五氯化磷气化法合成六氯环三磷腈的工艺研究

以N_2为载气,PCl_5气态进料,与NH_4Cl在惰性有机溶剂中催化反应合成了六氯环三磷腈(CTPP)。较佳工艺条件为:PCl_5用量23．1 g、n(PCl_5):n(NH_4Cl)=1:1,ZnCl_2用量0．1 g,N_2流量60 mL/min,PCl_5升华温度为170℃,溶剂用量110 mL,反应温度(131±1)℃,反应时间约190 min,PCl_5转化率达100%, CTPP总产率达40%。CTPP熔点为112．4～114℃,并对产物进行了元素分析和IR表征。

TECHNOLOGY FOR SYNTHESIS OF CHLOROCYCLOPHOSPHAZENE WITH SUBLIMED PHOSPHORUS PENTACHLORIDE

Hexachlorocyclotriphosphazene was prepared by reacting sublimed phosphorus pentachlo- ride with ammonium chloride in an inert organic solvent in the presence of metal compounds and N_2. The optimal conditions were found as follows:23.1 g PCl_5,the ratio of PCl_5 to NH_4Cl 1:1,sublima- tion temperature of phosphorus pentachloride 170℃,flowrate of N_2 60 mL/min,reaction temperature (131±1)℃,110 mL chlorobenzene and reaction time 190 min.Up to 100% conversion of phosphor- us pentachloride and 40% yield of hexachlorocyclotriphosphazene were achieved.The melting point of hexachlorocyclotriphosphazene was 112.4-114℃.The product was characterized by IR spectra and elemental analysis.