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机构地区:[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
出 处:《浙江大学学报(工学版)》2011年第3期563-565,共3页Journal of Zhejiang University:Engineering Science
基 金: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)
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0.3MPa,反应时间为10h,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%.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%.
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