摘要
以4-(4-羟基苯基)-2,3-二氮杂萘-1-酮、4,4’-二氟二苯甲酮和4-氨基苯酚为原料,通过两步一锅法合成了一种新型的氨基封端杂萘联苯聚芳醚酮(A-PPEK),采用差示扫描量热法(DSC)探究了其对间苯二酚基邻苯二甲腈(DPPH)的固化性能。相比于常用的芳香二胺固化剂4,4’-二氨基二苯砜(DDS),A-PPEK的5%热失重温度(T_(d5%))提高了69.3℃。另外,与DDS在400℃时快速升华不同,A-PPEK在相同温度下的质量保留率仍>95%,说明A-PPEK可以有效解决小分子固化剂高温下分解,容易在邻苯二甲腈树脂中形成缺陷的问题。一系列实验表明,以A-PPEK固化DPPH,体系具有优异的耐热性和加工流动性,当A-PPEK含量为DPPH质量的10%时,固化树脂的T_(d5%)可达553.2℃,玻璃化转变温度高于实验测试范围380℃,最低黏度可达0.167 Pa·s。
A novel amino terminated poly(phthalazinone ether ketone)(A-PPEK)was synthesized from 4-(4-hydroxylphenyl)(2H)-phthalazin-1-one,4,4'-difluoro benzophenone and 4-aminophenol by a two-step one pot method,and its curing performance for resorcinol phthalonitrile(DPPH)was then investigated by differential scanning calorimetry(DSC).Compared with commonly used aromatic diamine curing agent 4,4'-diaminodiphenyl sulfone(DDS),5%mass loss temperature(T_(d5%))of A-PPEK was increased by 69.3℃.Moreover,A-PPEK could still retain more than 95%of its mass at 400℃while DDS displayed rapid sublimation,suggesting that A-PPEK could effectively solve the problem of defects in phthalonitrile resin caused by the decomposition of small molecule curing agent at high temperature.Data from a series of tests showed that the system of DPPH cured with A-PPEK exhibited excellent heat resistance and processability.When A-PPEK content was 10%of DPPH mass,the T_(d5%)of the cured resin reaching 553.2℃,the glass transition temperature higher than the experimental test scope of 380℃,and the minimum viscosity up to 0.167 Pa·s.
作者
胡月
马守骏
蹇锡高
翁志焕
HU Yue;MA Shoujun;JIAN Xigao;WENG Zhihuan(State Key Laboratory of Fine Chemicals,School of Chemical Engineering,Dalian University of Technology,Dalian 116024,Liaoning,China;Shanxi Xinhua Chemical Defense Equipment Research Institute Co.,Ltd.,Taiyuan 030000,Shanxi,China)
出处
《精细化工》
EI
CAS
CSCD
北大核心
2023年第4期838-844,910,共8页
Fine Chemicals
基金
国家自然科学基金(51673033,51873027)
中央高校基本科研业务费(DUT20TD114)。
关键词
邻苯二甲腈树脂
杂萘联苯聚芳醚酮
氨基封端
耐高温
功能材料
phthalonitrile resin
poly(phthalazinone ether ketone)
amine termination
high-temperature resistant
functional materials
