菲咯啉镍配合物的合成工艺研究

Study on the synthesis process of phenanthroline Nickel complexes

研究了以菲咯啉为原料,经氧化,芳醛缩合,金属离子络合等反应合成新型金属有机三阶有机非线性光学化合物[2-(1H-咪唑[4,5-f][1,10]菲咯啉-2-基-κN7,κN8)苯酚]双(1,10-菲咯啉-κN1,κN10)镍(2+)的工艺过程.对氧化与芳醛缩合两步反应进行了工艺优化,氧化反应的较佳工艺条件:菲咯啉和溴化钠之间的摩尔比为1∶4,反应温度为110℃,反应时间4 h,氧化反应收率由40%提高到92%.缩合反应的较佳工艺条件:一锅煮的加料方式,反应温度80℃,酮醛比1∶1.2,反应时间2 h,酮铵比1∶20,缩合反应收率由70%提高到93.1%.

The novel organometallic compounds [2-（1H-imidazole phenanthroline-2-yl-κN7,κN8）phenol] bis（1,10-phenanthroline-κN1,κN10）Nickel（2＋） with the third-order nonlinear optical property were prepared using Phenanthroline as material through the successive reactions of oxidation,condensation of aryl-aldehyde and complexation of metal ions.The process parameters of oxidation and condensation reaction were optimized.The optimum conditions for oxidation reaction were obtained as follows： n（phenanthroline）∶n（sodium bromide） = 1 ： 4, reaction temperature 110℃, and refluxing reaction time for 4 h. For the condensation reaction, the optical conditiors were one-pot synthesis method, reaction temperature 80℃, n （-1-, 10- Phenanthroline-5,6-dione） ： n（O-Hydroxybenzaldehyde）=1 ： 1.2, refluxing reaction 2 h and n （1,10-Phenanthroline-5,6-dione） ： n and condensation reactions increased （ammonium acetate）= 1：20. The yields of the oxidation from 40% to 92% and from 70% to 93.1%, respectively.