……………………………38 Table 4 Mechamical Properties of Polyimide Films………………….39 附圖索引 附圖2-1 Mass spectrum of 1,1-bis(4-(2-methoxy-4-nitrophenoxy)phenyl) -1-phenyl-2,2,2-trifluoroethane………………………………48 附圖2-2 Mass spectrum of 1,1-bis(4-(2-hydroxy-4-nitrophenoxy)phenyl) -1-phenyl-2,2,2-trifluoroethane………………………………49 附圖2-3 Mass spectrum of 1,1-bis(4-(2-hydroxy-4-aminophenoxy)phenyl )-1-phenyl-2,2,2- trifluoroethane……………………………..50 附圖3-1 DMA curve of polyimide 5a in nitrogen atmosphere at a heating rate of 10℃/min…………………………………………...…51 附圖3-2 DSC curve of polyimide 5a in nitrogen atmosphere at a heating rate of 20℃/min………………………………………...……52 附圖3-3 TGA curve of polyimide 5a in nitrogen atmosphere at a heating rate of 10℃/min…………………………………………….53 附圖3-4 TGA curve of polyimide 5a in air atmosphere at a heating rate of 10℃/min…………………………………………………54 附圖3-5 DMA curve of polyimide 5b in nitrogen atmosphere at a heating rate of 10℃/min……………………………………………...55 附圖3-6 DSC curve of polyimide 5b in nitrogen atmosphere at a heating rate of 20℃/min…………………………………………….56 附圖3-7 TGA curve of polyimide 5b in nitrogen atmosphere at a heating rate of 10℃/min…………………………………………..….57 附圖3-8 TGA curve of polyimide 5b in air atmosphere at a heating rate of 10℃/min…………………………………………………..58附圖3-9 DMA curve of polyimide 5c in nitrogen atmosphere at a heating rate of 10℃/min……………………………………………...59 附圖3-10 DSC curve of polyimide 5c in nitrogen atmosphere at a heating rate of 20℃/min…………………………………………….60 附圖3-11 TGA curve of polyimide 5c in nitrogen atmosphere at a heating rate of 10℃/min…………………………………………….61附圖3-12 TGA curve of polyimide 5c in air atmosphere at a heating rate of 10℃/min…………………………………………………62附圖3-13 DMA curve of polyimide 5d in nitrogen atmosphere at a heating rate of 10℃/min……………………………………63 附圖3-14 DSC curve of polyimide 5d in nitrogen atmosphere at a heating rate of 20℃/min………………………………………….. ..64 附圖3-15 TGA curve of polyimide 5d in nitrogen atmosphere at a heating rate of 10℃/min……………………………………65 附圖3-16 TGA curve of polyimide 5d in air atmosphere at a heating rate of 10℃/min…………………………………………………66 附圖3-17 DMA curve of polyimide 5e in nitrogen atmosphere at a heating rate of 10℃/min……………………………………67 附圖3-18 DSC curve of polyimide 5e in nitrogen atmosphere at a heating rate of 20℃/min……………………………………………68 附圖3-19 TGA curve of polyimide 5e in nitrogen atmosphere at a heating rate of 10℃/min…………………………………………….69 附圖3-20 TGA curve of polyimide 5e in air atmosphere at a heating rate of 10℃/min………………………………………….……...70

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