膨胀型阻燃剂聚硫代苯基膦酰哌嗪的合成

以硫代苯基磷酰二氯和无水哌嗪为原料,采用无溶剂法合成了新型无卤膨胀阻燃剂聚硫代苯基膦酰哌嗪.最佳工艺条件为:n(硫代苯基磷酰二氯):n(无水哌嗪)=1:1,以吡啶做缚酸剂,在120℃反应20 h,产率达89%.并以红外光谱、核磁共振谱和差热分析对所得化合物进行了表征.

SYNTHESIS OF HALOGEN-FREE INTUMESCENT FLAME RETARDANT POLY-PHENYLPHOSPHONOTHIOIC-PIPERAZINE

A new halogen-free intumescent flame retardant poly-thio-phenyl-phosphine acyl piperazine was synthesized with phenylphosphonothioic dichloride and anhydrous piperazine as raw materials and pyridine as acid-trapping agent in the absence of solvent.Effects of reaction temperature,reaction time and acid-trapping agents on the yield were investigated.The optimum conditions were found as follows:n(phenylphosphonothioic dichloride):n(anhydrous piperazine) = 1:1,reaction time 20 h and reaction temperature 120℃,pyridine as acid-trapping agent with the yield of 89%.FT-IR, ~1H NMR and differential thermal analysis were used to characterize the obtained compounds.