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以苯基膦酰二氯及三羟甲基氧化膦为原料,合成了一种高含磷量同环双膦阻燃剂——羟甲基膦酰杂环状苯基膦酸酯(即1,4-二氧-1-苯基-4-羟甲基-2,6-二氧杂-1,4-二磷杂环己烷)。通过考察溶剂、原料物质量比、反应温度及反应时间等对该产物产率的影响,确定了最佳合成条件,同时利用傅里叶变换红外光谱(FTIR)、核磁共振氢谱(1H-NMR)、热重(TG)分析及极限氧指数(LOI)测试等手段表征了产物的结构及性能。结果表明:当采用乙二醇二乙醚作为溶剂,且苯基膦酰二氯和三羟甲基氧化膦的物质量比为1:1、反应温度为120℃、反应时间为6 h时,产物的产率达到最大值(94.5%)。产物具有较好的热稳定性,当其应用于191不饱和聚酯或聚对苯二甲酸丁二醇酯(PBT)时均表现出了良好的阻燃成炭效果;另外,当其与氰尿酸三聚氰胺盐(MCA)复配用于PBT阻燃时,表现出明显的协同阻燃效应。
Using phenylphosphonic dichloride and trimethylolphosphine oxide as raw materials, a high phosphorus content homocyclic bisphosphine flame retardant, hydroxymethylphosphonoheterocyclic phenylphosphonate (ie, 1 , 4-dioxo-1-phenyl-4-hydroxymethyl-2,6-dioxa-1,4-diphosphetane). The optimum synthesis conditions were determined by investigating the effects of solvent, mass ratio of raw materials, reaction temperature and reaction time on the yield of the product. Fourier transform infrared spectroscopy (FTIR) and 1H-NMR ), Thermogravimetry (TG) analysis and limit oxygen index (LOI) test were used to characterize the structure and properties of the product. The results showed that when ethylene glycol diethyl ether was used as the solvent and the mass ratio of phenylphosphonic dichloride to trimethylolphosphine oxide was 1: 1, the reaction temperature was 120 ℃ and the reaction time was 6 h, the product Reached the highest yield (94.5%). The product possesses good thermal stability and exhibits good flame retardant charring effect when applied to 191 unsaturated polyester or polybutylene terephthalate (PBT). In addition, The combination of melamine urate (MCA) with PBT showed significant synergistic flame retardancy.