單一散度次微米級中空聚醯胺酸顆粒製備

Preparation of Monodisperse Submicron-sized Hollow Poly(amic acid) Particles

謝惠鈞(Hui-Chun Hsieh)

指導教授 ： 許克瀛

中原大學/工學院/化學工程學系/碩士(2006年)

https://doi.org/10.6840/cycu200600536

摘要

本研究製備單一散度次微米級中空聚亞醯胺顆粒。使用無乳化劑乳化聚合法製備次微米級線性單一散度聚苯乙烯顆粒當粒種，將二酸酐單體與二胺單體以溶劑(甲酸)溶解進行加成聚合反應，形成反應物溶液，再加入粒種，以均質機攪拌或是超音波震盪，做高分子溶液與粒種之混合與攪拌，之後加入大量不良溶劑，沈澱聚醯胺酸與聚苯乙烯的殼核顆粒；再利用萃取液將粒種萃取出來，而合成出中空聚醯胺酸微球，此顆粒能有能力進行改質與醯亞胺化成聚醯亞胺。
由實驗結果得知，利用沉澱法製備殼核顆粒，首先須將高分子溶液和粒種在均質機以11,000rpm之速率攪拌，使粒種與高分子鏈充分分散於媒介中，並在適當時機加入大量不良溶劑使聚醯胺酸高分子沉澱，可以得到聚醯胺酸分子鏈平均的披覆於粒種上所形成之殼核顆粒；高分子非離子型穩定劑(聚乙烯基烷酮)，與離子型穩定劑(硫酸鈉十二烷酯)在適當的用量下，皆可以穩定系統，成功製備出單一散度之殼核顆粒；以甲苯做為萃取線性粒種聚苯乙烯之溶劑，有最佳之萃取效果，可以製備出中空聚醯胺酸顆粒，粒徑介於230nm至420nm，而3%的熱重損失介於580℃至620℃左右。

關鍵字

次微米級 ； 穩定劑 ； 無乳劑乳化聚合 ； 聚醯胺酸顆粒 ； 中空顆粒

並列摘要

The object of this research is to prepare monodisperse submicron-sized hollow polyimide particles. Firstly, the monodisperse submicron-sized polystyrene particles around 180nm in diameter will be prepared by using emulsifier-free emulsion polymerization as seeds. Add seeds into a solvent which dianhydride and diamine have already dissolved to form reactant media, put it into a reactor stirring by homogenizer or by ultrasonic cleaner. Polycondensation will proceed to form poly(amic acid) on the surface of the seeds. A large amount of non-solvent, as media, will be added to through disperse and precipitate the particles, then core-shell poly(amic acid) particles with seed inside will be formed. Hollow poly(amic acid) particles will been got after extraction with solvent. Chemical imidization will be applied on to obtain monodisperse submicron-sized hollow polyimide particles. The effects by changing the recipes of reaction conditions, the morphology of the hollow poly(amic acid) particles, and physical properties such as thermal stability, etc., were investigated.
To learn from the experimental result, we can get the morphology with dispersible core-shell particles by using the homogenizer stirring at 11,000 rpm, When PVP and SDS were used as stabilizer , we can get monodisperse core-shell particles. There is the best extraction result to prepare hollow particles by treating with toluene. We can get hollow particles in the ranbe between 230nm to 420nm. The 3% weight loss of particles was around 580℃ to 620℃.

並列關鍵字

hollow particles ； emulsifier-free polymerization ； submicron ； stabilizer ； Poly(amic acid) particles

參考文獻

5. R.Arshady, J. of Chromatography, 586, 181-197(1991)

6. R.Arshady, J. of Chromatography, 586, 199-219(1991)

10. Linda L. Lloyd, J. of Chromatography, 544, 201-207(1991)

11. C. E. Sroog et. al., J. Polym. Sci., Part A, 3, 1373(1965)

13. H.Yamane, The Second International Conference of Polyomode, 86, (1985)