选用4,4-二氨基二苯醚(ODA)、对苯二胺(PPD)及1,5-二氨基萘(NDA)3种二胺及二苯甲酮四羧酸二酐(BTDA)为单体,采用 Pluronic-F127/N,N-二甲基甲酰胺、司班85/液体石蜡非水乳液聚合首先制得聚酰亚胺(PI)微球.利用红外测试、扫描电子显微镜(SEM)及粒径测试等对 PI 微球的结构及形貌进行分析.结果表明,当使用不同的二胺与二酐 BTDA在非水乳液体系下均能成为PI微球,带有柔顺基团的二胺形成的PI 微球其形貌良好,而且分布比较均一,平均粒径为20μm 左右；而刚性较强的二胺合成微球其表面粗糙且形貌较差.产品仅经化学亚胺化处理亚胺化不完全,必须经进一步的热处理才能使完全亚胺化；亚胺化程度随温度的变化基本是呈 S 型.3种二胺 ODA、PPD 和 NDA 形成的 PI 微球的完全热亚胺化温度分别为300,330和370℃.
Non-aqueous emulsion was consist of N,N-dimethyl formamide/pluronic- F127-Span85/liquid paraf-fin.Poly(amic acid)precursors were fabricated by reacting with dianhydride (3,3’,4,4’-benzophenonetetracar-boxylic dianhydride)and diamines (diaminonaphthalene;1,4-phenylenediamine;4,4’-oxydianiline)in non-aqueous emulsion,and corresponding polyimide microspheres were prepared by chemical and thermal imidiza-tion.The chemical structures and morphologies of the PI(s)were characterized by means of Fourier transform infrared spectrum (FT-IR)and scanning electron microscopy (SEM).The result showed that the polyimide mi-crospheres with smooth surface and fine sphericity had been obtained by controlling the flexibility of the molec-ular chain which was synthesized by aromatic dianhydrides and aromatic diamines.The average diameters of particles was about 20μm.The complete imidization can obtain by “two-step imidization”i.e.,chemical fol-lowed by thermal imidization.The relationship of the imidization degree and the temperature of heat treatment showed the S-type curve.Meanwhile,by three kinds of diamine ODA,PPD and NDA form of PI microspheres, the temperature of complete imidization was achieved respectively in 300,330 and 370 ℃.
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