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

所屬欄目:染料、顏料及涂料

4-氨基-3-硝基苯酚的合成工藝改進(jìn)
郁惠珍,嚴 陽(yáng),蔡 勇,顧 燕 (健雄職業(yè)技術(shù)學(xué)院 化學(xué)工程系,江蘇 太倉 215411)
摘 要:以對氨基苯酚為原料,經(jīng);、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時(shí)加入乙醇做溶劑的方法,改進(jìn)了工藝條件:n(對氨基苯酚) ∶ n(醋酐) ∶ n(發(fā)煙硝酸) =1 ∶ 3.3 ∶ 1.2,;瘯r(shí)間2 h,硝化時(shí)間1.5 h;水解反應中物料比為n(3-硝基-4-乙酰胺基苯酚乙酯) ∶ n(氫氧化鈉) ∶ n(乙醇)=1 ∶ 4 ∶ 15,水解時(shí)間1 h。與文獻工藝條件相比,硝化反應中硝酸的用量減少為原來(lái)的1/5;水解反應時(shí)間縮短到原來(lái)的1/4,總收率從58.2%提高到69.4%。
關(guān)鍵詞:4-氨基-3-硝基苯酚;;;硝化;水解;優(yōu)化
中圖分類(lèi)號:TQ243.1  文獻標識碼:A  文章編號: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
作者簡(jiǎn)介:郁惠珍(1979-),女,江蘇蘇州人,碩士,主要從事有機化學(xué)的研究。(E-mail:yhz0822@yahoo.com.cn)
收稿日期:2008-08-11
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