【作者】 贾志刚；

【导师】 李方实；

【作者基本信息】 南京工业大学 ， 应用化学， 2004， 硕士

【摘要】 芳胺产品广泛应用于化工、医药、染料、农药等领域。绝大多数的芳胺都来自相应的硝基化合物。将硝基芳烃还原为芳胺是一类重要的还原反应，在精细化工中间体的生产中占有极重要的地位。将硝基芳烃还原为芳胺的方法较多，有化学还原法如铁粉还原，电解还原法和催化氢化法等。当前应用较广的化学还原法由于在生产过程中污染环境而逐渐被其他方法所取代。电解还原法由于较高的生产成本还无法在生产实践中发挥作用。催化氢化法，尤其是液相催化加氢法以其独特的还原过程，在提高产品品质的同时，大大缓解了对环境的污染。在环境问题日益受到人们关注的今天，在化工生产中推广和利用这一方法，无疑会产生显著的经济和社会效益。 随着生产实践的不断发展，人们对催化加氢的研究亦日益深入。本文综述了近年来液相催化加氢的研究成果。着重研究了液相催化加氢技术在医药特别是麻醉药普鲁卡因和氨苯丁酯合成中的应用。在催化加氢制备普鲁卡因的过程中，自制了Raney镍催化剂，探讨了Pd／C催化剂和Raney镍、催化加氢效果。从降低生产成本的角度，优选了一定目数的镍铝合金制备的Raney镍做催化剂，将催化加氢法引入普鲁卡因生产工艺。对反应中间产物硝基卡因催化加氢，探讨了催化剂用量、温度、压力、转速、反应时间等因素对产率的影响，确定了生产该产品的最佳工艺条件。催化加氢法制备普鲁卡因产率达85％，含量达98.02％，产品后处理简单经济，克服铁粉还原工艺中三废严重，劳动强度大，产率较低和产品品质较差的缺陷。 本文还考察了催化剂、温度、压力、转速、反应时间等因素对催化加氢制备氨苯丁酯的影响，确立了催化加氢法生产氨苯丁酯的最佳工艺条件：温度90℃，氢压2.5MPa，催化剂用量为原料量的15％。氨苯丁酯加氢转化率达99％，产率达75.4％，含量达95.6％。并对催化加氢制备对氨基苯甲酸作了初步探讨。更多还原

【Abstract】 Aromatic amines are widely used in dyestuffs, pharmaceutical products, agricultural chemicals, surfactants. And most of the aromatic amines come from corresponding nitro compounds. Reducing the nitroarene to aromatic amines is an important reaction in the production of fine chemical. There are many methods of reducing nitro to amine, such as the Bechamp reduction employed iron, electrolysis reduction, catalytic hydrogenation and so on. Bechamp reduction brought out serious pollution to environment, and it should be replaced by other means someday. Electrolysis reduction cannot be brought into practice because of higher cost. Catalytic hydrogenation, especially liquid catalytic hydrogenation, relieves pollution for environment greatly and promotes the production quality. With the increasing attention to environment problems, popularizing the catalytic hydrogenation technology in the industry production must bring prominent economic and social benefits.With the development of science, the study for catalytic hydrogenation has been pushed continuously. This paper summarizes the catalytic hydrogenation development in recent years.This dissertation studied the appliance of liquid catalytic hydrogenation technology to the production of procaine and butyl-4-aminobenzoate. For preparing procaine by liquid catalytic hydrogenation technology, Pd/C catalyst and the Raney-Ni catalysts which are prepared by different sizes Ni-Al alloys with the special methods, were studied. From the view of degrading the cost in the industry production, a special type of Raney Ni catalyst was chosen for the preparation of procaine. By catalytic hydrogenation instead of iron reduction, 4-nitrobenzoic acid -2-(diethylamino)ethyl ester is reduced to 4-aminebenzoic acid-2-(diethylamino)ethyl ester. The influence of the temperature, pressure, catalyst dosage and reaction time to yield were discussed, and the optimized technology was as follows: temperature 130, hydrogen pressure 3.0MPa, time 7 h. The conversion rate was 95%. The yieldof procaine was 83.5%, The purity is up to 98.02%.The catalytic hydrogenation applied to the preparation of procaine simplified the purification step and overcame the drawbacks such as serious pollution, inferior product and heavy work.In this dissertation the preparation of butyl-4-aminobenzoate from butyl-4-nitrobenzoate with catalytic hydrogenation was also studied. The influence of the temperature, pressure, catalyst dosage and reaction time to yield were discussed.The optimized technology was as follows: temperature 90癈, hydrogen pressure 2.5MPa. The conversion rate was 99%. The yield of butyl-4-aminobenzoate was 75.4%, The purity is up to 95.6%.And in the latter of this paper, the production of p-amine benzoic acid from p-nitro benzoic acid was also studied.更多还原