一种可熔融的烷基次膦酸复盐阻燃剂的合成及其在PBT中的应用研究  

Synthesis of a Meltable Alkylphosphinate Double Salt Flame Retardant and Its Application in PBT

作　　者：陈佳[1] 荣莉[1] 刘学清[1] 邹立勇[1] 刘继延[1] 周恒 CHEN Jia;RONG Li;LIU Xue-qing;ZOU Li-yong;LIU Ji-yan;ZHOU Heng(Key Laboratory of Optoelectronic Chemical Materials and Devices of Ministry of Education,School of Chemistry and Environmental Engineering,Jianghan University,Wuhan 430056,China)

机构地区：[1]江汉大学化学与环境工程学院,光电化学材料与器件教育部重点实验室,湖北武汉430056

出　　处：《塑料工业》2020年第2期21-25,78,共6页China Plastics Industry

基　　金：国家重点研发计划项目(项目编号2016YFB0401505)。

摘　　要：通过甲基亚膦酸单丁酯与环己烯的自由基加成,然后与氢氧化钠以及硫酸镁和硫酸锌成盐制备得到一种可熔融的烷基次膦酸复盐阻燃剂-甲基环己基次膦酸锌镁[MgZn(MHP)]。采用红外光谱(FTIR)、核磁氢谱(~1H NMR)以及X射线荧光光谱(XRF)等技术表征了目标产物,并通过熔融共混法制备MgZn(MHP)-PBT阻燃复合材料。添加质量分数为20%的MgZn(MHP)可使PBT的极限氧指数(LOI)由17. 7%提高至28. 2%,垂直燃烧测试达到UL94 V-0级别。微形量热测试表明MgZn(MHP)对PBT的热释放速率(HRR)抑制作用明显。热分解动力学结果表明,20%MgZn(MHP)-PBT复合材料在初始阶段的活化能比纯PBT的要低,而平均活化能则高于纯PBT。A meltable alkylphosphonate double salt flame retardant-magnesium zinc methylcyclohexyl-phosphinate [MgZn( MHP) ]was synthesized initially by radical addition reaction of n-butyl methylphosphonate with cyclohexene,followed by reacting with NaOH、MgSO4 and ZnSO4. The target product was characterized by fourier transforms infrared spectroscopy( FTIR) 、 hydrogen nuclear magnetic resonance(1 H NMR) and X-ray fluorescence spectrum( XRF). And the MgZn( MHP)-PBT composites were prepared by melt blending method. The limit oxygen index( LOI) of PBT containing 20% MgZn( MHP) increases from 17. 7% to 28. 2%,and the vertical burning test could pass UL94 V-0 rating. Microscale combustion calorimeter results indicate that MgZn( MHP) exhibites superior performance in the inhibition of heat release rate( HRR) for PBT. The results of thermal decomposition kinetics demonstrate that the20%MgZn( MHP)-PBT composite has lower activation energy( Ea) in initial decomposition stage but a higher average Eafor the whole stage comparing with pure PBT.

关 键 词：可熔融 烷基次膦酸复盐 聚对苯二甲酸丁二醇酯 阻燃 

分 类 号：TQ323.41[化学工程—合成树脂塑料工业]