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采用骤冷法制备了改性骨架镍,将其应用于3,4-二甲基硝基苯的催化加氢制备3,4-二甲基苯胺。考察了各反应参数的影响,结果表明,以甲醇为溶剂,3,4-二甲基硝基苯初始浓度1.0mol/L,催化剂质量为3,4-二甲基硝基苯质量的7%,在60℃和0.5MPa的条件下反应40min,3,4-二甲基硝基苯的转化率和3,4-二甲基苯胺的选择性均达到100%。反应过程中底物浓度与时间趋于线性关系,该反应近似表现为零级反应。反应中未检测到羟胺组分,仅有少量的亚硝基化合物以中间体形式产生,并最终完全转化为目标产物3,4-二甲基苯胺。
The modified nickel skeleton was prepared by quenching method, which was applied to the catalytic hydrogenation of 3,4-dimethylnitrobenzene to prepare 3,4-dimethylaniline. The effects of various reaction parameters were investigated. The results showed that the initial concentration of 3,4-dimethylnitrobenzene was 1.0 mol / L with methanol as solvent, the mass of catalyst was 7% of the mass of 3,4-dimethylnitrobenzene, , Under the conditions of 60 ℃ and 0.5MPa for 40min, the conversion of 3,4-dimethylnitrobenzene and the selectivity of 3,4-dimethylaniline reached 100%. The substrate concentration and reaction time tend to linear relationship, the reaction is approximately the performance of the zero order reaction. No hydroxylamine component was detected in the reaction, only a small amount of nitroso compound was produced as an intermediate, and the final product was completely converted to the target 3,4-dimethylaniline.