碳酸二乙酯作为乙基化试剂合成对硝基苯乙醚  

SYNTHESIS OF p-NITROANISOLE WITH DIETHYL CARBONATE AS ETHYLATION REAGENT

作　　者：李永昕[1] 张舒乐[1] 柳娜[1] 薛冰[1] 

机构地区：[1]江苏工业学院化学化工学院,江苏常州213164

出　　处：《精细石油化工》2009年第3期20-23,共4页Speciality Petrochemicals

基　　金：国家重大基础研究前期研究项目(2003CCA03200);江苏省高技术研究项目(BG2006015);江苏省高校重大基础研究项目(06KJA5013)

摘　　要：制备了负载型KOH/活性炭催化剂,研究了以碳酸二乙酯(DEC)与对硝基苯酚为原料在固体碱催化剂上液相合成对硝基苯乙醚的工艺方法。结果表明,以活性炭(AC)为载体,以KOH为活性组分,当KOH负载量达到20%时,催化剂的催化活性最高,并且催化剂的碱强度达到最大。采用CO_2-TPD对KOH/AC的碱性质进行了表征,结果表明,弱碱性位是该反应的活性位。考察了反应温度、反应时间、DEC和对硝基苯酚的摩尔比和催化剂用量对反应的影响。适宜的反应条件为:反应温度423 K、反应时间2 h、催化剂用量10%、n (DEC):n(对硝基苯酚)=12.5:1,在此条件下对硝基苯酚的转化率达到89.4%,对硝基苯乙醚的选择性达到100%。O-alkylation of p-nitrophenol with diethyl carbonate （DEC） in liquid phase was conducted to synthesize p-nitroanisole over solid base catalysts. The results showed that KOH/active carbon （AC） with KOH loading amount of 20% exhibited the highest catalytic activity. The base properties of KOH/AC were characterized by CO2-TPD. It was found that weak basic sites were the active sites for this reaction. The amount of basic sites on KOH/AC increased with increasing KOH loadings. A decrease in amount of basic sites was detected when KOH loadings were over 20%. The effects of reaction temperature, reaction time, molar ratio of DEC to p-nitrophenol and catalyst dosage on the reaction were investigated. Under the optimum reaction conditions, i. e. , reaction temperature 423 K, reaction time 2 h, catalyst dosage 10% and n（DEC） ： n（p-nitrophenol）= 12.5 ： 1, p-nitrophenol conversion and the selectivity to p-nitroanisole reached 89.4% and 100%, respectively.

关 键 词：碳酸二乙酯 对硝基苯酚 对硝基苯乙醚 氢氧化钾 活性炭 

分 类 号：TQ246.1[化学工程—有机化工]