论文部分内容阅读
以三氯氧磷和新戊二醇等为原料,合成了一种新型磷氮型季铵盐(PAHAC),通过红外光谱(FTIR)、核磁共振氢谱(1H-NMR)和高分辨质谱(HRMS)表征化合物结构。利用PAHAC与钠基蒙脱土(Na-MMT)离子交换反应制备有机磷氮系-蒙脱土阻燃剂(PAHAC-MMT)。FTIR和X射线衍射(XRD)研究表明:PAHAC通过离子交换对蒙脱土进行了有机化改性,经20%质量分数的PAHAC改性后的MMT(20%PAHAC-MMT)层间距增至1.87 nm,20%PAHAC-MMT的热分解温度在310℃以上。透射电镜(TEM)分析结果表明,20%PAHAC-MMT经LDPE熔融插层,形成了插层-剥离型纳米复合材料。锥形量热测试结果表明有机磷氮系-蒙脱土/LDPE纳米复合材料具有良好的阻燃性能,其中20%PAHAC-MMT(7%)/LDPE的热释放速率峰值(PHRR)比LDPE降低了21%,热释放总量(THR)下降了9.5%。炭层的扫描电镜(SEM)分析结果表明,20%PAHAC-MMT/LDPE燃烧后能形成致密的炭层,起到良好的阻燃作用。
A new type of phosphorus-nitrogen-containing quaternary ammonium salt (PAHAC) was synthesized by using phosphorus oxychloride, neopentyl glycol and the like as raw materials, and their structures were characterized by FTIR, 1H-NMR and high resolution mass spectrometry HRMS) characterize the compound structure. The organophosphorus nitrogen-montmorillonite flame retardant (PAHAC-MMT) was prepared by the ion exchange reaction between PAHAC and sodium montmorillonite (Na-MMT). FTIR and X-ray diffraction (XRD) studies showed that PAHAC was modified by ion exchange to montmorillonite. The spacing of MMT (20% PAHAC-MMT) modified by 20% PAHAC increased to 1.87 nm, 20% PAHAC-MMT thermal decomposition temperature above 310 ℃. Transmission Electron Microscopy (TEM) results showed that 20% PAHAC-MMT was intercalated by LDPE and intercalated-exfoliated nanocomposites were formed. The results of cone calorimetry show that the organophosphate-montmorillonite / LDPE nanocomposites have good flame retardancy. The peak heat release rate (PHRR) of 20% PAHAC-MMT (7%) / LDPE is lower than that of LDPE 21%, total heat release (THR) decreased by 9.5%. Scanning electron microscopy (SEM) analysis of the carbon layer showed that 20% PAHAC-MMT / LDPE could form a dense carbon layer after burning, which played a good flame retardant effect.