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Synthesis and characterization of phosphorus containing aromatic poly(amide-imide)s copolymers for high temperature applications

机译:高温应用中含磷芳族聚(酰胺-酰亚胺)共聚物的合成与表征

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摘要

A series of novel thermally stable poly(amide-imide)s (PAIs) based on non-coplaner diimide-diacid (DIDA) monomer is synthesized. These polymers are characterized by elemental analysis, FT-IR, ~1H-NMR, ~(13)C-NMR and ~(31)P-NMR spectroscopic techniques and their physical and thermal properties are also studied. Four different dianhydrides pyromellitic anhydride (PMDA)/3,3',4,4'-benzophenone tetracarboxylic dianhydride (BTDA)/l,4,5,8-naphthalene tetracarboxylic dianhy-dride (NTDA)/4,4'-oxydiphthalic anhydride (ODPA) and amino acid L-tryptophan are used to synthesize DIDA. The polymerization of DIDA with phosphorus containing triamines having phenyl moieties gives poly(amide-imide)s. The synthesized polymers are obtained in high yield and possessed inherent viscosity in the range 0.66-0.98 dL/g. These polymers display higher solubility in polar aprotic solvents, such as DMSO, NMP and DMF. In addition, the absorption edge values (λ0) obtained from their UV curves are determined, and all the resulting poly(amide-imide)s films exhibited high optical transparency. The glass transition temperature (T_g) of these polymers is recorded in the range 211-265 °C, initial decomposition temperature in excess of 435 °C and char yield at 800 °C in nitrogen ranged from 52 to 70 %. Wide angle X-ray diffraction showed that all the polymers are almost amorphous.
机译:合成了一系列基于非共平面二酰亚胺-二酸(DIDA)单体的新型热稳定聚(酰胺-酰亚胺)(PAI)。这些聚合物通过元素分析,FT-IR,〜1H-NMR,〜(13)C-NMR和〜(31)P-NMR光谱技术进行表征,并研究了它们的物理和热性能。四种不同的二酐均苯四甲酸酐(PMDA)/ 3,3',4,4'-二苯甲酮四羧酸二酐(BTDA)/ l,4,5,8-萘四甲酸二酐(NTDA)/ 4,4'-氧二邻苯二甲酸酐(ODPA)和氨基酸L-色氨酸用于合成DIDA。 DIDA与具有苯基部分的含磷三胺的聚合产生聚(酰胺-酰亚胺)。合成聚合物以高收率获得,并且具有0.66-0.98dL / g的比浓对数粘度。这些聚合物在极性非质子溶剂(如DMSO,NMP和DMF)中显示出更高的溶解度。另外,确定从它们的UV曲线获得的吸收边缘值(λ0),并且所有所得的聚(酰胺-酰亚胺)膜均显示出高的光学透明性。这些聚合物的玻璃化转变温度(T_g)记录在211-265℃的范围内,初始分解温度超过435℃,并且在氮气中在800℃下的炭产率为52-70%。广角X射线衍射表明所有聚合物几乎都是无定形的。

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