聚合型含硫有机膦阻燃剂的制备及其应用

在无溶剂条件下,以苯基硫代膦酰二氯、10-(2,5-二羟基苯基)-9-氧杂-10-磷酰杂菲(DOPO-HQ)为原料,合成了一种聚合型含硫有机膦阻燃剂聚苯基硫代膦酸(10-(2,5-二羟基苯基)-9-氧杂-10-磷酰杂菲)酯(PDPTP)。考察了反应时间和反应温度对收率的影响,确定了适宜的反应条件为:n(苯基硫代膦酰二氯)∶n(DOPO-HQ)=1∶1,160℃下恒温1 h,240℃下反应4 h。在此条件下,PDPTP收率为99.0%。采用FTIR、1H NMR、元素分析等方法对产物结构进行了表征,并采用TG-DTA方法对其热稳定性进行了分析。表征结果显示,所合成的化合物为目标产物PDPTP,热分解温度为270℃。利用氧指数测定仪测试PDPTP的阻燃性能时发现,PDPTP对聚对苯二甲酸丁二醇酯具有较好的阻燃性。

Preparation and Application of a Polymeric Sulfur-Containing Organophosphorus Flame Retardant

Poly-phenyl-phosphonothioic acid(10-(2,5-dihydroxyphenyl)-9-xa-10-phosphoryl hybrid-philippines) ester(PDPTP) as a polymeric sulfur-containing organophosphorus flame retardant was synthesized from phenylthiophosphonic dichloride and 10-(2,5-dihydroxyphenyl)-9-xa-10phosphoryl hybrid-philippines(DOPO-HQ) by a solvent-free method.The effect of reaction time and reaction temperature on the yield of PDPTP was studied.Under the optimal reaction conditions of n(phenylthiophosphonic dichloride)∶n(DOPO-HQ) 1∶1,reaction firstly at 160 ℃ for 1 h and then at 240 ℃ for 4 h,the yield of PDPTP can reach 99.0%.The chemical structure of the product was characterized by means of FTIR,1H NMR and elementary analysis.The results show that the product is PDPTP.Its thermal degradation behavior and flame retardancy were investigated by means of TGDTA and oxygen index analyzer.And the results indicate that its decomposition temperature is 270 ℃ and it has excellent flame retardancy for polybutylene terephthalate.