催化加氢法制备对苯二甲胺的研究

发布时间：2018-05-26 12:16

  本文选题：对苯二腈 + 对苯二甲胺　； 参考：《河北师范大学》2011年硕士论文

【摘要】：对苯二甲胺属于芳香胺类化合物,此类化合物是一种用途广泛的化工原料和精细化工中间体,目前在药物、染料、涂料、尼龙、人造树脂、添加剂、固化剂、纤维整理剂、防锈剂、鳌合剂、润滑剂、表面活性剂等许多方面都有广泛的应用。随着对苯二甲胺用途的逐渐增多,对于它的生产工艺研究具有重要的应用价值。目前,关于对苯二甲胺的生产工艺的研究比较少,本文主要研究对苯二甲腈经催化加氢制备对苯二甲胺的工艺条件。 腈基的还原通常比较困难,腈的催化加氢反应不仅具有理论研究上的重要意义而且在有机合成反应,精细化学品合成中具有重要的应用。催化剂是影响腈基加氢还原反应的主要因素。本文选用了雷尼镍、钯碳和镍铝铁铬合金三种催化剂催化氢化对苯二甲腈制备对苯二甲胺。其中镍铝铁铬合金催化剂为自制,通过XRD、BET、荧光等方法对其进行了表征。 本文分别选用雷尼镍、钯碳、镍铝铁铬合金作为催化加氢反应的催化剂,分别考察每种催化剂催化加氢反应时的反应条件,考察了溶剂、溶剂用量、催化剂用量、反应时间、反应温度、反应压力等条件对于催化加氢反应产物收率的影响,并且还对催化剂的使用寿命及再生进行了研究。通过对比三种催化剂催化加氢反应的最佳反应条件和产物收率,并结合工业化生产的实际,得出钯碳的催化加氢效果最好,得到的最佳工艺条件为:以钯碳为催化剂,甲醇作溶剂,原料/甲醇=1:15(质量比) ,温度为65℃,压力为2MPa,反应时间为1小时,产物对苯二甲胺的收率为81.3%,这个工艺条件比较适合工业化生产,因此本论文对于对苯二甲腈催化加氢制备对苯二甲胺的研究具有非常重要的应用价值。
[Abstract]:P-phenylenediamine is an aromatic amine compound, which is a widely used chemical raw material and fine chemical intermediate, and is currently used in drugs, dyes, paints, nylon, artificial resins, additives, curing agents, fiber finishing agents, Antirust agents, chelating agents, lubricants, surfactants and many other aspects have been widely used. With the increasing use of p-phenylenediamine, it has important application value for the study of its production technology. At present, there are few studies on the production process of p-phenylenediamine. In this paper, the process conditions of catalytic hydrogenation of p-phenylenediamine were studied. The reduction of nitrile group is usually difficult. The catalytic hydrogenation of nitrile not only has important significance in theoretical research but also has important applications in organic synthesis and fine chemical synthesis. Catalyst is the main factor affecting the hydrogenation reduction of nitrile group. In this paper, the catalytic hydrogenation of p-phenylenedionitrile to p-phenylenediamine was carried out on three catalysts: Raney nickel, palladium carbon and Ni-Al-Fe-Cr alloy. The Ni-Al Fe Cr alloy catalyst was prepared and characterized by XRDX BETand fluorescence method. In this paper, Reni nickel, palladium carbon, nickel, aluminum, iron and chromium alloys were selected as catalysts for hydrogenation. The reaction conditions of each catalyst were investigated, and the solvent, catalyst dosage, reaction time and solvent were investigated. The effect of reaction temperature and reaction pressure on the yield of the product was also studied. The service life and regeneration of the catalyst were also studied. By comparing the optimum reaction conditions and product yields of the three catalysts, and combining with the industrial production practice, it is concluded that the catalytic hydrogenation effect of palladium carbon is the best, and the optimum process conditions are as follows: palladium carbon as catalyst, palladium carbon as catalyst. Methanol as solvent, raw material / methanol 1: 15 (mass ratio), temperature 65 鈩，

本文编号：1937203