摘要
以4,4′-二苯基联二氮杂萘酮(DBD),4-(4-羟基苯基)-2,3-二氮杂萘-1-酮(DHPZ),4,4′-二氟二苯酮(DFK),4,4′-二氟二苯砜(DFS)为单体,进行高温溶液缩聚反应,DBD与DHPZ两种类双酚单体的物质的量比为8∶2,通过调节DFK与DFS的配比,合成了一系列含联苯基双二氮杂萘酮联苯结构共聚芳醚砜酮(PPDESKs)树脂。采用核磁共振氢谱、傅里叶变换红外光谱和广角X射线衍射等表征了PPDESKs的分子结构,并通过差示扫描量热仪和热重分析仪研究了该系列PPDESKs的热性能。结果表明,PPDESKs的玻璃化转变温度(Tg)为322~362℃,随砜基含量的提高而升高,氮气气氛下的初始分解温度为443~468℃,5%热失重温度最高可达505℃。对PPDESKs进行溶解性能测试,发现其可溶解在四氯乙烷和N-甲基吡咯烷酮强极性非质子有机溶剂中。采用溶液浇铸法制膜,并测试了聚合物薄膜的拉伸性能,聚合物薄膜的拉伸弹性模量为0.90~1.47 GPa,随砜基含量增加而增加;拉伸强度为72~82 MPa,断裂伸长率为8.39%~18.92%,且随着酮羰基含量的增加而增大。
The high-temperature solution polycondensation of diphenyl-biphthalazin-dione(DBD),4-(4-hydroxy-phenyl)-2Hphthalazin-1-one(DHPZ),4,4′-difluorodiphenylketone(DFK),and 4,4′-difluorodiphenyl sulfone(DFS)was carried out,and the molar ratio of DBD to DHPZ biphenol-like monomers was 8∶2.By adjusting the molar ratio of DFK to DFS,a series of copoly(aryl ether sulfone ketone)containing diphenyl-biphthalazin-dione structure(PPDESKs)were synthesized.The molecular structures of the PPDESKs were characterized by nuclear magnetic resonance hydrogen spectroscopy,Fourier transform infrared spectroscopy and wide-angle X-ray diffraction,and the thermal properties of PPDESKs were investigated by differential scanning calorimetry and thermal gravimetric analyzer,with the glass transition temperature(Tg)in the range of 322-362℃which increases with the increase of sulfone content,initial decomposition temperature between 443℃and 468℃in nitrogen atmosphere,and 5%mass loss temperature up to 505℃.Conduct solubility of PPDESKs was tested.It is found that the resultant copolymers exhibited good solubility in strong polar aprotic organic solvents,such as tetrachloroethane and N-methyl pyrrolidone.The polymer films were prepared by solution casting method,and their tensile properties were tested.And the tensile modulus of the polymer films is ranged from 0.90 GPa to 1.47 GPa,decreasing with the increase of sulfone group content.However,the tensile strength and the elongation at break of the polymer films are in the range of 72-82 MPa and 8.39%-18.92%,respectively,enhancing with the increase of ketone carbonyl group content.
作者
陈曦
刘程
顾宏剑
刘乾
张守海
蹇锡高
Chen Xi;Liu Cheng;Gu Hongjian;Liu Qian;Zhang Shouhai;Jian Xigao(Department of Polymer Materials,School of Chemical Engineering,Dalian University of Technology,Dalian 116024,China;Technology Innovation Center of High Performance Resin Materials,Dalian 116012,China)
出处
《工程塑料应用》
CAS
CSCD
北大核心
2023年第6期1-8,共8页
Engineering Plastics Application
基金
国家自然科学重点基金项目(91860204)
中央高校基本科研业务费资助项目(DUT22LAB605)
辽宁省应用基础研究计划项目(22JH2/101300232)。
关键词
联苯基双二氮杂萘酮
聚芳醚砜酮
溶液缩聚
热性能
溶解性能
拉伸性能
diphenyl-biphthalazin-dione
poly(aryl ether sulfone ketone)
solution polycondensation
thermal property
solubility
tensile property
