有机磷氮系蒙脱土/LDPE纳米复合材料的制备及阻燃性能
Preparation and flammability properties of phosphorus-nitrogen-montmorillonite/LDPE nanocomposites
-
摘要: 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(PAHACMMT)。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1.87nm, 20%PAHACMMT的热分解温度在310℃以上。透射电镜(TEM)分析结果表明, 20%PAHACMMT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%PAHACMMT(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%PAHACMMT/LDPE燃烧后能形成致密的炭层, 起到良好的阻燃作用。Abstract: A novel phosphorus-nitrogen quaternary ammonium salts (PAHAC) was synthesized with phoshorus oxychloride and neopentyl glycol as main raw materials. PAHAC was characterized by FTIR, 1H-NMR and HRMS. Montmorillonite (MMT) modified with PAHAC (PAHACMMT) was prepared by ion-exchanging of Na+-montmorillonite (Na-MMT) and PAHAC. FTIR and XRD indicate that PAHAC is intercalated with Na-MMT and the layer spacing and the decomposition temperature of MMT modified with 20wt% PAHAC (20%PAHACMMT) is 1.87nm and 310℃, respectively. The results of TEM show that the intercalated-exploitated nanocomposite of 20%PAHACMMT/LDPE is formed by melting intercalation blending LDPE with 20%PAHACMMT. The flame retardancy of phosphorus-nitrogenmontmorillonite/LDPE nanocomposites was investigated by cone calorimeter test. The results show that the flame retardancy properties of phosphorus-nitrogen-montmorillonite/LDPE nanocomposites are good. In comparison with LDPE, the peak heat release rates (PHRR) and the total heat release (THR) of 20%PAHACMMT(7%)/LDPE reduce by 21% and 9.5%, respectively. The results of SEM show that the compact and dense char is formed for 20%PAHACMMT/LDPE nanocomposite after combustion, which can inhibit burning effectively.