摘要
以质量分数30%的过氧化氢为氧化剂,Na2WO4.2H2O为催化剂,乙酸为溶剂,在酸性配体存在条件下,进行菲催化氧化制2,2'-联苯二甲酸。考察反应条件对产率的影响,确定较佳工艺为:菲25 mmol,30%过氧化氢用量20 mL,Na2WO4.2H2O用量0.5 mmol,草酸2 mmol,在8 mL乙酸中回流反应3 h,得到高纯度2,2'-联苯二甲酸,收率达72%。产品结构经IR、1H NMR、13C NMR和元素分析进行了表征。
Using 30% hydrogen peroxide as the oxidant,Na2WO4 · 2H20 as the catalyst and acetic acid as the solvent,2,2＇-diphenic acid was synthesized by catalysis oxidation of phenanthrene in the presence of acid ligands. The effects of reaction conditions on the yield were investigated. The optimal conditions were determined as follows ： phenanthrene 25 mmol, 30% H202 20 mL, Na2WO4 · 2 H20 0.5 mmol, oxalic acid 2 mmol, acetic acid 8 mL, and reflux time 3 h. 2,2＇-Diphenic acid with high purity was obtained and its yield reached 72%. The product was characterized by IR,1H NMR, 13C NMR and elemental analysis.
出处
《工业催化》
CAS
2012年第10期60-62,共3页
Industrial Catalysis
关键词
精细化学工程
菲
联苯二甲酸
过氧化氢
催化氧化
fine chemical engineering
phenanthrene
diphenic acid
hydrogen peroxide
catalytic oxidation
