以含季戊四醇骨架的螺环磷酸酯二酰氯（PDD）和双环笼状磷酸酯（PEPA）为反应物，合成既有螺环又有双环笼状的磷酸酯阻燃剂PDD-PEPA，对该阻燃剂的合成条件（三乙胺催化剂用量、反应时间）进行优化，通过质谱、红外光谱和核磁等方法对PDD-PEPA的结构进行表征，采用热重分析对PDD-PEPA在氮气氛下的热稳定性和成炭性进行了分析。结果表明：以乙腈为溶剂、三乙胺与理论释放氯化氢的摩尔比为1.2:1、回流温度下反应10 h时可得到较高产率的PDD-PEPA；该条件下制得的阻燃剂理论磷含量为21.2%，起始分解温度为351 ℃，650 ℃时的残炭率为63.6%。

A spiro and caged bicyclic phosphate flame retardant named as PDD-PEPA was synthesized with pentaerythritol diphosphate dichloride (PDD) and caged bicyclic phosphate 1-oxo-1-phospha-2, 6, 7–trioxabicyclo [2.2.2]-4-hydroxymethyl octane (PEPA) as reactants, and the synthesis conditions of the flame retardant, namely the dosage of triethylamine as a catalyst and the reaction time, wereare optimized. Then, the structure of PDD-PEPA was characterized by means of MS, IR and NMR, and the thermal stability and charring capacity of PDD-PEPA were investigated in N2 atmosphere through thermalgravimetric analysis. The results show that (1) when PDD- and PEPA reacts with a mole ratio of triethylamine to theoretical hydrogen chloride of 1:2 in the acetonitrile solvent at a reflux temperature for 10 h, the yield of PDD-PEPA is higher, and (2) under such conditions, the theoretical phosphorus content of the flame retardant is 21.2%, the initial decomposition temperature is 351℃, and the carbon yield is 63.6% at 650℃.