Chen Chin-Hsing, Chiang Chin-Lung
Department of Chemical and Materials Engineering, Chinese Culture University, Yang-Ming-Shan, Taipei City 11114, Taiwan.
Green Flame Retardant Material Research Laboratory, Department of Safety, Health and Environmental Engineering, Hung-Kuang University, Taichung 433, Taiwan.
Polymers (Basel). 2019 Apr 19;11(4):720. doi: 10.3390/polym11040720.
The NCO functional group of 3-isocyanatoproplytriethoxysilane (IPTS) and the OH functional group of 10-(2,5-dihydroxyphenyl)-10H-9-oxa-10-phospha-phenantbrene-10-oxide (DOPO-BQ) were used to conduct an addition reaction. Following completion of the reaction, triglycidyl isocyanurate (TGIC) was introduced to conduct a ring-opening reaction. Subsequently, a sol-gel method was used to initiate a hydrolysis-condensation reaction on TGIC-IPTS-DOPO-BQ to form a hyperbranched nitrogen-phosphorous-silicon (HBNPSi) flame retardant. This flame retardant was incorporated into a polyurethane (PU) matrix to prepare a hybrid material. Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), limiting oxygen index (LOI), UV-VIS spectrophotometry, and Raman analysis were conducted to characterize the structure and analyze the transparency, thermal stability, flame retardancy, and residual char to understand the flame retardant mechanism of the prepared hybrid material. After the flame retardant was added, the maximum degradation rate decreased from -36 to -17 wt.%/min, the integral procedural decomposition temperature (IPDT) increased from 348 to 488 °C, and the char yield increased from 0.7 to 8.1 wt.%. The aforementioned results verified that the thermal stability of PU can be improved after adding HBNPSi. The LOI analysis indicated that the pristine PU was flammable because the LOI of pristine PU was only 19. When the content of added HBNPSi was 40%, the LOI value was 26; thus the PU hybrid became nonflammable.
利用3-异氰酸酯基丙基三乙氧基硅烷（IPTS）的NCO官能团和10-(2,5-二羟基苯基)-10H-9-氧杂-10-磷杂菲-10-氧化物（DOPO-BQ）的OH官能团进行加成反应。反应完成后，引入三缩水甘油基异氰脲酸酯（TGIC）进行开环反应。随后，采用溶胶-凝胶法在TGIC-IPTS-DOPO-BQ上引发水解缩合反应，形成超支化氮-磷-硅（HBNPSi）阻燃剂。将该阻燃剂引入聚氨酯（PU）基体中制备杂化材料。通过傅里叶变换红外光谱（FTIR）、热重分析（TGA）、极限氧指数（LOI）、紫外-可见分光光度法和拉曼分析对其结构进行表征，并分析透明度、热稳定性、阻燃性和残炭情况，以了解所制备杂化材料的阻燃机理。添加阻燃剂后，最大降解速率从-36降至-17 wt.%/min，积分程序分解温度（IPDT）从348升高至488℃，残炭率从0.7 wt.%提高至8.1 wt.%。上述结果证实，添加HBNPSi后PU的热稳定性得以提高。LOI分析表明，纯PU易燃，因为其LOI仅为19。当HBNPSi的添加量为40%时，LOI值为26，此时PU杂化材料变为不可燃。
