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標題: 功能性聚醯亞胺與環氧樹脂之合成及其性質探討
Synthesis and Characterization of Functionized Polyimide and Epoxy Resin
作者: 胡裕明
Hu, Yu-Ming
關鍵字: polyimide;聚醯亞胺;clay;epoxy;黏土;環氧樹脂
出版社: 化學工程學系所
引用: 1 陳學仕,”高分子奈米複合材料”, 化工科技與商情,32 卷,29-32,2002/5 2 謝正悅、林慶炫、王春山,”非鹵素難燃電子材料-含磷環氧樹脂”,科學發展月刊,28 卷,11 期,843-850,民89/9 3 吳震裕,”高分子黏土奈米複材”,材料會訊,7 卷,5 期,16,2000. 4 LeBaron, P.C.; Wang, Z.; Pinnavaia, T. J. Applied Clay Science 1999,15, 11. 5 Yano, K.; Usuki, A.; Okada, A.; Kurauchi, T.; Kamigaito, O. J. Polym.Sci., A, Polym. Chem. 1993, 31, 2493. 6 Lan, T.; Kaviratna, P. D.; Pinnavaia, T. J. Chem. Mater. 1994, 6, 573. 7 Tyan, H. L.; Liu, Y. C.; Wei, K. H. Chem. Mater. 1999, 11, 1942. 8 Tyan, H. L.; Wei, K. H.; Hsieh, T. E. J. Polym. Sci., B, Polym. Phys.2000, 38, 2873. 9 Tyan, H. L.; Liu, Y. C.; Wei, K. H. Chem. Mater. 2001, 13, 222. 10 王春山,”環氧樹脂簡介與最新發展”,化工技術,2 卷,10期,55,1994. 11 Cho, C. S.; Chen, L. W.; Chiu, Y. S. Polymer Bulletion 1998, 41, 45. 12 Lin, C. H.; Wang, C. S. Polymer 2001, 42, 1869. 13 曹雅如,”藉由新穎方法合成氧代氮代苯并環已烷與其性質之研究”,中興大學碩士論文,民國95. 14 Agag, T.; Koga, T.; Takeichi, T. Polymer, 2001, 42, 3399. 15 Vaia, R. A.; Teukolsky, R. K.; Giannelis, E. P. Chem. Mater., 1994,1017. 16 Ishida, H.; Rodriguez, Y. Polymer 1995, 36, 3151.146 17 Rimdusit, S.; Ishida, H. Polymer 2000, 41, 7941.
本論文分成兩部份(1)聚醯亞胺-黏土奈米複合材料 (2)帶有Benzoxazine的新型含磷環氧樹脂。
在第一部份中,使用2,2’-bis(p-(p-aminophenoyx)phenyl)propane (BAPP)將黏土改質,使其由親水性轉變成親油性,製成有機化黏土。製備poly(amic acid)和其反應,藉此達到插層效果,經由熱閉環,可得clay-polyimide[4,4’-oxydiphthalic dianhydride- 2,2’-bis(p-(p- amino phenoyx)phenyl)propane (ODPA-BAPP)] 奈米複合材料。藉由改變雙酐的比例,探討其對複合材料之影響。利用XRD和TEM觀察黏土在聚醯亞胺的分散狀況為脫層和插層並存; DSC和TGA觀察聚醯亞胺-黏土奈米複材之熱性質;DMA和萬能拉力機觀察其機械性變化及UV-vis觀察其顏色變化。可發現雙酐過量所合成的clay-polyimide複合材料的熱性質與機械性質都呈明顯的增加,且其製成的薄膜顏色較淡。
在第二部分研究中,先利用兩步法合成出4-(4-(6-oxido-6h-dibenz <1,2> oxaphosphorin-6-yl)- 2H-benzo[1,3]oxazin-3-yl)phenol (3) 及4-(4-(6-oxido-6h-dibenz <1,2> oxaphosphorin-6-yl) -2H-benzo [1,3]oxazin-3-yl)benzoic acid (6),藉由FTIR及NMR鑑定其結構。再和Cresol Novolac Epoxy (CNE)反應,合成帶有Benzoxazine的新型含磷環氧樹脂,藉由FTIR及NMR鑑定其結構。取三種硬化劑4,4’-diaminodiphenylmethane (DDM)、4-aminophenyl sulfone (DDS)及phenol novolac (PN),依照等當量比和含磷環氧樹脂硬化。利用DSC及UL-94試驗檢測硬化後樣品的熱性質和難燃性,可發現硬化後的環氧樹脂固化物有高的玻璃轉移溫度及良好的耐燃性。

In our experience, two major topics were investigated in the present study. First, polyimide-clay nanocomposites. Second, phosphorus- containing epoxy resins.
In part one experience, the reactive organoclay was formed by using 2,2'-bis(p-(p-aminophenoyx)phenyl)propane (BAPP) as a swelling agent for silicate layers of montmorillonite. Clay-polyimide [4,4'-oxydiphthalic dianhydride-2,2'-bis(p-(p-aminophenoyx)phenyl)propane(ODPA-BAPP)] nanocomposites were synthesized from organoclay and poly(amic acid). The layered silicates of organoclay were intercalated by polyimide (ODPA-BAPP), as confirmed by X-ray diffraction and by transmission electron microscopy, and the tensile mechanical properties of the nanocomposites were measured. The thermal properties of clay- polyimide nanocomposites were studied by the TGA, DSC and DMA. It was found that the dispersion of silicate layers in ODPA-BAPP was intercalated and exfoliated structures. It was found that the modulus and the max stress of these clay-polyimide nanocomposites were much higher than those of pure ODPA-BAPP.
In part two experience , we used two step method to synthesize 4-(4-(6-oxido-6h-dibenz <1,2> oxaphosphorin-6-yl)- 2H-benzo[1,3] oxazin-3-yl) phenol (3) and 4-(4-(6-oxido-6h-dibenz <1,2> oxa phosphorin-6-yl)-2H-benzo[1,3]oxazin-3-yl)benzoic acid (6). Two series of novel multifunctional phosphorus-containing epoxy resins were synthesized from the (3,6) and Cresol Novolac Epoxy (CNE), and then cured with 4,4'-diaminodiphenylmethane (DDM), 4-aminophenyl sulfone (DDS), and phenol novolac (PN). The addition reaction was monitored by epoxide equivalent weight (EEW) titration. The proposed structure was confirmed by FTIR and NMR spectra. Thermal properties of cured epoxy resins were studied using differential scanning calorimetry (DSC). The flame-retardancy of cured epoxy resins was tested by UL-94 vertical test. These cured epoxy resins exhibited high glass transition and high thermal stability and achieved UL-94 vertical tests of V-0 grade (nonflammable).
其他識別: U0005-0908200708300400
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