六苯胺基环三磷腈合成工艺的改进

Improvement of Synthesis Process for Hexaanilinocyclotriphosphazene

对以六氯环三磷腈和苯胺为原料,三乙胺为缚酸剂合成六苯胺基环三磷腈进行了研究。结果表明,溶剂类型和用量是影响六苯胺基环三磷腈合成的关键因素。氯苯是较理想的溶剂,且其用量愈小,产品产率愈高。较理想的合成条件是:n(六氯环三磷腈)∶n(苯胺)∶n(三乙胺)=1∶7.2∶6.6,m(六氯环三磷腈)∶m(氯苯)=1∶3.5,反应温度90℃,反应时间15h。在以上条件下,产品的产率为80.42%,熔点为268~270℃,含量接近95%(^(31)P NMR法)。该方法具有工艺简单、条件温和、产品产率及质量高等优点。

Hexaanilinocyclotriphosphazene was synthesized using hexachlorocyclotriphosphazene and aniline as starting materials,and triethylamine as an acid-binding agent.The results showed that the type and amount of solvents were key factors for the synthesis.Chlorobenzene was an ideal solvent and the yield was increased with the reducing the amount of chlorobenzene.The optimum reaction conditions were as follows：n（hexachlorocyclotriphosphazene）∶n（aniline）∶n（the acid）∶n（triethylamine）=1∶7.2∶6.6,m（hexachlorocyclotriphosphazene）∶m（chlorobenzene）=1∶3.5,reaction temperature being 90℃,and reaction time being 15 h.Under the above conditions,the yield of the product could be up to 80.42%,the melting point was 268—270℃,the purity was close to 95%.The method has some advantages such as simple process,mild reaction conditions,high yield,good quality,and so on.