反相非水乳液制备多孔聚酰亚胺微球  

PREPARATION OF POROUS POLYIMIDE MICROSPHERES IN NON-AQUEOUS INVERSE EMULSION

作　　者：刘妙青[1] 卢建军[1] 林立[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：《高分子学报》2013年第9期1226-1234,共9页Acta Polymerica Sinica

基　　金：国家重点基础研究发展计划(973计划;项目号2005CB221204)资助项目

摘　　要：在Span85/N,N-二甲基甲酰胺/液体石蜡稳定反相非水乳液体系中,以均苯四甲酸酐和4,4＇-二氨基二苯醚为单体,选用甲醇、二硫化碳作为致孔剂,制备多孔聚酰亚胺（PI）微球.通过SEM、量子化学模拟、粒径测试等手段考察致孔剂种类、致孔剂用量、吡啶/酸酐滴加速度及反应温度和单体浓度对致孔的影响.结果表明,选用二硫化碳、甲醇为致孔剂时所制得的微球形貌良好,但CS2为致孔剂时,所得到的微球孔道很少;而甲醇为致孔剂时,则得到了孔道明显的多孔PI微球.致孔的最佳条件为反应温度20℃,单体浓度10%,吡啶/酸酐滴加速度0.5 s/滴时,才可得到的形貌良好、分布均一的多孔PI微球.而且随着甲醇/液体石蜡的体积比增加,多孔PI微球比表面积也随着增大,最大可达29.38 m2/g.所得产物粒径分布在20~30μm之间,热稳定性良好,其起始热分解温度为517℃.Porous polyimide（PI） microspheres were prepared using carbon disulfide and ethyl ether as porogens.Porous PI microspheres derived from pyromellitic dianhydride（PMDA） and 4,4＇-diaminodiphenyl ether（ODA） were carried out in a non-aqueous emulsion system,in which liquid paraffin was the continuous phase and N,N-dimethylformamide（DMF） was the dispersed phase.The morphologies and chemical structures of the PI porous microspheres were characterized by scanning electron microscopy,quantum chemical simulation,infrared absorption spectroscopy,mercury porosimetry and thermal gravimetric analysis.The results indicated that the morphology of microspheres is good,when carbon disulfide or methanol is used as porogen.However,if carbon disulfide is used as porogen,the number of microsphere pores is small.If methanol is used as porogen,clear pore and porous PI microspheres can be obtained.Hydrogen bonding interaction existing between polyamic acid and ethyl ether plays a critical role in the pore formation process.The pore morphology is mainly controlled through keeping the consistency of curing rate and the evaporation rate.The best porogenic conditions： the temperature of system was 20 ℃,the monomer concentration was 10%,drop speed of pyridine / acetic anhydride was 0.5 s / drop.The specific surface of the porous microspheres is increased with increasing the ratio of ethyl ether / liquid paraffin,which can reach 29.38 m2/ g determined with mercury porosimetry.The average particle diameter is about 20 ~ 30 μm.The resulting samples possess good thermal stability with a decomposition onset temperature of about 517 ℃.

关 键 词：聚酰亚胺 反相非水乳液 多孔微球 

分 类 号：TB383.4[一般工业技术—材料科学与工程]