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研究生: 廖學一
Hsueh-yi Liao
論文名稱: 合成新的含雙苯胺側基之聚醯亞胺和聚醯胺及其性質研究
Synthesis and Characterization of New Polyimides and Polyamides containing pendent Biphenylamine moieties
指導教授: 陳燿騰
Yaw-terng Chen
口試委員: 陳志堅
陳志堅
江選雅
江選雅
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: 2006
畢業學年度: 94
語文別: 中文
論文頁數: 90
中文關鍵詞: 雙苯胺
外文關鍵詞: biphenylamine
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  • 首先,以含雙苯胺側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0.51∼0.84 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介於294∼315℃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532∼584℃之間,於氮氣下介於537∼577℃之間,於氮氣下700℃燃燒殘餘率介於65∼74%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70∼99 MPa之間,斷裂伸長率介於4.0∼6.3%之間,Ultra violet (UV/Visible)測試所合成之聚醯亞胺之光學性質,其主要UV吸收峰在300 nm左右,而由光基發所產生螢光主要發生在477 nm左右,屬於藍光範圍。

    以含雙苯胺側基之二胺單體與芳香族二酸所合成的聚醯胺的固有黏度範圍在0.32∼0.47 dL/g之間,且具有好的溶解度,這些聚醯胺可溶於N,N'-Dimethylformamide (NMP)、o-Chlorophenol、 N,N'-Dimethylacetamide (DMAc)、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257∼303℃與273∼332℃之間,經thermogravimetic analyzer (TGA)測試所合成之聚醯胺的熱安定性,其10%熱重量損失,於空氣下介於504∼536℃之間,於氮氣下介於480∼526℃之間,於氮氣下700℃燃燒殘餘率介於64∼74%之間,經抗張強度測試所合成之聚醯胺的機械性質,其抗張強度介於102~106 MPa之間,斷裂伸長率介於6.5~10.0%之間Ultra violet (UV)測試所合成之聚醯胺之光學性質,其主要UV吸收峰在310 nm左右,而由光激發所產生螢光主要發生在475 nm左右,屬於藍光範圍。


    The polyimides derived from 2,2’-bis(2-diphenylamine)-4,4’-diaminobiphenyl, had inherent viscosities of 0.51~0.84 dL/g. The 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 294∼315℃. In addition, the temperatures of 10% weight loss in air and nitrogen ranged on 532∼584℃ and 537∼577℃, respectively. The polymer films had tensile strengths of 70∼99 MPa, and elongation to breakage values of 4.0∼6.3%.These polymers exhibited strong UV-vis absorption bands at 300 nm in Chloroform solution. The photoluminescence spectra showed maximum bands around 477 nm in the blue region.

    The polyamides derived from 2,2’-bis(2-diphenylamine)-4,4’-diaminobiphenyl, had inherent viscosities of 0.32~0.47 dL/g. The polyamides were readily soluble in N,N'-Dimethylformamide (NMP) , N,N'-Dimethylacetamide (DMAc), o-chlorophenol, and cyclohexanone. The differential scanning calorimeter (DSC) and dynamic mechanical analysis (DMA) reveals that the glass transition temperatures ranged on 257∼303℃ and 273∼332℃, respectively. In addition, the temperatures of 10% weight loss in air and nitrogen ranged on 504∼536℃ and 480∼526℃, respectively. The polymer films had tensile strengths of 102~106 MPa, and elongation to breakage values of 6.5~10.0%.These polymers exhibited strong UV-vis absorption bands at 310 nm in NMP solution. The photoluminescence spectra showed maximum bands around 475 nm in the blue region.

    摘要 .............................................................................................I Abstract ……………………………………………………...……III 目錄 …………………………………………….……………. V Scheme索引 ……………………………………………………..…..VIII Table索引 …………………………………………………………..IX 附圖索引 …………………………………………………………. X 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………………………………… ..9 1-5 聚醯胺簡介.............................................................................14 1-6 聚醯胺的合成方式.................................................................15 1-7 含三苯胺側基的應用與文獻回顧……………………….....20 1-8 擬進行之研究………………………………….....…………25 第二章 實驗………………………………………………......27 2-1 實驗藥品……………………………………………….……27 2-2 實驗程序…………………………………………….............31 2-2-1 單體製備……………………………………………….31 2-2-2 聚醯亞胺的合成…………………………………….....34 2-2-3 聚醯胺的合成.................................................................35 2-3 單體鑑定及聚合物之物性與化性分析…………………....37 第三章 結果與討論...........................................................................40 3-1 製備2,2’-bis(2-diphenylamine)-4,4’diaminobiphenyl單體…40 3-1-1單體之製備...........................................................................40 3-2 聚醯亞胺的合成…………………………………………......41 3-3 聚醯亞胺的物性分析………………………………………..43 3-3-1 溶解度測試..........................................................................43 3-3-2 機械性質測試......................................................................44 3-3-3 熱性質測試..........................................................................44 3-3-4 光學性質測試......................................................................45 3-4 聚醯胺的合成...........................................................................47 3-4-1 溶解度測試......................................................................48 .3-4-2 機械性質測試...................................................................48 3-4-3 熱性質測試........................................................................49 3-4-4 光學性質測試..................................................................50 第四章 結論.......................................................................................51 4-1聚亞醯胺.......................................................................................51 4-2 聚醯胺...........................................................................................52 參考文獻………………………………………………………………..54 作者簡介………………………………………………………………..88

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