吲哚甲基海因的制备 I.加氢过程研究及催化剂的磁分离

The Preparation of 3-(Indolmethyl)-Hydantoin. I. The Hydrogenation Process of 3-(Indolmethylene)-Hydantoin and Separation of Raney-Ni with Magnetic Material

采用30%T-1型Raney-Ni催化剂,以NaOH(1mol/L)为溶剂,在45℃,初始压力为3.0MPa的条件下,吲哚亚甲基海因加氢可以得到吲哚甲基海因,收率为85.6%。实验结果表明,吲哚亚甲基海因加氢速度对催化剂浓度为一级关系;在一定范围内,与初始氢压成正比关系。由不同反应温度下的反应初速度计算吲哚亚甲基海因加氢反应的表观活化能Ea为15.92kJ/mol。采用磁性材料固定方法可实现催化剂的回收利用。经20批次吲哚亚甲基海因加氢反应结果可知,催化剂的使用量降低为4.5%,吲哚甲基海因的收率可稳定在80%左右。

3-(indolmethyl)-hydantoin was prepared from 3-(indolmethylene)-hydantoin at 45℃ and (3.0MPa) with T-1 Raney-Ni as catalyst and 1mol/L NaOH as solvent. It was found that the reaction rate of hydrogenation was direct proportional to catalyst concentration and hydrogen pressure respectively. The activation energy evaluated form initial reaction rates was 15.92kJ/mol. Activity carbon was used as promoter. But triethylamine was inhibitor. The magnetic material was placed in reactor to keep the cutalyst from lossing. During 20-batch hydrogenations, the average yield of 3-(indolmethyl)-hydantoin was 80%, and the amount of Raney-Ni catalysts was reduced to 4.5%.