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研究生:吳信瑜
研究生(外文):wu hsin-yu
論文名稱:合成含金剛烷之聚脂及其物性分析
論文名稱(外文):Synthesis and Characterization of Adamantane-based Polyesters
指導教授:陳燿騰
指導教授(外文):chern yaw- terng
學位類別:碩士
校院名稱:國立臺灣科技大學
系所名稱:化學工程系
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:1999
畢業學年度:87
語文別:中文
論文頁數:74
中文關鍵詞:金剛烷聚酯側基主鏈
外文關鍵詞:adamantanepolyesterside groupmainchain
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由1,3-Bis[4-(4-chloroformylphenoxy)phenyl]adamantane與數種二元醇合成主鏈含有金剛烷的新型聚酯,所合成聚酯之固有黏度範圍在0.38 - 0.82 dL/g,而由GPC測得其分子量 ( Mn ) 範圍在31,000 - 92,000。這些聚酯具有良好的溶解度,可溶於o-chlorophenol、chloroform、o-dichlorobenzene、N-Methyl-2-pyrrolidone( NMP )及tetrahydrofuran( THF )等溶劑中。它們的抗張強度範圍於40.1-56.7 MPa之間,斷裂伸長率為8.5-20.2 ﹪,初始剛性模數為1.6-1.7 GPa。經由DSC分析,測得其玻璃轉移溫度(Tg)在194-284 ℃ 之間。而由TGA分析測得它們在10%重量損失時溫度,在氮氣下為468-489 ℃,在空氣下為454-493 ℃,而其在700 ℃氮氣下之燃燒殘餘率為34-48 % 。
另外也由1,4—Bis(4-carboxyphenoxy)—2-adamantylbenzene acyl chloride與數種二元醇合成新型聚酯,它們的固有黏度範圍在0.32-1.11 dL/g,這些聚酯都可塗佈成具韌性薄膜,而且這些聚酯具有良好的溶解度,可溶於o-chlorophenol、chloroform、o-dichlorobenzene、NMP、nitrobenzene及THF等溶劑中,而它們的抗張強度範圍於46.5-78.4 MPa之間,斷裂伸長率為8.7-15.7 ﹪,初始剛性模數為1.6-1.8 GPa。經由DSC分析,測得其玻璃轉移溫度(Tg)在210-288 ℃ 之間。而由TGA分析測得這些聚酯在10 %重量損失時溫度,在氮氣下為428-482 ℃,在空氣下為419-483 ℃,而其在700 ℃氮氣下之燃燒殘餘率為30-42 %。另外,也比較主鏈含金剛烷之聚脂與含金剛烷側基之聚脂的性質差異。

The new adamantane-based polyesters were synthesized by reacting of 1,3-Bis[4-(4-chloroformylphenoxy)phenyl] adamantane with various diols. The adamantane-containing polyesters had inherent viscosities of 0.38 - 0.82 dL/g and number-average molecular weights ( Mn ) of 31,000 - 92,000. All polyesters had good solubility and were soluble in o-chlorophenol, chloroform, o-dichlorobenzene, NMP and THF. Those polyesters had tensile strengths of 40.1-56.7 MPa, elongations to break of 8.5-20.2 ﹪, and initial moduli of 1.6-1.7 GPa. DSC reveal that their glass transition temperatures were found to be 194-284 ℃. The temperatures of polyesters at 10 % weight loss ranged from 468-489 ℃ in N2 atmosphere and from 454-493 ℃ in air. Their char yield ranged from 34-48 % at 700 ℃ in N2.
In addition, the new polyesters were also synthesized by reacting of 1,4—Bis(4-carboxyphenoxy)—2-adamantylbenzene acyl chloride with various diols. The polyesters with adamantane side group had inherent viscosities of 0.32-1.11 dL/g and all the films were flexible. All polyesters had good solubility and were soluble in o-chlorophenol, chloroform, o-dichlorobenzene, nitrobenzene, NMP and THF. Those polyesters had tensile strengths of 46.5-78.4 MPa, elongation to break of 8.7-15.7 ﹪, and initial moduli of 1.6-1.8 GPa. DSC reveal that their glass transition temperatures were found to be 210-288 ℃. The temperatures of polyesters at 10 % weight loss ranged from 428-482 ℃ in N2 atmosphere and from 419-483 ℃ in air. Their char yield ranged from 30-42 % at 700 ℃ in N2. In addition, a comparison of physical properties of the polyesters derived from 1,3-Bis[4-(4-chloroformylphenoxy)phenyl]adamantane with those derived from 1,4—Bis(4-carboxyphenoxy)—2-adamantylbenzene acyl chloride is also presented.

摘要................................................Ⅰ
Abstract............................................Ⅲ
目錄................................................Ⅴ
圖表索引............................................Ⅷ
第一章 緒論.........................................1
1-1 金剛烷(adamantane)的介紹........................1
1-2 聚酯的回顧......................................3
1-3 聚酯的種類......................................5
1-3-1 PET與 PBT聚酯.................................5
1-3-2 PCT聚酯.......................................6
1-3-3 全芳香族聚酯(Polyarylate).....................7
1-4 聚酯之合成方法..................................9
1-4-1 酯交換法......................................9
1-4-2 氯醯法........................................10
1-4-3高溫直接聚酯化法...............................11
1-4-4固態聚縮合法...................................12
1-5 擬進行之研究....................................13
第二章 實驗.........................................15
2-1 實驗藥品........................................15
2-2 實驗儀器........................................18
2-3 實驗程序........................................20
2-3-1 單體製備......................................20
2-3-1.1 單體的純化..................................20
2-3-1.2 製備1,3-Bis[4-(4-chloroformylphenoxy)
phenyl]adamantane (Ⅰ)..............................20
2-3-1.3 製備1,4—Bis(4-carboxyphenoxy)—2-
adamantylbenzene acyl chloride (Ⅳ)..........21
2-3-2 聚酯之合成....................................25
2-4 單體鑑定及聚合物之物性與化性分析................26
第三章 結果與討論...................................29
3-1 1,3-Bis[4-(4-chloroformylphenoxy)phenyl]
adamantane (Ⅰ)...............................29
3-1-1 單體的製備....................................29
3-1-2 聚酯的合成....................................29
3-1-3 聚酯的物性分析................................30
3-2 1,4—Bis(4-carboxyphenoxy)—2-adamantyl
benzene acyl chloride (Ⅳ)....................34
3-2-1 單體的製備....................................34
3-2-2 聚酯的合成....................................35
3-2-3 聚酯的物性分析................................36
3-3 二系類聚酯之比較................................40
第四章 結論.........................................41
參考文獻............................................42

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