采用复式催化剂/缚酸剂体系,合成了六氯环三磷腈。研究了反应溶剂、投料比例、催化剂、反应时间和原料粒径对六氯环三磷腈产率的影响,优化了合成条件和纯化方法,并确定了最佳反应条件。采用熔点测试、元素分析、红外光谱、X射线衍射、核磁共振等测试手段对产物进行了表征。结果表明,所得产物为目标化合物。产率可稳定在75%～80%之间,产物纯度达到98%。在聚合反应前,需要用重结晶结合升华的方法对六氯环三磷腈单体进行精制,以使聚合反应顺利进行。
Hexachlorocyclotriphosphazene was synthesized by adopting mixed catalyst/acid binding agent synthesis system.The influences of reaction solvent,ratio of reactants,catalysts,reaction time,reactant particle size on the yield were investigated.Synthetic conditions and purification method were optimized and the best reaction condition was determined.The product was characterized by melting point determination,elemental ana-lysis,infrared spectrometer（IR）,XRD and nuclear magnetic resonance（NMR）.The result showed that the pro-duct obtained is just the target compound.It turned out that the yield of the product was maintained at a level between 75% and 80%,and the purity of the product was increased to 98%.Before polymerization reaction,HCCP needs to be purified by recrystallization and sublimation for the polymerization reaction to be done smoothly.
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