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J4  2011, Vol. 45 Issue (3): 563-565    DOI: 10.3785/j.issn.1008-973X.2011.03.027
化学工程﹑环境工程     
乙酸对硝基苯酯的合成
计立1, 毛筱媛2, 钱超1, 陈新志1
1.浙江大学 化学工程与生物工程学系, 浙江 杭州 310027;2.浙江工业大学
化学工程与材料学院, 浙江 杭州 310014
Synthesis of p-nitrophenyl acetate
JI Li1, MAO Xiao-yuan2, QIAN Chao1, CHEN Xin-zhi1
1.Department of Chemical and Biological Engineering, Zhejiang University, Hangzhou 310027, China;
2.College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, China
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摘要:

为了解决乙酸对硝基苯酯(PNPA)工业生产中设备腐蚀严重﹑收率较低的问题,以对硝基氯苯(PNCB)为原料, 在加压条件下经碱性水解, 直接与乙酸酐反应合成PNPA, 分别研究了反应温度、反应时间、碱液所含氢氧化钠的质量分数等条件对合成反应的影响. 该方法合成对硝基苯酚钠的最佳工艺条件如下:反应温度为140 ℃, 反应压力为0.3 MPa, 反应时间为10 h, PNCB与氢氧化钠的投料量摩尔比为1∶2.5, 最佳碱液中氢氧化钠的质量分数为15%, PNPA的收率为90.6%.

Abstract:

A novel process was developed in order to solve the problems in the manufacturing of p-nitrophenyl acetate (PNPA) , such as equipment corrosion and low yielding. The p-nitrophenyl acetate was synthesized by the acetylization of sodium p-nitrophenolate, which was prepared by the hydroxylation of pnitrochlorobenzene (PNCB) under pressure. The effects of reaction temperature, reaction time, alkali liquor concentration on the synthesis were studied. The proper technological conditions of sodium p-nitrophenolate preparation were given as follows:  140 ℃,  0.3 MPa, the reaction time is 10 h, the molar ratio of sodium hydroxide and p-nitrochlorobenzene was 2.5, the optimal mass fraction of lye was 15%. The yield of p-nitrophenyl acetate was 90.6%.

出版日期: 2012-03-16
:  TQ 243.1  
基金资助:

国家“十一五”科技支撑计划资助项目(2007BAI34B07);国家自然科学基金资助项目(20776127);浙江省自然科学基金资助项目(Y4090045,R4090358).

通讯作者: 钱超, 男, 助理研究员.     E-mail: supmoney@163.com
作者简介: 计立(1986-), 男, 浙江海宁人, 博士生, 从事精细有机合成研究. E-mail: jili05@hotmail.com
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引用本文:

计立, 毛筱媛, 钱超, 陈新志. 乙酸对硝基苯酯的合成[J]. J4, 2011, 45(3): 563-565.

JI Li, MAO Xiao-yuan, QIAN Chao, CHEN Xin-zhi. Synthesis of p-nitrophenyl acetate. J4, 2011, 45(3): 563-565.

链接本文:

http://www.zjujournals.com/eng/CN/10.3785/j.issn.1008-973X.2011.03.027        http://www.zjujournals.com/eng/CN/Y2011/V45/I3/563

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