2,5-二氯对苯二胺的合成工艺研发 毕业论文.doc

毕业设计报告(论文) 2,5-二氯对苯二胺的合成工艺研发 姓　　名 所 属 系 化工与制药工程系 专 业 化学工程与工艺 学 号 指导老师 顾问老师 起讫日期 2011.01--2011.05 设计地点 盐城市庙港化学品有限公司  毕业设计（论文）诚信承诺 本人承诺所呈交的毕业设计报告（论文）及取得的成果是在导师指导下完成，引用他人成果的部分均已列出参考文献。如论文涉及任何知识产权纠纷，本人将承担一切责任。 学生签名： 日 期： 2,5-二氯对苯二胺的合成工艺研发 摘 要 2,5-二氯对苯二胺是一种重要的化学原料、药品合成中间体在染料工业，合成偶氮颜料也可作为聚氨酯合成的原料。2,5-二氯对苯二胺的制备方法以－二氯苯胺为原料，包括苯甲酰化，混酸硝化，性中水解，铁粉还原四步反应。对其中酰化进行工艺改进，即(反应温度，反应时间，质量收率)分别为：酰化反应：25℃，0.5h，98.09%；硝化反应：50℃，7-8h，93.90%；水解反应：95℃，2-3h，81.31%；还原反应：95℃，7h，80.14%。最后，四步反应总收率为60.25%。产物熔点与文献报道中的一致，并通过H-NMR和IR确认了标题化合物的结构。 关键词：2,5-二氯对苯二胺；酰化反应；硝化反应；水解反应；还原反应 Synthesis process research of 2,5-dichloro-p-phenylenediamine Abstract 2,5-dichloro-p-phenylenediamine is an important chemical material, pharmaceutical synthesis intermediate. In pesticide, medicine industry, it has a very wide range of applications. In dyestuff industry, it can be used for azo pigments, also can be used as the raw material polyurethane synthesis, and also can be applied in hair colorings,rubber made,imaging agents production. The preparation method is based on 2,5-dichloroaniline as raw material, the route includes acylation reaction, nitratlon reaction, alkali hydrolysis reaction, reduction reaction. In this article, the process improvement of acylation reaction and nitratlon reaction is to use halogenated hydrocarbon solvents, so it’s productivity-boosting. The mild reaction conditions, high purity and low cost preparation method is suitable for industrial production. In acylation reaction, we use Ac2O for reaction, hence, the operation is convenient and this way is efficient. The hydrolysis reaction in alkaline medium hydrolysis, is to solve the problem of waste acid treatment. The optimal reaction conditions (temperature, time，weight yield) were asfollows: cylation reaction: 25℃, 0.5h, 98.09%; nitratlon reaction: 50℃，7-8h，93.90%ydrolysis