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New imide-based thermosets with propargyl ether groups for high temperature composite application
Polymer ( IF 4.6 ) Pub Date : 2022-06-07 , DOI: 10.1016/j.polymer.2022.125038
Timofey I. Kolesnikov , Alexandra M. Orlova , Fedor V. Drozdov , Alexander I. Buzin , Georgij V. Cherkaev , Alexander S. Kechekyan , Petr V. Dmitryakov , Sergey I. Belousov , Alexander A. Kuznetsov

Development of new thermosetting polyimides with good processability is highly demanded. Oligomers with two imide cycles (bisimides), containing propargyl ether groups using 4-aminophenyl propargyl ether were prepared for the first time. Bisimides were synthesized without using of toxic solvents in benzoic or acetic acids. Use of acids as solvent allows to combine synthesis of bisimides with reaction of removing tret-butyloxycarbonyl group from amine in one step. Chemical structure of bisimides was confirmed using 1H, 13C NMR, FT-IR and elemental analysis. Pre-polymers exhibited wide temperature processing window and good solubility in low boiling point organic solvents. Thermal curing was investigated using differential scanning calorimetry (DSC) and FT-IR analysis. Propargyl ether groups cross-link completely after 1 h at 300 °C. Thermogravimetric analysis (TGA) indicated that the temperatures of 10% weight loss of cured polymers in nitrogen and air atmosphere were in the ranges of 492–499 °C and 503–515 °C, respectively. Samples of Carbon fiber reinforced plastics (CFRP) were prepared using bisimides with propargyl ether groups and investigated by dynamic mechanical analysis (DMA) and scanning electron microscopy (SEM). CFRP demonstrated glass transition temperature in the range of 309–370 °C and homogeneous structure of cross-section sample. Therefore, new highly thermally stable thermosets with great processability, prepared by eco-friendly synthesis for using as high performance polymer matrix for CFRP were developed in our work.



中文翻译:

用于高温复合材料应用的具有炔丙基醚基的新型酰亚胺基热固性材料

高度需要开发具有良好加工性的新型热固性聚酰亚胺。首次使用 4-氨基苯基炔丙基醚制备了具有两个酰亚胺环的低聚物(双酰亚胺),其中包含炔丙基醚基团。双酰亚胺的合成不使用苯甲酸或乙酸中的有毒溶剂。使用酸作为溶剂允许在一个步骤中将双酰亚胺的合成与从胺中除去叔丁氧羰基的反应结合起来。使用1 H, 13确认双酰亚胺的化学结构C NMR、FT-IR 和元素分析。预聚物在低沸点有机溶剂中表现出宽的温度加工窗口和良好的溶解性。使用差示扫描量热法 (DSC) 和 FT-IR 分析研究热固化。炔丙基醚基团在 300 °C 下 1 小时后完全交联。热重分析 (TGA) 表明,固化聚合物在氮气和空气气氛中 10% 失重的温度分别在 492–499 °C 和 503–515 °C 范围内。使用具有炔丙基醚基团的双酰亚胺制备碳纤维增强塑料 (CFRP) 样品,并通过动态机械分析 (DMA) 和扫描电子显微镜 (SEM) 进行研究。CFRP 的玻璃化转变温度在 309–370 °C 范围内,且横截面样品结构均匀。所以,

更新日期:2022-06-10
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