Preparation of monodisperse fully aromatic polyimide particles via the polycondensation of diethyl hexafluoroisopropylidenediphthalate with 4,4′-diaminodiphenylether in ethylene glycol
Preparation of monodisperse fully aromatic polyimide particles via the polycondensation of diethyl hexafluoroisopropylidenediphthalate with 4,4′-diaminodiphenylether in ethylene glycol
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DOI：
10.1038/s41428-018-0156-1
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发表时间：
2018-12
期刊：
影响因子：
2.8
通讯作者：
Shinji Watanabe;Kozue Okamoto;Takeshi Namikoshi;Yoshihito Kohari;Miki Murata
中科院分区：
文献类型：
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作者：
Shinji Watanabe;Kozue Okamoto;Takeshi Namikoshi;Yoshihito Kohari;Miki Murata
以聚乙烯吡咯烷酮（PVP）为位向稳定剂，以邻苯二甲酸二乙酯（6FE）和4,4′-氧二胺（ODA）为原料，在乙二醇中一步缩聚制得全芳香烃聚酰亚胺颗粒。由于单体可溶于乙二醇，而聚酰亚胺不溶于乙二醇，聚酰亚胺颗粒在缩聚过程中逐渐增大。通过改变PVP的分子量和用量来控制其粒径和粒径分布。随着稳定剂浓度的增加和分子量的增加，稳定剂的粒径减小。此外，溶剂组成影响颗粒大小，即随着作为助溶剂的甘油体积的增加，颗粒大小减小。通过改变PVP和甘油的用量，得到了粒径为8.5 ~ 1.8 μm的单分散颗粒。
Fully aromatic polyimide particles were obtained in a single step via the polycondensation of diethyl (hexafluoroisopropylidene)diphthalate (6FE) and 4,4′-oxydianiline (ODA) using polyvinylpyrrolidone (PVP) as a steric stabilizer in ethylene glycol. Since the monomers are soluble in ethylene glycol, but the polyimide is insoluble, the polyimide particles grew gradually during the polycondensation process. The particle size and size distribution were controlled by varying the molecular weight and amounts of PVP. The particle size decreased with both increasing concentration and increasing molecular weight of the stabilizer. Furthermore, the solvent composition affected the particle size, i.e., the particle size decreased with increasing volume of glycerol as a cosolvent. Monodisperse particles (diameter: 8.5–1.8 μm) were obtained by varying the amounts of PVP and glycerol.