热自缩聚法合成超支化芳族聚酰亚胺及其性能研究

K. Senthil, Ryoya Hata, Kazuya Matsumoto, M. Jikei
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引用次数: 0

摘要

缩合剂的使用合成了ab2型超支化芳族聚酰亚胺。HBPI-AA是在相对低温下加热ab2型单体合成的超支化聚酰亚胺,通过凝胶渗透色谱(GPC)、光散射检测器和核磁共振测量对其进行了表征。ab2型单体4-(3,5-双(4-氨基苯氧基)苯氧基)邻苯二甲酸在140℃下成功地进行了热自缩聚,形成了超支化聚酰胺酸。聚酰胺的后续化学亚胺化反应得到了带有乙酰酰胺(HBPI-Ac)或亚胺末端(HBPI-Im)基团的超支化芳族聚酰亚胺。高分子量聚合物的形成是通过光散射检测器的凝胶渗透色谱测量证实的。所得聚合物具有良好的溶解性和较低的溶液粘度,这是典型的超支化聚合物。HBPI-Ac的分支度测定为0.48。此外,模型邻苯二甲酸化合物在120°C下的1h NMR测量表明,羧酸酐单元的形成促进了酰胺键的形成,导致超支化聚酰胺酸。HBPI-Im的失重温度为470℃,远高于HBPI-Ac(400℃)。HBPI-Im薄膜涂覆在玻璃板上,280℃加热10 min后不溶于酰胺类溶剂,可作为耐溶剂、热稳定的涂层应用于微电子工业。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Synthesis and Properties of Hyperbranched Aromatic Polyimides via Thermal Self-Polycondensation
hyperbranched aromatic polyimides synthesized from AB 2 type monomers the use of condensation agents. The HBPI-AA synthesized heating the AB 2 type monomer at a relatively low temperature chemical imidization the hyperbranched polyimides, characterized by gel permeation chromatography (GPC) a light scattering detector and NMR measurements. The thermal properties, the film foaming ability, the solubility change after heating The thermal self-polycondensation of 4-(3,5-bis(4-aminophenoxy)phenoxy)phthalic acid, an AB 2 type monomer, proceeded successfully at 140°C to form a hyperbranched poly(amic acid). The subsequent chemical imidization of the poly(amic acid) afforded hyperbranched aromatic polyimides bearing acetylamide ( HBPI-Ac ) or imide terminal ( HBPI-Im ) groups. The formation of high molecular weight polymers was confirmed by gel permeation chromatography measurements using a light scattering detector. The resulting polymers exhibited good solubility and low solution viscosity, which is typical for hyperbranched polymers. The degree of branching of HBPI-Ac was determined to be 0.48. Moreover, the 1 H NMR measurement of the model phthalic acid compound at 120 ° C suggested that the formation of carboxyl anhydride units facilitated the amide bond formation, resulting in the hyperbranched poly(amic acid). HBPI-Im showed the temperature for a 5 % weight loss at 470°C, which was much higher than that of HBPI-Ac (400°C). HBPI-Im fi lm, coated on a glass plate, became insoluble in amide solvents after heating at 280 °C for 10 min, indicating that it could be applied as a solvent-resistant and thermally stable coating in the microelectronics industry.
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