苄胺的合成研究：苯甲醛氨化加氢法与苄氯氨解法的比较

【作者】 于强；

【导师】 李亚明；

【作者基本信息】 大连理工大学 ， 应用化学， 2001， 硕士

【摘要】 本文对苄胺的两种合成方法进行了研究。采用苯甲醛为原料氨化加氢法合成了苄胺。考察了原料配比、催化剂种类及用量、反应温度、反应压力等因素对苄胺收率的影响。确定了最佳的实验条件：Raney—Ni催化剂（A）质量为苯甲醛质量的5％；液氨与苯甲醛物质的量之比为：15：1；反应釜内压力：7.5MPa；反应温度为60℃，利用GC/MS技术对反应产物进行了分析鉴定。由苯甲醛计算苄胺产率为84.1％，纯度为98.64％。并对反应机理进行了讨论。虽然苯甲醛氨化加氢法合成苄胺反应步骤少，环境友好，产率高，可达84％，远远高于传统的苄氯氨解法（43.3％），但需在高压（7.5MPa）条件下反应，条件苛刻，设备投资大。 以苄氯为原料，苯甲醛做副反应抑制剂在温和条件下合成了苄胺。传统的苄氯氨解法，副反应多，收率低，只有40％左右，本文通过对反应机理的研究，提出加入苯甲醛作为副反应抑制剂，有效的抑制了副产物二苄胺、三苄胺的生成，苯甲醛可以重复使用，收率提高至84％。考察了氨解温度、氨水用量、盐酸浓度、酸解温度等因素对苄胺产率的影响，确定了最优的实验条件，氨水用量为苄氯的10倍，苯甲醛用量为苄氯的2倍，反应温度50℃，酸解盐酸的浓度为10％，酸解温度40℃。由苄氯计算苄胺产率为84.1％，纯度99.87％。以苄氯为原料，苯甲醛做副反应抑制剂合成苄胺，在温和条件下同样可达到高收率（84.1％），是一种具有工业化前景的方法。更多还原

【Abstract】 The two synthetic methods of benzylamine were studied. Benzylamine was prepared by hydrogenation of benzaldehyde in the presence of liquid ammonia. Some factors, such as the ratio of raw materials, different catalysts and different quantities, temperature and hydrogen pressure were studied. Thereby , The optimum experiment condition for preparing benzylamine was obtained. The optimum experiment condition was that Raney nickel was in the amount of 5% on the benzaldehyde, the ration of liquid ammonia to benzaldhyde is 15:1, hydrogen pressure is 7.5MPa, temperature is 60 癈. Products were analyzed by GC/MS. The yield is 84.1%, and the product purity is 98.88%. The mechanism was discussed. Benzylamine was prepared in simple steps, friendly environment and good yield by this method. The yield is 84% and much higher than the yield(43.3%) by the traditional method of benzylchloride ammoniating with ammonia. However, the higher pressure was required by this method. So the investment of equipment will be much more because of the rigor reactive condition.Benzylamine was prepared by reacting benzylchloride and aqueous ammonia solution in the presence of benzaldhyde used as a side reaction inhibiter. The effects of the ammoniated reaction temperature, the quantity of aqueous ammonia solution, the concentration of hydrochloric acid, and the temperature of acid hydrolyze reaction were investigated. The optimum experiment condition for preparing benzylamine was obtained. The optimum experiment condition was that the ratio of ammonia to benzylchloride is 15:1, the ratio of benzaldhyde to benzylchloride is 2:1, the ammoniated reaction temperature is 50癈, the concentration of hydrochloric acid is 10%, and the temperature of acid hydrolyze reaction is 40癈. The yield is 84.1%, and the product purity is 99.87%. Benzylamine could be obtained in mild condition by this method and the yield up to 84.1% was obtained. This method is a good method for industrial.更多还原