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机构地区:[1]天津大学化工学院精细化工系,天津300072
出 处:《精细化工》2013年第3期348-352,共5页Fine Chemicals
基 金:国家自然科学基金(21103121);教育部博士点基金(20110032120011)~~
摘 要:在硫酸介质中1-萘胺先形成硫酸铵盐,再经锰矿粉氧化合成1,4-萘醌。考察了反应温度、反应时间、原料摩尔比、反应介质、硫酸质量分数等因素对产品收率的影响。得到较优的反应条件为:1-萘胺1.8 g、n(1-萘胺)∶n(MnO2)=1∶7、w(H2SO4)=40%的硫酸61 g、反应温度80℃、反应时间3 h。在该条件下,1,4-萘醌的收率59.8%。该法具有操作简单、反应时间短和产物易分离等优点。1,4-Naphthoquinone was prepared by oxidation of 1-naphthylamine with manganese ore powder as oxidant in sulfuric acid which first reacted with 1-naphthylamine to form the related ammonium sulfate. The effects of reaction temperature, oxidation time, reactant molar ratio, types of acids, concentration of sulfuric acid on the product yield were investigated in detail. The optimal reaction conditions were as follows : 1 -naphthylamine 1.8 g, n ( 1 -naphthylamine) : n ( MnO2 ) = 1:7, mass fraction 40% sulfuric acid 61 g, reaction temperature 80 ℃, reaction time 3 h. The yield of 1,4-naphthoquinone was above 59.8% in this condition. This newly developed process has the advantages of convenient operation, easy separation of the product and short productive period.
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