非水乳液法制备结构不同的聚酰亚胺微球  

Preparation of different structures polyimide microspheres in non-aqueous inverse emulsion

作　　者：刘妙青[1] 卢建军[1] 李兴南[1] 黄伟[1] 

机构地区：[1]太原理工大学教育部与山西省煤科学与技术重点实验室,太原030024

出　　处：《功能材料》2014年第9期117-121,共5页Journal of Functional Materials

基　　金：国家重点基础研究发展计划(973计划)资助项目(2005CB221205)

摘　　要：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 paraffin.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 imidization.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 microspheres with smooth surface and fine sphericity had been obtained by controlling the flexibility of the molecular 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 followed 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 ℃.

关 键 词：非水乳液 聚酰亚胺微球 亚胺化 

分 类 号：TQ246.3[化学工程—有机化工]