以三氯氧磷和季戊四醇磷酸酯为原料合成了一种膨胀型无卤阻燃的中间体二((1-氧化-2,6,7-三氧-1-磷酸甲酯[2,2,2]辛烷-4-甲基)磷酸氯化物(PASPO),然后将PASPO与双酚A反应得到添加型阻燃剂四((1-氧化-2,6,7-三氧-1-磷酸双环[2,2,2]辛烷-4-甲基)(丙烷-2,2-二(4,1-苯基)二(磷酸盐)(PPSPBA),在聚对苯二甲酸丁酯(PBT)中添加PPSPBA制备了阻燃PBT复合材料。采用傅里叶变换红外光谱仪、核磁共振氢谱仪对磷系阻燃剂PPSPBA进行表征;使用氧指数测定仪和水平/垂直燃烧测定仪对复合材料阻燃性能进行测试;采用扫描电子显微镜对复合材料燃烧后的残炭进行分析;使用拉伸试验机、数字冲击试验机对复合材料力学性能进行测试。结果表明:在PBT中加入80份PPSPBA阻燃剂,在不影响力学性能的前提下,使PBT的极限氧指数达到29%,阻燃效果提高了31.82%。
A new expansion type halogen-free flame retardant intermediate,bis(1-oxido-2,6,7-trioxa-1-phosphabicyclo[2,2,2]octan-4-ly)methyl)phosphorochloridate(PASPO) was synthesized by using phosphorous oxychloride and pentaerythritol phosphate ester as raw materials.Then PASPO was reacted with bisphenol A to produce an additive flame retardant,tetrakis(1-oxido-2,6,7-trioxa-1-phosphabicvclo[2,2,2]loctan-4-ymethv)(propane-2,2divlbis(4,1-phenvlene)) bis(phosphate)(PPSPBA).Next,adding PPSPBA to polybutyl terephthalate (PBT) to prepare flame retardant PBT composites.The structure of the PPSPBA was characterized by Fourier transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance hydrogen spectrum (1H-NMR).The flame retardancy of the PPSPBA composites was tested by oxygen index tester and horizontal/vertical combustion tester.The carbon residue of the composites after combustion was analyzed by scanning electron microscope (SEM).The mechanical properties of the composites were tested by tensile testing machine and digital impact testing machine.The results showed that when 80 phr PPSPBA was added into PBT,the limiting oxygen index of PBT reached 29% without affecting the mechanical properties,and the flame retardant effect was improved by 31.82%.
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基金资助
“2021级大学生创新创业训练计划项目”资助项目(S202110149003);辽宁省教育厅青年育苗项目(LQ2020010);辽宁省博士科研启动基金指导计划(2021-BS-184)
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