中国塑料 ›› 2013, Vol. 27 ›› Issue (09): 57-62 .DOI: 10.19491/j.issn.1001-9278.2013.09.013

• 材料与性能 • 上一篇    下一篇

含吡啶环二胺及其可溶性聚酰亚胺的制备与表征

赵丽萍 寇开昌 卓龙海 王益群   

  1. 西北工业大学
  • 收稿日期:2013-05-06 修回日期:2013-06-23 出版日期:2013-08-26 发布日期:2013-08-26

Preparation and Characterization of Soluble Polyimide Based on a Novel Pyridine-containing Aromatic Diamine

  

  • Received:2013-05-06 Revised:2013-06-23 Online:2013-08-26 Published:2013-08-26

摘要: 以对羟基苯乙酮和苯甲醛为原料,通过亲核取代反应、改进的Chichibabin反应和水合肼催化还原合成了一种新型含吡啶环的芳香二胺4-苯基-2,6-双[4-(4-胺基苯氧基)苯]吡啶(ρ-PAPP),以N,N-二甲基甲酰胺(DMF)为溶剂,将ρ-PAPP与双酚A型二酐(BPADA)通过2步法合成了含吡啶环的新型聚酰亚胺。用红外光谱、差示扫描量热分析、热重分析、X射线衍射、溶解性测试等对聚合物的结构和性能进行了表征。结果表明,所得聚合物在1780、1723、1376 cm-1左右出现了聚酰亚胺的特征吸收峰;实验所得的聚酰亚胺能很好地溶解在常见有机溶剂中;玻璃化转变温度为191.2 °C;氮气气氛中,热失重10 %时的温度为473.8 °C,800 °C的残炭率为43 %;同时还有较好的力学性能,拉伸强度为98.5 MPa,拉伸模量为1.24 GPa,吸水率为0.67 %。

关键词: 制备, 含吡啶环二胺, 聚酰亚胺, 可溶性

Abstract: A novel pyridine-containing aromatic diamine monomer,4-phenyl-2,6-bis[4-(4-aminoph enoxy) phenyl]pyridine (ρ-PAPP) was successfully synthesized via nucleophilic substitution reaction, modified Chichibabin reaction, and catalytic reduction with hydrazine monohydrate,4-hydroxyacetophenone and benzaldehyde. Based on this, a pyridine-containing polyimide was synthesized via conventional two-step method by using ρ-PAPP as a diamine monomer, 2,2-bis[4-(3,4dicarboxyphenoxy)phenyl] propane dianhydride as a dianhydride monomer in N,N-dimethylformamide(DMF).The structure and properties of the polymer were characterized by FTIR, DSC, TGA, XRD, solubility testing. There were characteristic peaks of polyimide around 1780、1723、1378 cm-1 in the FTIR spectrum. The polyimide was soluble in common organic solvents. The polyimide had good thermal stability with glass transition temperature(Tg) of 191.2 °C, the temperature at 10 % weight loss was 473.8 °C in nitrogen atmosphere and the residual mass at 800 °C was 43 %. The other properties included tensile strengths of 98.5 MPa, tensile modulus of 1.24 GPa, and water uptake of 0.67 %.

Key words: preparation, pyridine-containing diamine, polyimide, solubilty

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