High-Pressure Synthesis and Properties of Aliphatic−Aromatic Polyimides via Nylon-Salt-Type Monomers Derived from Aliphatic Diamines with Pyromellitic Acid and Biphenyltetracarboxylic Acid

High-Pressure Synthesis and Properties of Aliphatic−Aromatic Polyimides via Nylon-Salt-Type Monomers Derived from Aliphatic Diamines with Pyromellitic Acid and Biphenyltetracarboxylic Acid
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脂肪族二胺与均苯四酸和联苯四甲酸衍生的尼龙盐型单体高压合成脂肪族-芳香族聚酰亚胺及其性能

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发表时间:
1997
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通讯作者:
J. Watanabe
J. Watanabe
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作者:
Tatsuo Inoue;Yoshihiro Kumagai;M. Kakimoto;Y. Imai;J. Watanabe

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通过由具有6 - 12个亚甲基单元的脂肪族二胺和均苯四甲酸(PMA)和联苯四甲酸(BPA)组成的盐单体在220 MPa和250 °C下在高压下固态热缩聚5 h,容易地合成了具有明确结构的两个脂肪族系列的聚酰亚胺,其特性粘度为0.4 - 2.7 dL g-1。值得注意的是,缩聚反应在高压下在封闭反应容器中快速进行,除去水,主要在1小时内产生高分子量聚酰亚胺。还详细讨论了PMA和BPA基聚酰亚胺的热行为(熔融温度和玻璃化转变温度)和结晶度。
Two aliphatic series of polyimides having well-defined structures with inherent viscosities of 0.4−2.7 dL g-1 were readily synthesized by the solid-state thermal polycondensation under high pressure of the salt monomers composed of aliphatic diamines having 6−12 methylene units and both pyromellitic acid (PMA) and biphenyltetracarboxylic acid (BPA) under 220 MPa at 250 °C for 5 h. It is noteworthy that the polycondensation proceeded rapidly with the elimination of water in a closed reaction vessel under high pressure, producing high molecular weight polyimides mostly within only 1 h. The thermal behavior (melting temperature and glass transition temperature) and crystallinity of the PMA- and BPA-based polyimides are also discussed in detail.