苯磷酰二硅油的合成及阻燃聚碳酸酯

Synthesis of Phenylphosphoryl Disiloxane Oil and Its High Flame Retardancy for Polycarbonate

以苯基磷酰二氯和单羟丙基硅油为反应基体,通过亲核取代反应合成了苯磷酰二硅油(SiP-FR),然后以SiP-FR为阻燃剂,通过熔融共混的方法在双辊密炼机上制备了聚碳酸酯基共混阻燃材料。采用红外光谱和核磁共振磷谱表征了SiP-FR的化学结构;垂直燃烧和极限氧指数(LOI)测试结果表明,当添加2.2 phr阻燃剂时,共混材料可通过UL-94 V-0等级测试,LOI值达到29%;通过锥形量热仪分析了燃烧行为,发现阻燃剂的加入提高了共混材料的抑烟性能并降低了火灾危险性;采用热重红外联用与场发射扫描电子显微镜、拉曼光谱探究了阻燃机理,研究结果表明SiP-FR起到了气相与凝聚相协同阻燃的效果。

Phenylphosphoryl disiloxane oil(SiP-FR)was synthesized by nucleophilic substitution reaction between phenylphosphonic dichloride and monohydroxypropyl silicone oil.Polycarbonate/SiP-FR blends were prepared via melt blending method by an internal mixer.The chemical structure of SiP-FR was characterized by FT-IR and 31P-NMR.The flame retardant properties were explored by vertical burning test and limit oxygen index(LOI)test.The results show that the blends pass the UL-94 V-0 rate and the LOI value reaches 29%in the case of 2.2%SiP-FR loading level.The combustion behaviors of the blends were investigated by cone calorimeter test,and the results confirm that the smoke suppression performance is improved and the fire risk is reduced with the incorporation of SiP-FR.The flame retardant mechanism was investigated by TG-IR,FE-SEM and Raman spectroscopy.The results show that SiP-FR plays a synergistic flame retardant effect including gas phase and condensed phase.