以9,10-二-氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)和乙二醇为主要原料,碘化钠为催化剂,设计合成了一种新型的桥链DOPO衍生物(Di-DOPO).采用红外光谱、差示扫描量热分析、热重分析、质谱分析、核磁共振等方法对其进行分析表征,确定了其结构.将该化合物与聚乳酸(PLA)共混,通过氧指数(LOI)测试、垂直燃烧、热重分析、锥形量热等手段考察了其对PLA的阻燃性能及热降解行为的影响.结果表明,Di-DOPO质量分数达到10％时就可以使阻燃PLA材料通过UL-94 V-0级,并能有效抑制PLA的熔滴现象,LOI值也由纯PLA的20％提升到36.3％.阻燃剂质量分数为5％,10％和15％时,热释放速率峰值(PHRR)分别降低了5.2％,12.7％,19.6％.当加入Di-DOPO后,阻燃PLA复合材料的热稳定性比纯PLA明显提高.综上,所制备的Di-DOPO阻燃剂对PLA具有很好的阻燃效果.
A new bridged DOPO derivative (Di-DOPO) was synthesized by the reaction between ethylene glycol (EG) and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) with sodium iodide as catalyst.The structure of the compound was characterized by FT-IR,DSC,TG,MS,1H-NMR,13C-NMR and 31p-NMR.Then,effects of the flame retardant properties and thermal degradation behavior of PLA based on the synthesized compound were investigated by limiting oxygen index (LOI),vertical burning test (UL-94),cone calorimeter test and TG test.The results indicate that the PLA composites with mass fraction 10％ of Di-DOPO could pass UL-94 V-0 rating,and the melting drop phenomenon of PLA is effective suppressed.Moreover,the LOI rises to 36.3％ from 20％ of pure PLA.In addition,the peak of heat release rate (PHRR) of PLA composites containing 5％,10％ and 15％ of Di-DOPO decreases by 5.2％,12.7％,19.6％,respectively.Furthermore,after the addition of Di-DOPO,the thermal stability of the flame retardant PLA composites is significantly improved as comparison to pure PLA.Overall,the flame retardant properties and thermal stability of PLA are significantly enhanced based on the developed product of Di-DOPO.
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