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標題: 可交聯型磷系聚酯與磷系活性聚酯及環氧樹脂組成物之合成與性質研究
Synthesis and properties of phosphinated crosslinkable polyesters and compositions of phosphinated active ester and epoxy
作者: 林敬堯
Ching Yao Lin
關鍵字: 阻燃
Flame retardant
Crosslinkable group
引用: 1. US Patent 2556295, 1951. 2. M. A. G. Jansen, L. H. Wu, J. G. P. Goossens, G. De Wit, C. Bailly, C. E. Koning, Journal of Polymer Science: Part A: Polymer Chemistry, 2007, 45, 882–899. 3. C. S. Wang, C. H. Lin, Polymer, 1999, 40, 747-757. 4. V. Jankauskaite, G. Macijauskas, R. Lygaitis, Materials Science, 2008, 14(2) , 1392–1320. 5. I408144 6. C. H. Lin, C. M. Huang, M. W. Wang, S. A. Dai, H. C. Chang, T. Y. Juang, Journal of Polymer Science: Part A: Polymer Chemistry, 2014, 52, 424–434. 7. X. Han, P. A. Williams, A. B. Padias, H. K. Hall Jr., Macromolecules, 1996, 29, 8313-8320. 8. M. C. Stuparu, J. Xu, H. K. Hall Jr., Tetrahedron Lett, 2009, 50, 6743-6744. 9. J. Huanc, J. P. Leblanc, H. K. Hall Jr, J. Polym. Sci. Part A: Polym. Chem,1992, 30, 345-354. 10. X. Han, P. A. Williams, A. B. Padias and H. K. Hall Jr., Macromolecules, 1996, 29, 8313-8320. 11. A. B. Padias, H. K. Hall Jr., Polymers, 2011, 3, 833-845. 12. W. J. Jackson, H. F. Kuhfuss, Journal of Polymer Science: Polymer Chemistry Edition, 1976, 14, 2043-2058. 13. T. S. Chung, Polym. Eng. Sci, 1986, 26, 901-919. 14. T. H. Shinn, J. Y. Chen and C. C. Lin, J. Appl. Polym. Sci, 1993, 47, 1233-1241. 15. C. S. Wang, C. H. Lin, C. Y. Chen, Journal of Polymer Science: Part A: Polymer Chemistry, 1998, 36, 3051–3061. 16. C. S. Wang, C. H. Lin, Polymer, 1999, 40, 4387–4398. 17. A. S. More, P. V. Nail, K. P. Kumbhar, P. P. Wadgaonar, Polym Int, 2010, 59, 1408–1414 18. T. Fukuhara, Y. Shibasaki, S. Ando, M. Ueda, Polymer, 2004, 45, 843-847. 19. C. H. Lin, S. L. Chang, Y. R. Wang, C. K. Hsu, T. Y. Juang, Journal of Polymer Science Part A: Polymer Chemistry, 2013, 51, 1734-1741. 20. Y. Liu, J. Zhang, Z. Li, X. Luo S. Jing, M. Run, Polymer, 2014, 55, 1688-1697. 21. C. H. Lin, T. I. Wong, M. W. Wang, H. C. Chang, T. Y. Juang, Journal of Polymer Science Part A: Polymer Chemistry 2015, 53, 513–520 22. IE020678I 23. 王春山,”環氧樹脂簡介與最新發展”,化工技術,2卷,10期,55,1994 24. C. H. Lin, C. S. Wang, Polymer, 2001, 42(5), 1869-1878. 25. Y. L. Liu, Journal of Polymer Science Part A: Polymer Chemistry, 2002, 40, 359–368. 26. US 20140342161 A1
摘要: 第一部分實驗是利用先前實驗室成功合成之含磷雙醇單體(1) ,並利用單體(1)分別與PBT與PET進行醇解縮合反應得到磷系共聚酯,在XRD可觀察到隨著導入單體(1)的量增加,共聚酯的結晶度則有下降的趨勢。 從DMA的分析可以看到共聚酯玻璃轉移溫度(Tg)的提升與導入單體(1)的量有關。在UL-94測試中可以看到將單體(1)導入PBT與PET中具有阻燃效果,在共聚酯磷含量分別為1.65%與0.72%時即可達到UL-94 V-0等級。由於能夠直接跟回收型態的PBT與PET來製備出阻燃型的聚酯,所以能夠達到綠色工業的精神。 第二部分實驗是合成一系列的磷系半芳香族聚酯與磷系全芳香族聚酯,並將丙烯基(allyl group)導入於聚酯中,從溶解度測試可以觀察到,乙烯醚鍵與丙烯基的導入能有效的提升聚酯對於有機溶劑的溶解度,在DMA的測定下可以觀察到隨著固化溫度的提升,含丙烯基結構之聚酯在熱交聯的影響下具有較好的熱性質與熱穩定性。然而含丙烯基(allyl group)異構化成烯丙基(propenyl group)後,在DMA與TGA測定下可以觀察到,含烯丙基(propenyl group)之聚酯在熱交聯後的熱性質與熱穩定性都有所提升。 第三部分實驗是以第二部分成功合成的磷系全芳香族聚酯當作環氧樹脂固化劑,在TMA與介電性質的測定下可觀察到,與DIC活性酯硬化劑HPC-8000-65T作比較,具有更優異的熱性質與介電常數。
Part Ⅰ. Using the previously successful synthesis of phosphorated diol (1) in the laboratory, phosphinated copolyesters based on the alcoholysis and polycondensation of (1) with poly(ethylene terephthalate) (PET) and poly(butylene terephthalate) (PBT) were prepared. The crystallinity of copolyesters decreased gradually with the content of (1), as shown in wide-angle X-ray diffractograms and differential scanning calorimetry thermograms. Dynamic mechanical analysis show Tg increased with the content of (1). UL-94 flame retardant test shows that the flame resistance of PBT and PET was enhanced with the content of (1), copolyesters with UL-94 V-0 grade can be achieved with a phosphorus content as low as 1.65 wt % and 0.72 wt %. The ability to directly with the recovery patterns of PBT and PET to prepare a flame-retardant polyester, it is possible to reach the spirit of green industries. Part Ⅱ. Synthesis of a series of phosphinated semi-aromatic polyesters and phosphinated polyarylates, allyl group introduced into the polyesters. From the solubility test can be observed ethylene ether linkage and propenyl group introduced can effectively enhance the solubility of the organic solvent for the polyesters. In the dynamic mechanical analysis measurement can be observed with the enhancement of the curing temperature. Allyl-containing polyesters with good thermal properties and thermal stability under the influence of heat crosslinking. It can be observed that after isomerization of allyl into propenyl, propenyl-containing polyesters thermal properties and thermal stability of the heat after crosslinking have increased in the dynamic mechanical analysis and thermogravimetric analysis measurement. Part Ⅲ. Using the previously successful PartⅡ synthesis of phosphorated polyarylates as epoxy curing agent, in the thermal mechanical analysis and dielectric properties measurement can be observed. Phosphorated polyarylates as epoxy curing agent with DIC poxy curing agent HPC-8000-65T comparison has superior thermal properties and the dielectric constant.
文章公開時間: 2019-07-28
Appears in Collections:化學工程學系所



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