双(4-氨基苯氧基)二甲基硅烷及其聚酰亚胺合成  

Synthesis of bis(p-aminophenoxy)dimethylsilane and silicone-containing polyimide

作　　者：段宏伟[1] 周浩然[1] 徐双平[2] 赵德明[1] 刘新刚[1] 林飞[1] 范勇[1] 

机构地区：[1]哈尔滨理工大学材料科学与工程学院高分子系,哈尔滨150040 [2]齐齐哈尔大学化学与化工学院,黑龙江齐齐哈尔161006

出　　处：《材料科学与工艺》2009年第3期436-440,共5页Materials Science and Technology

基　　金：国家自然科学基金重点项目(50137010);哈尔滨市科技人才研究专项资金项目(2007RFXXG024)

摘　　要：为了改善聚酰亚胺的加工性能,以对氨基酚和二氯二甲基硅烷为原料合成了一种含硅二胺活性单体双(4-氨基苯氧基)二甲基硅烷(简写APMSI),采用不同配比的APMSI和4,4’-二氨基二苯醚(ODA)混和胺与均苯四甲酸二酐(PMDA)共缩聚制得含硅聚酰亚胺.采用傅立叶变换红外光谱(FTIR)、核磁共振谱(1H和13C)、熔点测定仪对对乙酰氨基酚、双(4-氨基苯氧基)二甲基硅烷(APMSI)的结构进行了表征,其总产率达到67%.采用傅立叶变换红外光谱仪(FTIR)、差热分析仪(DTA)、热重分析仪(TG)和溶解实验分别对纯聚酰亚胺和含硅聚酰亚胺的结构、热性能和溶解性进行了表征.结果表明,含硅聚酰亚胺较纯聚酰亚胺耐热性低,但随含硅二胺单体增多而升高;其玻璃化转变温度随含硅二胺单体增多而大幅下降;其溶解性相对于纯聚酰亚胺有大幅提高.To improve the processability of polyimide （ PI）, taking p-amino-phenol and dimethyl dichlorosilane as raw materials, an activated monomer of bis（p-aminophenoxy） dimethylsilane （APMSI） containing silicon was prepared. Then the silicone-containing PI was synthesized from APMSI, pyromellitic dianhydride （PMDA） and 4,4＇ -oxydianilline （ODA） with different contents in N, N＇ -dimethylacetamide （DMAC）. The structure of p-acetaminophenol and APMSI was characterized by Fourier transform infrared spectroscopy （ FTIR） , nuclear magnetic resonance spectroscopy （ 1H NMR and 13 C NMR） and melting point apparatus, and the total yield of APMSI was 67%. The construction, thermal property and solution property of pure PI and silicone-containing PI were characterized by FFIR, differential thermal analyzer （DTA）, thermo-gravimetric analyzer （TGA） and solution experiment, respectively. Results illustrate that compared with the pure PI, the silicone-containing PI has lower heat resistance and highly improved dissolubility, and its heat resistance becomes higher with the increasing content of activated monomer containing silicon, while its glass transition temperature is decreased greatly.

关 键 词：对氨基酚 二氯二甲基硅烷 双(4-氨基苯氧基)二甲基硅烷 合成 含硅聚酰亚胺 

分 类 号：O634.4[理学—高分子化学] TQ323.7[理学—化学]