摘要
以三氯氧磷和双酚A为原料制备了具有超支化结构的聚磷酸酯阻燃剂(HPPEA),通过红外(FTIR),核磁(1H-NMR,31P-NMR)及热重分析表征了产物的结构和热稳定性.将HPPEA与三聚氰胺聚磷酸盐(MPP)进行复配,通过熔融共混法制备阻燃尼龙6,通过氧指数法和垂直燃烧法测试了其阻燃性能,采用热重分析(TGA)研究其热分解过程及成炭性能,采用扫描电镜(SEM)观察了其炭层形貌,通过旋转流变仪测试阻燃尼龙6的熔体黏度.结果表明,HPPEA与MPP对尼龙6起到了协同成炭的作用,使尼龙6在空气中的热稳定性和成炭量高于氮气中,在空气中600℃高温下添加30 wt%复合阻燃剂的尼龙6成炭量可达16.4 wt%,氮气中为13.6 wt%.20 wt%复合阻燃剂的加入即可使尼龙6氧指数由21.1提高到27.3,并且通过UL-94 V-0级.对降解动力学、炭层形貌和流变行为研究表明HPPEA的添加促进了尼龙6在降解过程中的交联成炭,提高了炭层致密性,阻碍了热和可燃气体传递,因而提高了阻燃性能.
A hyperbranched polyphosphate bisphenol-A ester flame retardant(HPPEA) was prepared by using phosphorus oxychloride and bisphenol-A.The structure and thermal stability of the product were characterized by Fourier transform infrared spectrometer(FTIR),nuclear magnetic resonance spectrometer(1H-NMR,31P-NMR) and thermogravimetric analysis(TGA).Branching degree of HPPEA determined by 31P-NMR spectrogram was about 51%.HPPEA combined with melamine pyrophosphate(MPP) was incorporated into polyamide 6(PA6).The flame retardant and thermal properties of the flame retardant PA6(FR-PA6) were studied through limiting oxygen index(LOI) and UL-94 vertical burning and TGA tests.The results showed that the LOI for flame retardant PA6 was improved to 27.3 from 21.1 for PA6,and UL-94 V-0 rating was achieved with 20 wt% flame retardant.According to TGA results,the char yield of FR-PA6 at 600℃ was also increased to 16.4 wt% in air atmosphere and 13.6 wt% in N2.Combining with the study of kinetics of thermal degradation and complex viscosity of FR-PA6 samples,clearly synergistic effect existed between HPPEA and MPP,which improved cross linking and char forming of PA6.Furthermore,morphology of char residues of FR-PA6 samples was also investigated by SEM method.Honeycomb and compact char layer was found which effectively protects the internal structure,inhibits the heat transmission and reduces the fuel gas during combustion.
出处
《高分子学报》
SCIE
CAS
CSCD
北大核心
2011年第1期55-62,共8页
Acta Polymerica Sinica
基金
国家自然科学基金(基金号20804056)
宁波市自然科学基金(基金号2009A610051)资助项目
关键词
超支化
聚磷酸双酚A酯
阻燃剂
尼龙6
成炭
Hyperbranched
Polyphosphate bisphenol-A ester
Flame retardant
Polyamide 6
Char forming