本研究製備次微米級中空聚醯亞胺顆粒,先利用無乳化劑乳化聚合法合成線性聚苯乙烯顆粒當粒種,再以二胺溶液腫入粒種,再加入二酸酐溶液反應,進行脫水環化,使粒種表面聚醯胺酸脫水環化成聚醯亞胺。再把粒種熱萃取出,製備中空聚亞醯胺顆粒。改變配方及反應條件,探討其對中空聚醯亞胺顆粒形態及其熱性質、結晶性等物性的影響。 由實驗結果得知,聚合物顆粒隨二胺溶液腫脹粒種的時間增加及反應器攪拌速率的增加而顆粒較不沾黏,在腫脹時間3小時及攪拌速率10000rpm時可獲得較不沾黏的聚醯亞胺顆粒;高分子型的穩定劑聚乙烯基烷酮比離子型界面活性劑硫酸鈉十二烷酯更可以穩定系統,製備出較不沾黏均一的中空聚合物顆粒;中空聚醯亞胺顆粒的殼層,隨著單體劑量的增加而有變厚,粒子粒徑也隨之增加,約在180nm至240nm左右,其3%的熱重損失介於530℃~580℃左右。
The objective of this work is to prepare polyimide particles with hollow void. Hollow polyimide particles were prepared by using monodisperse polystyrene as seeds, prepared by emulssionless polymerization. Diamine solution was swollen into seeds and then added dianhydride solution to proceed condensation polymerization, after dehydrating to imidization and extracting the seeds. We can get the hollow polyimide particles, subsequently. The effects by changing the recipes and reaction conditions, the morphology of the hollow polyimide particles, and physical properties, such as: thermal stability, crystallinity…etc., were investigated. From the experimental results, we can get the morphology with no aggregation by increasing the swelling time and stirring rate. Using PVP as a stabilizer can get better morphology of the hollow polyimide particles than that of SDS. The thickness and the size of the hollow polyimide particles were increased with the increasing of the amount of the added monomer and in the range between 180nm and 240nm . The 3% weight loss of particles was around 530 and 580℃.