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作 者:宋成盈[1] 刘志生[1] 王留成[1] 赵建宏[1] 徐海升[1] 王福安[1]
出 处:《精细化工》2007年第7期684-687,共4页Fine Chemicals
基 金:河南省自然科学基金项目(0611023300)~~
摘 要:以Ti/PbO2为阳极、Pb为阴极、硫酸为支持电解质,采用Cr6+/Cr3+为氧化媒质,四丁基溴化铵为相转移剂,在阳离子交换膜为隔膜的“板框式”电解槽中,进行“槽内式”间接电氧化2-甲基萘(2-MN)合成2-甲基-1,4-萘醌(2-MNQ)的研究。考察了2-MN间接电氧化制备2-MNQ的工艺条件对2-MNQ选择性和电流效率的影响规律。实验结果表明:在2-MN和Cr2O72-浓度分别为0.02 mol/L和0.03 mol/L,硫酸质量分数20%,温度50℃,电流密度110 A/m2,通电量为理论通电量0.2倍的工艺条件下进行电解,2-MNQ的平均选择性为71.9%,平均表观电流效率为69.7%。2-Methyl-1,4-naphthoquinone ( 2-MNQ ) was prepared from 2-methylnaphthalene (2-MN) by "in-cell" indirect electrolytic oxidation, using cation-exchange membrane as diaphragm, Ti/PbO2 as anode,Pb as cathode, sulfuric acid as supporting electrolyte, Cr^6+/Cr^3+ as oxidative medium and tetrabutylammonium bromide as phase transfer agent. The process conditions for synthesizing 2-MNQ were optimized in the plate and frame electrolytic cell. Under the optimum conditions that c(2-MN) = 0. 02 mol/L,c( Cr2O7^2- ) = 0. 03 mol/L, w ( H2SO4 ) = 20% , reaction temperature = 50 ℃, current density = 110 A/m^2 and the electric quantity was 0. 20 times the theoretical value, the mean selectivity for 2-MNQ was 71.9% ,and the mean apparent current efficiency was 69.7%.
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