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基于1,4-双（3,4-二羧基苯氧基）苯二酐（HQDPA）的可熔融加工半结晶聚酰亚胺：合成、结晶及熔融行为

Melt-Processable Semicrystalline Polyimides Based on 1,4-Bis(3,4-dicarboxyphenoxy)benzene Dianhydride (HQDPA): Synthesis, Crystallization, and Melting Behavior.

作者信息

Zhang Hongfei, Wang Wei, Chen Guofei, Zhang Anjiang, Fang Xingzhong

机构信息

Key Laboratory of Additive Manufacturing Materials of Zhejiang Province, Ningbo Institute of Material Technology and Engineering, Chinese Academy of Sciences, 1219 Zhongguan West Rd, Zhenhai District, Ningbo 315201, Zhejiang, China.

University of Chinese Academy of Sciences, 19 A Yuquan Rd, Shijingshan District, Beijing 100049, China.

出版信息

Polymers (Basel). 2017 Sep 6;9(9):420. doi: 10.3390/polym9090420.

DOI:10.3390/polym9090420
PMID:30965727
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC6418867/
Abstract

It is a great challenge to develop semicrystalline polyimides exhibited significant recrystallization ability and fast crystallization kinetics from the melt. A series of semicrystalline polyimides based on 1,4-bis(3,4-dicarboxyphenoxy)benzene dianhydride (HQDPA) and different diamines, including 1,3-bis(4-aminophenoxy)benzene (TPER), 1,4-bis(4-aminophenoxy)benzene (TPEQ), 4,4'-oxydianiline (4,4'-ODA) and 4,4'-bis(4-aminophenoxy)biphenyl (BAPB), end capped with phthalic anhydride were synthesized. Crystallization and melting behaviors were investigated by differential scanning calorimetry (DSC). The polyimide derived from HQDPA/TPER (PI-1) exhibited a glass transition temperature () at 190 °C and double melting temperatures (s) at 331 °C and 350 °C, and the polyimide derived from HQDPA/TPEQ (PI-2) displayed a at 214 °C and a at 388 °C. PI-1 and PI-2 showed significant recrystallization ability from melt and high crystallization rate by isothermal crystallization kinetics study, while polyimides based on 4,4'-ODA and BAPB lost crystallizability once taken to the melt. These polyimides also exhibited excellent thermo-oxidative stability with 5% weight loss temperature higher than 500 °C and good mechanical properties with tensile moduli of 2.0⁻3.3 GPa, tensile strengths of 85⁻105 MPa and elongations at break of 5⁻18%. PI-1 also possessed outstanding melt flowability with less than 300 Pa·s around 370 °C by rheological measurements.

摘要

开发具有显著重结晶能力和快速熔体结晶动力学的半结晶聚酰亚胺是一项巨大挑战。合成了一系列基于1,4-双(3,4-二羧基苯氧基)苯二酐(HQDPA)和不同二胺（包括1,3-双(4-氨基苯氧基)苯(TPER)、1,4-双(4-氨基苯氧基)苯(TPEQ)、4,4'-二氨基二苯醚(4,4'-ODA)和4,4'-双(4-氨基苯氧基)联苯(BAPB)）并以邻苯二甲酸酐封端的半结晶聚酰亚胺。通过差示扫描量热法(DSC)研究了结晶和熔融行为。由HQDPA/TPER衍生的聚酰亚胺(PI-1)在190℃表现出玻璃化转变温度(Tg)，在331℃和350℃表现出双重熔融温度(Tm)，由HQDPA/TPEQ衍生的聚酰亚胺(PI-2)在214℃表现出Tg，在388℃表现出Tm。通过等温结晶动力学研究，PI-1和PI-2显示出显著的熔体重结晶能力和高结晶速率，而基于4,4'-ODA和BAPB的聚酰亚胺一旦熔融就失去了结晶性。这些聚酰亚胺还表现出优异的热氧化稳定性，5%失重温度高于500℃，并具有良好的机械性能，拉伸模量为2.0⁻3.3 GPa，拉伸强度为85⁻105 MPa，断裂伸长率为5⁻18%。通过流变学测量，PI-1在370℃左右还具有小于300 Pa·s的出色熔体流动性。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e96a/6418867/d4565c758477/polymers-09-00420-g012.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e96a/6418867/d4565c758477/polymers-09-00420-g012.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e96a/6418867/128fc48610d4/polymers-09-00420-sch001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e96a/6418867/893611aff8bb/polymers-09-00420-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e96a/6418867/4814286523f1/polymers-09-00420-g002.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e96a/6418867/fa96cd1f8ac4/polymers-09-00420-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e96a/6418867/a08ff7793ba3/polymers-09-00420-g008.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e96a/6418867/d9d2da32364a/polymers-09-00420-g009.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e96a/6418867/fd5cb0708d11/polymers-09-00420-g010.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e96a/6418867/d4565c758477/polymers-09-00420-g012.jpg

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