三相相转移催化合成邻硝基苯甲醚的工艺条件  

Synthesis Process of o-Nitroanisole over Triphase Transfer Catalysts

作　　者：陈亚飞[1] 周文[2] 梅华[1] 陈晓蓉[1] 

机构地区：[1]南京工业大学化学化工学院,江苏南京210009 [2]北京市防化研究院,北京102205

出　　处：《化学反应工程与工艺》2014年第2期145-149,共5页Chemical Reaction Engineering and Technology

基　　金：江苏省科技厅产学研前瞻(BY2012033)

摘　　要：以聚苯乙烯-二乙烯苯阴离子树脂固载聚乙二醇400作为三相相转移催化剂(PS-C5)催化邻氯硝基苯(ONCB)甲氧基化合成邻硝基苯甲醚(ONA)。考察了甲醇、氢氧化钠及催化剂用量、反应温度等工艺条件对反应的影响。实验结果表明,在邻氯硝基苯为0.1 mol,甲醇为0.6 mol,30 g质量分数40%的NaOH,4 g催化剂PS-C5,反应温度70℃,反应时间10 h的适宜条件下,邻氯硝基苯转化率大于99.5%,邻硝基苯甲醚收率达到93.4%。催化剂回收简单并可以重复使用六次以上,催化性能无明显下降。The triphase transfer catalyst PS-C5 was synthesized by polystyrene-o-divinylbenzene anion resin supported polyethylene glyol（PEG-400） and used to catalyze the o-nitroanisole （ONA） synthesis process from o-nitrochlorobenzene （ONCB）. The influence of process conditions such as methanol amount, sodium hydroxide amount, catalyst dosage and reaction temperature on ONCB conversion were investigated. Under the better reaction conditions, such as ONCB 0.1mol, CH3OH 0.6mol, 40%NaOH 30 g, PS-C5 4 g, reaction temperature 70 ℃ and reaction time 10 h, the ONCB conversion reached 99.5%and the yield of ONA was 93.4%. The catalyst can be recovered easily and its catalytic performance is not decreased evidently for 6th used.

关 键 词：三相相转移催化剂 邻氯硝基苯 邻硝基苯甲醚 

分 类 号：TQ246.1[化学工程—有机化工]