含醚键双二氮杂萘酮结构聚芳醚腈砜的合成与性能  

Synthesis and Properties of Poly(aryl ether nitrile sulfone)Containing Bis-Phthalazinone and Ether Moieties

作　　者：张振东 刘程[1,2] 安晓亮 陈曦 顾宏剑 赵文淇 蹇锡高 Zhendong Zhang;Cheng Liu;Xiaoliang An;Xi Chen;Hongjian Gu;Wenqi Zhao;Xigao Jian(Department of Polymer Materials,School of Chemical Engineering,Dalian University of Technology,Dalian 116024,China;Technology Innovation Center of High Performance Resin Materials,Liaoning Province,Dalian 116012,China)

机构地区：[1]大连理工大学化工学院高分子材料系,辽宁大连116024 [2]辽宁省高性能树脂材料专业技术创新中心,辽宁大连116012

出　　处：《高分子材料科学与工程》2024年第1期1-7,共7页Polymer Materials Science & Engineering

基　　金：国家自然科学基金重点基金资助项目(91860204);中央高校基本科研业务费(DUT22LAB605);辽宁省应用基础研究计划(22JH2/101300232);大连市创新基金(2022JJ12GX042)。

摘　　要：文中以含醚键双二氮杂萘酮结构化合物4,4’-双(氧基(1,4-苯撑))-双二氮杂萘-1(2H)酮-二苯醚(OBDHPZ)为类双酚单体,与4,4’-二氟二苯砜(DFS)和2,6’-二氟苯腈(DFBN)进行高温溶液缩聚反应,通过调节聚合物分子主链中砜基和氰基等的含量,合成了一系列不同腈砜比的含醚键双二氮杂萘酮联苯结构聚芳醚腈砜树脂(PBPENS),其N-甲基吡咯烷酮(NMP)溶液在25℃的特性黏度为0.63~0.90 dL/g。通过红外光谱、核磁共振氢谱和广角X射线衍射仪表征了所合成聚芳醚腈砜的结构;通过差示扫描量热仪和热失重分析仪分析了该类聚芳醚腈砜的热性能,聚合物的玻璃化转变温度(Tg)在322~325℃,5%热失重温度(Td5%)在485~500℃。该类聚合物在常温时可溶解于NMP、N,N-二甲基乙酰胺(DMAc)、氯仿等极性非质子有机溶剂;采用溶液浇筑法制备了含醚键双二氮杂萘酮结构聚芳醚腈砜薄膜,薄膜的拉伸强度可以达到56~65 MPa。A series of poly(aryl ether nitrile sulfone)s containing bis-phthalazinone and ether moieties(PBPENS)were synthesized by high-temperature-solution polymerization of 4,4'-(oxybis(4,1-phenylene))bis(phthalazin-1(2H)-one)-diphenyl ether(OBDHPZ),4,4'-difluorodiphenyl sulfone(DFS)and 2,6-difluorobenzonitrile(DFBN),by adjusting the mole ratio of sulfone and nitrile group in chain.The copolymers obtained have inherent viscosities in the range of 0.62~0.90 dL/g in N-methylpyrrolidone(NMP)at 25℃.The polymer structures were characterized by FT-IR,1H-NMR and WAXD.Furthermore,the thermal properties of PBPENSs were evaluated by differential scanning calorimeter(DSC)and thermal gravimetric analyzer(TGA),with the glass transition temperatures(Tg)and 5%mass retention(Td5%)ranged from 322℃to 325℃and 485℃to 500℃,respectively.Moreover,PBPENSs can be dissolved in polar non-protonic organic solvents such as NMP,N,N-dimethylacetamide(DMAc),chloroform and so on at room temperature.And PBPENS films prepared by solution casting method exhibit a tensile strength of 55~65 MPa.

关 键 词：双二氮杂萘酮 聚芳醚腈砜 合成 耐热性 溶解性 

分 类 号：TQ326.5[化学工程—合成树脂塑料工业]