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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。
Using 30% T-1 type Raney-Ni catalyst and NaOH (1 mol / L) as solvent, the indoline methyl hydantoin can be obtained under the conditions of 45 ℃ and initial pressure of 3.0 MPa Hain, yield was 85.6%. The experimental results show that the hydrogenation rate of indole-methylene hydantoin is a first-order relationship to the catalyst concentration, and in a certain range, it is directly proportional to the initial hydrogen pressure. The apparent activation energy Ea of hydrogenation of indole methylene hydride was 15.92 kJ / mol calculated from the initial velocity of reaction at different reaction temperatures. The use of magnetic materials can be fixed catalyst recycling. After 20 batches of indole methylene hydride hydrogenation results show that the amount of catalyst used was reduced to 4.5%, the yield of indole methyl heroin can be stabilized at about 80%.