摘要
通过己二酸(AA)和二乙烯三胺(DETA)改性制得了一种氨基功能化氢氧化镁(DETA-AA-MH),并将其用作环氧树脂固化剂。采用FTIR、XRD、固体核磁、纳米粒径分析仪、SEM和TGA对DETA-AA-MH的化学结构、形貌以及热稳定性进行了表征,并通过FTIR和DSC分析得到环氧树脂(DGEBA)和DETA-AA-MH发生固化反应的最佳质量分数分别为84.03%和15.97%,热固化实验分析得到最佳反应条件为:预固化温度及时间(80℃/0.5 h)和后固化温度及时间(110℃/3 h)。LOI测试分析结果表明,DGEBA/DETA-AA-MH较DGEBA/DETA的LOI提高了10.15%。采用SEM和EDS对环氧树脂燃烧后的炭残留物进行分析,结果表明,在燃烧过程中DETA-AA-MH促进保护碳层的形成。机械性能测试表明,DGEBA/DETA-AA-MH(固化剂质量分数15.97%)与DGEBA/DETA(固化剂质量分数7.38%)对比发现其弯曲强度、弯曲模量和冲击强度分别提高了663.64%、49.92%、235.77%。
A novel amine-functionalized curing agent for epoxy resin( EP) based on magnesium hydroxide( DETA-AA-MH) was obtained by successive treatment of magnesium hydrate( MH) with hexanedioic acid and diethylenetriamine( DETA). DETA-AA-MH was characterized by Fourier transform infrared spectroscopy( FTIR),X-ray power diffraction( XRD),solidstate nuclear magnetic resonance( SSNMR) technique,nano particle analyzer,scanning electron microscope( SEM) and thermogravimetric analysis( TGA). The curing reaction was investigated by FTIR and differential scanning calorimeter( DSC). The best mass ratio between epoxy resin( DGEBA) and DETA-AA-MH was 84. 03% and 15. 97%,and the optimum curing conditions were that the precured reaction was carried out at 80 ℃ for 0. 5 h and the post curing was performed at 110 ℃ for 3 h. Flame retardance of the EPs was evaluated by LOI tests,the LOI value of DGEBA/DETA-AA-MH was an improvement of10. 15% compared with that of DGEBA/DETA. In addition,the char residue of epoxy resin after combustion was characterized by SEM and EDS. The results showed that DETA-AA-MH could promotethe char formation served as a protective char layer during burning. The experiments for determining the mechanic properties of DETA-AA-MH cured EPs were also conducted,which indicated that compared to the properties of EP containing 7. 38% DETA( mass fraction),the flexural strength,flexural modulus and impact strength of EP containing 15. 97% DETA-AA-MH( mass fraction) efficiently increased by 663. 64%,49. 92% and 235. 77%,respectively.
作者
高承永
张哲
刘雅妮
杨志旺
雷自强
马德龙
郭幸
徐小欢
GAO Cheng-yong ZHANG Zhe LIU Ya-ni YANG Zhi-wang LEI Zi-qiang MA De-long GUO Xing XU Xiao-huan(Key Laboratory of Eco-Environment Related Polymer Materials of Ministry of Education, Key Laboratory of Polymer Materials of Gansu Province, College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070, Gansu , China College of Science, Gansu Agricultural University, Lanzhou 730070, Gansu, China)
出处
《精细化工》
EI
CAS
CSCD
北大核心
2017年第10期1093-1101,共9页
Fine Chemicals
基金
国家自然科学基金(No.21174114)~~
关键词
环氧树脂
氢氧化镁
固化剂
功能材料
epoxy resin
magnesium hydroxide
curing agent
functional materials