几种新型高含磷含氮聚磷酰胺阻燃剂的合成与表征

Synthesis and characterization of some novel flame retardants polyphosphamides with enhanced phosphorus-nitrogen content

以螺环季戊四醇双磷酸酯二酰氯(SPDPC)和苯基二氯磷酸酯(PDCP)为酰氯单体,分别与哌嗪及乙二胺通过溶液缩聚合成了4种聚磷酰胺阻燃剂——聚哌嗪季戊四醇双磷酸酯(PPS)、聚乙二胺季戊四醇双磷酸酯(PES)、聚哌嗪苯基磷酸酯(PPP)及聚乙二胺苯基磷酸酯(PEP)。以IR、1H NMR,31 P NMR、元素分析、TGA表征其结构及热性能,以乌氏粘度计测定PPS与PES特性黏度,结果发现反应18h聚合度最大,分别为0.19和0.21dL/g。以激光解吸电离-飞行时间质谱仪(MALDI-TOF MS)表征PPP与PEP分子量及组成。结果表明聚合度均在7～8之间。

Four novel polymers with enhanced phosphorus-nitrogen content-poly（pipera-zine spirocyclic pentaerythritol bisphosphonate）（PPS）,poly（ethylene-diamine spirocyclic pentaerythritol bisphosphonate）（PES）,poly（piperazine-phenylphosphonate）（PPP）,poly（ethylenediaminephenylphosphonate）（PEP） were synthesized,which were prepared by solution polycondensation from dichloropentate（SPDPC and PDCP） with diamine（piperazine and ethylenediamine）.The structure and performance of obtained polymers were characterized by IR,1H NMR,31P NMR,elemental analysis,Ubbelodhe viscometer and TGA,and influence of time of reaction on the inherent viscosity of polymers（PPS and PES） was studied.The results showed that the maximum degree of polymerization are respectively 0.19 and 0.21dL/g in the reaction of 18h.Characterize structure and mole mass polymers（PPP and PEP） by MALDI-TOF MS,and degree of polymerization is 7-8.