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研究生:資端文
研究生(外文):Tuan-Wen Tzu
論文名稱:新型含氟之可溶性芳香族聚醯亞胺之合成與性質
論文名稱(外文):SYNTHESIS AND PROPERTIES OF NOVEL SOLUBLE FLUORINE-CONTAINING AROMATIC POLYIMIDES
指導教授:蕭勝輝
指導教授(外文):Sheng-Huei Hsiao
學位類別:碩士
校院名稱:大同大學
系所名稱:化學工程學系(所)
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:2004
畢業學年度:92
語文別:英文
論文頁數:43
中文關鍵詞:聚醯亞胺介電常數
外文關鍵詞:dielectric constantspolyimides
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本論文在探討含氟結構之雙醚胺所衍生的新型芳香族聚醯亞胺之合成與性質。一種新型含氟的二醚胺1,1-bis[4-(4-amino-2-trifluoromethyl- phenoxy)phenyl]-1-phenyl-2,2,2-trifluoroethane 是以1,1-bis(4-hydroxy- phenyl)-1-phenyl-2,2,2-trifluoroethane和2-chloro-5-nitrobenzotrifluoride為起始原料,經由二個步驟合成。而一系列含氟結構之聚醯亞胺,是由上述含氟之二胺單體和市售六種芳香族二酐,經由常用的二步驟法合成。第一個步驟所製得的聚醯亞胺前驅體聚醯胺酸的固有粘度值介於0.29-0.39 dL/g 之間。這些聚醯胺酸經化學醯亞胺化成聚醯亞胺後均可被鑄成可撓曲且強韌的薄膜。這些聚醯亞胺對有機溶劑具有良好的溶解性,例如NMP和DMAc,並具有低的介電常數 (2.87-3.17, 10 kHz) 、吸濕性 (0.37-0.58%)及良好的光學透過特性 (cutoff wavelength, 370-411 nm)。這些聚醯亞胺的玻璃轉移溫度 (Tg) 在227 到269 oC之間,他們在空氣或氮氣中分解掉10% 重量的溫度皆在500 oC以上,顯示這些聚醯亞胺具有良好的熱穩定性。為了與上述的聚合物的性質做比較,另一系列的聚醯亞胺是由結構類似的二胺單體1,1-bis[4-(4-aminophenoxy)- phenyl]-1-phenyl-2,2,2-trifluoroethane 製備而得,其合成與性質測定方法類似於上述聚醯亞胺所使用之方法。
A new trifluoromethyl-substituted bis(ether amine) monomer, 1,1-bis[4-(4- amino-2-trifluoromethylphenoxy)phenyl]-1-phenyl-2,2,2-
trifluoroethane, was synthesized that led to a series of novel fluorinated polyimides by the chemical imidization route when reacted with various commercially available aromatic tetracarboxylic dianhydrides. These polyimides were highly soluble in a variety of organic solvents such as N-methyl-2-pyrrolidone, and N,N-dimethylacetamide, and most of them could afford transparent, flexible, and strong films with low dielectric constants of 2.87-3.17 at 10 kHz, low moisture absorptions of 0.37-0.58%, and an ultraviolet-visible absorption cutoff wavelength at 370-411 nm. The glass-transition temperatures of the polyimides were in the range of 227-269 oC, and the 10% weight-loss temperatures were higher than 500 oC. For a comparative study, a series of analogous polyimides based on 1,1-bis[4-(4-aminophenoxy)phenyl]- 1-phenyl-2,2,2-trifluoroethane were also prepared and characterized.
ACKNOWLEDGEMENTS….……………….………………..….………i
ABSTRACT IN ENGLISH….........……………......……………….…….ii
ABSTRACT IN CHINESE………..……………………….…….………iii
TABLE OF CONTENTS….……………......…….…………..…….…….iv
LIST OF TABLES……………….......…………………….…….……….vi
LIST OF FIGURES………………….......………………………….….. vii
LIST OF SCHEMES…………….......…………………….……...…….viii
CHAPTER
1 INTRODUCTION………..…..…………...…….……….……..1
2 EXPERIMENTAL………..…………...…….……..……….…..4
2.1 Materials………………....…………..……………..…..4
2.2 Monomer Synthesis......…………….…………………..5
2.2.1 1,1-Bis[4-(4-nitro-2- trifluoromethylphenoxy)
phenyl]-1-phenyl-2,2,2-trifluoroethane (3a)….5
2.2.2 1,1-Bis[4-(4-amino-2-trifluoromethylphenoxy)
phenyl]-1-phenyl-2,2,2-trifluoroethane (4a)….6
2.3 Polyimide Synthesis ……....……….…........…….…..….8
2.4 Measurement…………………………………...……..…9
3 RESULTS AND DISCUSSION…..…...………..…………...12
3.1 Monomer Synthesis….....……..….……………………12
3.2 Polymer Synthesis………………….…….…..………..18
3.3 Polymer Properties………….……….……….………..23
3.3.1 X-Ray Diffraction Data…………..…………….23
3.3.2 Solubility……………………………….………26
3.3.3 Tensile Properties…………………..…………..26
3.3.4 Thermal Properties………………………..……28
3.3.5 Color Intensity and Optical Transparency……...33
3.3.6 Dielectric Constants and Moisture
Absorption……………………………..……….36
4 CONCLUSION………...………………….……...………39
REFERENCES…........………………….………….………...……….40
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