香草醛基苯并噁嗪树脂的绿色合成及性能  

Green Synthesis and Properties of Vanilla-Aldehyde-Based Benzoxazine Resins

作　　者：杨林长青 李正山 刘宏 孔庆红[1,2] YANG Linchangqing;LI Zhengshan;LIU HONG;KONG Qinghong(School of the Environment and Safety Engineering,Jiangsu University,Zhenjiang 212013,China;School of Emergency Management,Jiangsu University,Zhenjiang 212013,China)

机构地区：[1]江苏大学环境与安全工程学院,江苏镇江212013 [2]江苏大学应急管理学院,江苏镇江212013

出　　处：《塑料工业》2024年第6期49-54,109,共7页China Plastics Industry

基　　金：江苏大学应急管理学院专项科研项目(KY-B-06)。

摘　　要：为探索六元环及其数量对苯并噁嗪树脂阻燃性和热性能的影响,通过绿色溶剂合成了香兰素-甘氨酸钠型苯并噁嗪单体(XG-BOZ,不含六元环)、香兰素-烟酰胺型苯并噁嗪单体(XY-BOZ,单六元环)、香兰素-二氨基二苯基甲烷型苯并噁嗪单体的合成(XD-BOZ,2个六元环)和香兰素-三聚氰胺型苯并噁嗪单体(XS-BOZ,3个六元环)。热分析和燃烧性能测试表明,XY-BOZ的热性能和阻燃性优于XG-BOZ、XD-BOZ和XS-BOZ。XY-BOZ在氮气下的700℃时残炭率为60.9%,其热释放速率峰值为64.6 W/g,热释放总量为6.8 kJ/g,理论极限氧指数(LOI)为41.8%。测试了XY-BOZ和XG-BOZ在不同加热速率的热分解行为,通过热降解动力学计算法(Flynn-Wall-Ozawa法)计算出在质量转化率为5%时,单六元环的XY-BOZ的降解反应的表观活化能(E_(a)为140 kJ/mol),无六元环的XG-BOZ的E_(a)为50.7 kJ/mol,比单六元环XY-BOZ的E_(a)低了63.8%。To explore the effects of six-membered rings and their quantities on the flame retardancy and thermal properties of benzoxazine resins,vanillin-and sodium-glycinate-based benzoxazine monomer(XG-BOZ,without six-membered ring),vanillin-and nicotinamide-based benzoxazine monomer(XY-BOZ,single six-membered ring),vanillin-and diaminodiphenylmethane-based benzoxazine monomer(XD-BOZ,two six-membered rings),vanillin-and melamine-based benzoxazine monomer(XS-BOZ,three six-membered rings)were synthesized by green solvents.Thermal analysis and combustion performance tests show that the thermal performances and flame retardancy of XY-BOZ are better than those of XG-BOZ,XD-BOZ and XS-BOZ.At 700℃under nitrogen,the carbon residue rate of XY-BOZ is 60.9%,the peak heat release rate is 64.6 W/g,the total heat release is 6.8 kJ/g,and the theoretical limited oxygen index(LOI)is 41.8%.The thermal decomposition behaviors of XY-BOZ and XG-BOZ at different heating rates are tested.According to the thermal degradation kinetics calculation method(Flynn-Wall-Ozawa method),when the mass conversion is 5%,the apparent activation energy(E_(a))of the degradation reaction of XY-BOZ with single six-membered ring is 140 kJ/mol,while that of XG-BOZ without six-membered ring is 50.7 kJ/mol.The E_(a) of XG-BOZ is 63.8%lower than that of XY-BOZ.

关 键 词：香草醛 苯并噁嗪 噁嗪环 热降解动力学 热性能 阻燃性 

分 类 号：TQ323[化学工程—合成树脂塑料工业]