CO/H_2O体系水相还原制备1-氨基蒽醌  

Reduction Preparing 1-Aminoanthraqinone with CO/H_2O in Aqueous Solution

作　　者：刘云法 安萌[1] 卢圣茂 王志伟 尹明娟 刘晓智[1] 

机构地区：[1]辽宁大学化学院,沈阳110033 [2]盐城市瓯华化学工业有限公司,盐城224555

出　　处：《染料与染色》2016年第6期28-30,42,共4页Dyestuffs and Coloration

基　　金：辽宁省教育厅自然基金(12012002);创新团队项目(LT2012001);沈阳市重点实验室项目(F13-289-1-00)的资金支持

摘　　要：该反应以硫和硒作为催化剂,CO作为还原剂,在高温高压下还原1-硝基蒽醌制备1-氨基蒽醌。通过探究实验条件,选出了在底物量为6.00 g(27mmol)的前提下,确定了较优的反应条件:S 0.100 0 g(3.1 mmol);Se 0.015 8 g(0.2 mmol);Na HCO_3 2.00g;H_2O 40m L;反应温度150℃;压强PCO6 MPa;反应时间6h。高效液相色谱测得产物纯度最高可达98.18%。1-Aminoanthraqinone was prepared from 1-nitroanthraqinone by high pressure reduction of CO/H2O in cyclohexane solvent in the presence of catalyst sulfur/selenium. The optimum condition was obtained by experiments： 1- nitroanthraquinone 6. 00 g（ 27mmol）,S 0.1500 g（ 0. 47 mmol）,Se 0. 0158 g（ 0. 20 mmol）,H2O 40 m L,Na HCO32. 00 g,temperature 150 ℃,PCO6.0 MPa and reaction time 6 hours. 1-Aminoanthraqinone yield was 98. 18%. The effect order of different factors for the reduction was gotten by orthogonal experiments L16（ 45） ： the amount of selenium powder 〉 reaction temperature〉CO gas pressure〉the amount of sulfur powder〉reaction time.

关 键 词：硫 一氧化碳 水相还原 1-氨基蒽醌 

分 类 号：TQ613.2[化学工程—精细化工]