聚醯亞胺顆粒之製備及其性質研究

Preparation and Characterization of Polyimide Particles

黃信錠(Hsin-Ting Huang)

指導教授 ： 許克瀛

中原大學/工學院/化學工程研究所/碩士(2002年)

https://doi.org/10.6840/cycu200200406

摘要

本研究利用分散聚縮合反應及沉澱聚縮合反應製備聚醯亞胺顆粒。將二酸酐單體與二胺單體溶於聚合媒介中，以均質機高速攪拌使其分散均勻後進行聚合反應，製得聚醯胺酸顆粒，再經由熱醯亞胺化成聚醯亞胺顆粒。利用配方及反應條件的改變，探討對聚醯亞胺顆粒粒徑大小、表面形態及其熱性質、結晶性等物性的影響。由實驗結果獲得製備單一散度次微米級聚醯亞胺顆粒穩定聚合系統。
由實驗結果得知，聚合顆粒粒徑隨二酸酐單體及二胺單體之總量增加而增加；隨脂肪族二胺單體亞甲基鏈長增加及芳香族二胺單體苯基鏈長減少而增加；隨聚合顆粒分子鏈之骨架密度增加而減少。所得顆粒依配方及反應條件不同，其粒徑介於0.05 mm~2.55 mm之間，其固有黏度介於0.1 dL/g~0.63 dL/g，其10%熱重損失介於403℃~633℃之間。

關鍵字

單一散度 ； 聚醯亞胺顆粒 ； 次微米級 ； 沉澱聚縮合反應

並列摘要

In this study, polyimide polymer particles prepared by using dispersion polycondensation and precipitation polycondensation.
Monomers, dianhydride and diamine dissolved in polymerization medium, disperse homogeneously by using homogenizer at a high speed, then polymerize in a batch reactor. After completely polycondensation, poly(amic acid) particles can be obtained firstly. Subsequently, polyimide particles formed by via of thermal imidization.
By changing the recipes and reaction condition, the effects on the size and morphology, and physical properties, such as: thermal stability, crystallinity…etc., were investigated. The stable polymerization system to prepare submicron-sized monodisperse polyimide particles can be obtained from experimental runs.
From the experimental results, the diameter of particles increased with increasing the total amount of dianhydride monomer and diamine monomer, and increasing the number of methylene groups of aliphatic diamine monomer and decresing the number of phenylene groups of aromatic diamine monomer, and decreased with increasing the skeletal density of particle molecular chain.
In this study, polyimide polymer particles prepared under various recipes and various reaction conditions were in the range between 0.55 and 2.55 mm. The inherent viscosities of particles were in the range from 0.1 to 0.63 dL/g, and the 10% weight loss of particles was in the range of 403 and 633℃.

並列關鍵字

Monodisperse ； Polyimide particle ； Precipitation polycondensation ； Submicron-sized

參考文獻

21. Yasuhisa Nagata, Yuuki Ohnishi, and Tisato Kajiyyama, Polymer Journal, 28(11), 980-985(1996)

14. C. H. Yang and R. S. Chen, Polymer, 40 1025(1999)

20. Hiroshi Inoue, Tadao Muramatu, Yoshikazu Sasaki and Toshio Ogawa, 61, 929-933(1996)

22. François Basset, Alain Lefrant, Thierry Pascal, Bernard Gallot and Bernard Sillicon, Polym. Adv. Technol., 202-209(1998)

1. Sober. H. A ; Peterson. E. A., J. Am.Chem. Soc., 76, 1711(1954).