摘要
提出了五氯化磷气化法合成六氯环三磷腈新工艺。以氮气做载气,五氯化磷气态进料,与氯化铵在惰性有机溶剂中催化反应合成了六氯环三磷腈。在N2流量60mL/min,五氯化磷升华温度170℃,溶剂用量110mL,反应温度131±1℃,ZnCl20.1g,PCl523.1g,NH4Cl5.4g,反应时间185min条件下得粗磷腈12.0g,收率92.31%。经精制,得到六氯环三磷腈7.9g,总产率达40%(以五氯化磷计)。产品六氯环三磷腈熔点112.4～114℃。元素分析结果N11.98%,P26.50%,Cl60.64%;用IR谱、质谱进行了表征。
A new technology for synthesis of hexachlorocyclotriphosphazene is proposed. Hexachlorocyclotriphosphazene is prepared by reacting gaseous phosphorus pentachloride carried by nitrogen with ammonium chloride in an inert organic solvent in presence of different metallic compounds. The optimum conditions are as follows： sublimation temperature of phosphorus pentachloride is 170℃ , flow rate of N2 is 60mL/min, the amount of ZnCl2 is 0.1g, reaction temperature is 131 ±1℃ , volume of chlorobenzene is 110mL, and the amount of PCl5 and NH4Cl is 23. 1g and 5.4g respectively. Under above-mentioned conditions, 12.0g crude product is gained with yield of 92.31%. And 7.9g hexachlorocyclotriphosphazene is obtained with total yield of 40% （calculated based on PCl5 ）. The final hexachlorocyclotriphosphazene is characterized by IR spectra, MS spectra, meldometer and elementary analysis.
出处
《精细与专用化学品》
CAS
2006年第12期10-11,20,共3页
Fine and Specialty Chemicals
基金
吉林省教育厅科技基金资助项目(项目编号200245)
关键词
六氯环三磷腈
五氯化磷
磷腈
氯化铵
hexachlorocyclotriphosphazene
phosphoric chloride
phosphazene
ammonium chloride
