高耐热聚芳醚酮固化邻苯二甲腈树脂  

Curing of phthalonitrile resin with high-temperature resistant poly(phthalazinone ether ketone)

作　　者：胡月[1,2] 马守骏 蹇锡高 翁志焕[1] 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)

机构地区：[1]大连理工大学精细化工国家重点实验室化工学院,辽宁大连116024 [2]山西新华防化装备研究院有限公司,山西太原030000

出　　处：《精细化工》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)。

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.

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 

分 类 号：TQ323[化学工程—合成树脂塑料工业] TQ630