Chen Liping, Luo Zhonglin, Wang Biaobing
Jiangsu Key Laboratory of Environmentally Friendly Polymeric Materials, Jiangsu Collaborative Innovation Center of Photovoltaic Science and Engineering, School of Materials Science and Engineering, Changzhou University, Changzhou 213164, China.
Materials (Basel). 2022 Apr 27;15(9):3155. doi: 10.3390/ma15093155.
A novel bio-based flame retardant designated AVD has been synthesized in a one-pot process via the reaction of 9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide (DOPO), vanillin (VN), and 2- aminobenzothiazole (ABT). The structure of AVD was confirmed using Fourier transform infrared spectroscopy (FTIR), and H and P nuclear magnetic resonance spectroscopy (NMR). The curing process, thermal stability, flame retardancy, and mechanical properties of the epoxy resin (EP) modified with AVD have been investigated comprehensively. The extent of curing, the glass transition temperature and the crosslinking density of the blend decreased gradually with increasing AVD content. The thermogravimetric analysis (TGA) was used to demonstrate that the presence of AVD reduced the thermal decomposition rate for EP and enhanced the formation of carbon residue during resin decomposition. A blend of 7.5 wt% AVD (0.52% phosphorus) displays a UL-94V-0 rating and a LOI of 31.1%. Reduction of the peak heat release rate, total heat release rate and total smoke production was 41.26%, 35.70%, and 24.03%, respectively, as compared to the values for pure EP. The improved flame retardancy of the flame retardant epoxy (FREP) may be attributed to the formation of a compact and continuous protective char layer into the condensed phase as well as the release of non-combustible gases and phosphorus-containing radicals from the decomposition of AVD in the gas phase. AVD is a new and efficient biobased flame retardant for epoxy with great prospects for industrial applications.
一种名为AVD的新型生物基阻燃剂通过9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)、香草醛(VN)和2-氨基苯并噻唑(ABT)的反应在一锅法中合成。使用傅里叶变换红外光谱(FTIR)以及氢和磷核磁共振光谱(NMR)对AVD的结构进行了确认。对用AVD改性的环氧树脂(EP)的固化过程、热稳定性、阻燃性和机械性能进行了全面研究。随着AVD含量的增加,共混物的固化程度、玻璃化转变温度和交联密度逐渐降低。热重分析(TGA)用于证明AVD的存在降低了EP的热分解速率,并提高了树脂分解过程中残炭的形成。7.5 wt% AVD(0.52%磷)的共混物具有UL-94 V-0等级和31.1%的极限氧指数。与纯EP的值相比,峰值热释放速率、总热释放速率和总产烟量分别降低了41.26%、35.70%和24.03%。阻燃环氧树脂(FREP)阻燃性的提高可能归因于在凝聚相中形成了致密且连续的保护性炭层,以及在气相中AVD分解释放出不可燃气体和含磷自由基。AVD是一种新型高效的环氧树脂生物基阻燃剂,具有广阔的工业应用前景。