以PCl5和NH4Cl作原料,在惰性有机溶剂对称四氯乙烷中,以金属氯化物(氯化镁、氯化锌、氯化铁等)为催化剂,吡啶作缚酸剂,合成六氯环三磷腈.探索原料配比、催化剂、反应物粒度等因素对反应时间和产率的影响.实验确定最佳合成工艺条件为在温度130℃,NH4Cl:PCl5=1.3:1,反应时间5.5h,PCl5和NH4Cl的粒度越小,产品收率越高,最高产率可达65%.
Hexachlorocyclotriphosphazene is synthesized from phosphorus pentachloride and ammonium chloride in the presence of catalysts of metal chloride (MgCl2 ,ZnCl2 ,and FeCl3 ) and acid-captor of pyridine by using tetrachloroethane as the inert organic solvent. The influence of the ratio of reactants, catalysts, reactant particle size on the reaction time and productivity are investigated. The experiment shows that the optimal reaction conditions are the molar ratio of phosphorus pentachloride: ammonium chloride being 1.3 : 1, reaction temperature 130 ℃ and reaction time 6-7 h. The smaller the reactant particle size, the larger the productivity is. The highest productivity is 65%.