第 38 卷第 5 期Vol. 38 No. 5
2008 年 10 月Oct 2008

所属栏目:染料、颜料及涂料

4-氨基-3-硝基苯酚的合成工艺改进
郁惠珍,严 阳,蔡 勇,顾 燕 (健雄职业技术学院 化学工程系,江苏 太仓 215411)
摘 要:以对氨基苯酚为原料,经酰化、硝化、水解制得4-氨基-3-硝基苯酚,采用控制醋酐、硝酸的用量以及水解时加入乙醇做溶剂的方法,改进了工艺条件:n(对氨基苯酚) ∶ n(醋酐) ∶ n(发烟硝酸) =1 ∶ 3.3 ∶ 1.2,酰化时间2 h,硝化时间1.5 h;水解反应中物料比为n(3-硝基-4-乙酰胺基苯酚乙酯) ∶ n(氢氧化钠) ∶ n(乙醇)=1 ∶ 4 ∶ 15,水解时间1 h。与文献工艺条件相比,硝化反应中硝酸的用量减少为原来的1/5;水解反应时间缩短到原来的1/4,总收率从58.2%提高到69.4%。
关键词:4-氨基-3-硝基苯酚;酰化;硝化;水解;优化
中图分类号:TQ243.1  文献标识码:A  文章编号:1009-9212(2008)05- 0040-03
The Optimization of Synthesis Process of 4-Amino-3-nitrophenol
YU Hui-zhen,YAN Yang,CAI Yong,GU Yan (Chemical Engneering Department,Chien-Shiung Institute of Technology,Taicang 215411,China)
Abstract:4-Amino-3-nitrophenol can be synthesized from p-aminophenol as raw material through acetylation,nitration and hydrolysis. The synthesis method was optimized by controlling of the dosage of acetic anhydride and nitric acid,and using ethanol as solvent. The optimum conditions include as following:a dosage ratio of n(p-aminophenol) ∶ n(acetic anhydride) ∶ n(fuming nitric acid) =1 ∶ 3.3 ∶ 1.2,acetylation for 2 h and nitration for 1.5 h;n(4-acetamido-3-nitrobenzoicphenol acetate) ∶ n(sodium hydroxide) ∶ n(ethanol)=1 ∶ 4 ∶ 15 in hydrolysis,and hydrolysis for 1h. Comparing with the conditions that mentioned in the literature[2],the consumption of nitric acid for nitration was reduced to 1/5,the hydrolysis time was reduced to 1/4,and the total yield was increased from 58.2% to 69.4%.
Key words:4-amino-3-nitrophenol;acetylation;nitration;hydrolysis;optimization
作者简介:郁惠珍(1979-),女,江苏苏州人,硕士,主要从事有机化学的研究。(E-mail:yhz0822@yahoo.com.cn)
收稿日期:2008-08-11