催化加氢制备3,4-亚甲二氧基苯胺

3,4 亚甲二氧基硝基苯在95%乙醇溶剂中用雷尼镍催化加氢制备了3,4 亚甲二氧基苯胺。对催化剂用量和活性稳定性进行了研究,讨论了溶剂用量、温度、压力等因素对加氢反应的影响。结果表明最佳工艺参数为:雷尼镍∶乙醇∶3,4 亚甲二氧基硝基苯=0.15∶6∶1(质量比),反应温度40℃,氢压0.45～0.50MPa,搅拌速度450r/min,反应至不再吸氢为止,产品收率在97%以上,纯度为98%。

Preparation of 3,4-methylene-dioxy aniline by catalytic hydrogenation

3,4-methylene-dioxy aniline was prepared by catalytic hydrogenation with Raney nickel from 3,4-methylene-dioxy nitrobenzene in solvent of 95% ethanol. The active stability and amount of the catalyst were studied and the influential factors ,such as solvent, temperature and pressure were investigated,and then the optimal process parameters were given∶Raney∶ethanol∶3,4-methylene-dioxy nitrobenzene is 0.15∶6∶1(mass ratio);the reaction temperature is 40℃;the hydrogenation pressure is 0.45～0.50 MPa;the stir velocity is 450 r/min.In this way the yield of 3,4-methylene-dioxy aniline is up to 97%, purity is 98%.