一种新型烷基磷系阻燃剂的合成及其在尼龙6中的应用

Synthesis of A Novel Alkyl-substituted Phosphinate and Its Application in PA6

以次磷酸钠为原料合成异丁基次磷酸铝(A-MBPa)阻燃剂,利用氢核磁(1H NMR)、磷核磁(31P NMR)、元素分析、等离子发射光谱仪(i CP)及红外光谱仪确定了A-MBPa的结构,并通过熔融共混法制备出AMBPa阻燃尼龙6(PA6)复合材料。采用热重分析仪(TG)、极限氧指数(LOI)、垂直燃烧(UL94)及锥形量热仪等方法对其热性能及阻燃性能进行了表征。结果表明,随着A-MBPa添加量的增加,PA6/A-MBPa复合材料的热稳定性降低,热重测试后残余量增多;当A-MBPa添加量为20%时,PA6/A-MBPa复合材料的LOI为26.4%,UL94达到V-0级,且形成明显的炭层,此外PA6/A-MBPa复合材料的力学性能呈现出随着A-MBPa添加增多而降低的趋势。结果表明,A-MBPa在阻燃PA6体系中是一种有效的阻燃剂。

A phosphorus-containing compound of aluminum monoisobutylphosphinates （A-MBPa） was synthesized by using sodium hypophosphite as the raw material. The target product was confirmed by 31P nuclear-magnetic resonance （^31P NMR） ,^1H NMR, ultimate analysis, plasma emission spectrometer （ICP） and Fourier transform infrared spectroscopy （ FTIR ）, which confirmed the success synthesis of the target product. PA6/A-MBPa composites were prepared by melt blending method. Thermal and flame retardant properties were characterized by thermogravimetric analysis （TG）, limiting oxygen index （LOI） test, UL94 vertical burning test and cone calorimetry. The results show that thermal stability of PA6/A-MBPa decreases with the increase of the adding A-MBPa amount and the residue increases after TG test. When A-MB19a adding amount is 20% , the LOI value of PA6/A-MBPa composites is 26.4% , reaching UL94 V-0 rate, and a clear carbon layer is formed. Moreover the mechanical properties of the PA6/A-MBPa composite material decrease with the increasing addition of A-MBPa. The above results prove that A-MBPa is an effective flame retardant for PA6 matrix.