磷酰胺酯类化合物的合成及阻燃性能

Synthesis and Flame Retardant Properties of Phosphoramidates

以三氯氧磷、1,3-丙二醇、N-羟乙基哌嗪为原料,合成了磷酰胺酯类化合物PN1,并利用PN1与氯磷酸二乙酯的亲核反应制备了磷酰胺酯类化合物PN2.采用核磁共振(nuclear magnetic resonance,NMR)1 H谱和13C谱、傅里叶变换红外光谱(Fourier transform infrared spectroscopy,FT-IR)、高分辨率质谱(high resolution mass spectroscopy,HRMS)表征了PN1和PN2的结构.采用二浸二轧的工艺,将不同质量分数(2%~27%)的PN1和PN2溶液应用于棉织物整理,研究其阻燃性能.经PN1整理后,棉织物的极限氧指数(LOI)从18%最高可提升至30.1%,在600℃时的成碳率从8%最高可上升至41.8%;经PN2整理后,棉织物的LOI从18%最高可提升至33.1%,在600℃时的成碳率从8%最高可上升至44.3%.

Starting from phosphorus oxychloride, 1,3-propanediol, N-（2-hydroxyethyl）piper-azine, a phosphoramidate compound PN1 was synthesized. And then phosphoramidate derivative PN2 was prepared via nucleophilic reaction between PN1 and diethyl chlorophosphate. Their structures were characterized by^H NMR,13C NMR, FT-IR and HRMS analyses, respectively. Phosphoramidates PN1 and PN2 were applied on cotton fabrics with different content（2%-27%） by the dip-pad-cure process and the flame retardant properties of treated cotton fabrics were then studied. The cotton fabrics treated with PN1 had limited oxygen index（LOI） up to 30. 1% compared with original of 18.0% , the char residue at 600℃ was increased to 41.8% from the original 8%. Meanwhile, cotton fabrics treated with PN2 showed maximum LOI and char residue as 33.1% and 44.3% , respectively.