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硒催化CO/H2O体系水相还原1-硝基蒽醌制1-氨基蒽醌
引用本文:高扬,兰诗龙,张欣,刘晓智.硒催化CO/H2O体系水相还原1-硝基蒽醌制1-氨基蒽醌[J].染料与染色,2013(5):51-53.
作者姓名:高扬  兰诗龙  张欣  刘晓智
作者单位:[1]辽宁大学化学院,沈阳110033 [2]沈阳化工研究院有限公司,沈阳110036
基金项目:辽宁省教育厅自然基金(L2012002);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:用硒作催化剂,CO/H2O体系水相高压还原1-硝基蒽醌制1-氨基蒽醌,选用碳酸氢钠为助催化剂。由L9(34)正交实验得出各因素对反应的影响强弱顺序为:水量>压强>Se量>温度。最佳反应条件为:1-硝基蒽醌1.265 g(5 mmol),Se用量0.0158 g(0.2 mmol),水量30 mL,NaHCO3用量0.42 g(5 mmol),反应温度150℃,压强5.0 MPa,反应时间3小时。1-氨基蒽醌的纯度为96.53%,最高收率大于98%。

关 键 词:  还原  1-硝基蒽醌  1-氨基蒽醌  一氧化碳  水相

Selenium-catalyzed Reduction of 1-Nitroanthraquinone to Prepare 1-Aminoanthraqinone with CO/H2O in Aqueous Solution
GAO Yang,LAN Shi-long,ZHANG Xin,LIU Xiao-zhi.Selenium-catalyzed Reduction of 1-Nitroanthraquinone to Prepare 1-Aminoanthraqinone with CO/H2O in Aqueous Solution[J].Ranliao yu Ranse,2013(5):51-53.
Authors:GAO Yang  LAN Shi-long  ZHANG Xin  LIU Xiao-zhi
Affiliation:1. Chemistry collage, Liaoning University, Shenyang 110033, Liaoning China; 2. Shenyang Research Institute of Chemical Industry, Shenyang 110021, Liaoning China)
Abstract:1-Aminoanthraqinone was prepared from 1-nitroanthraquinone by high pressure reduction of CO/H2O in aqueous solution in the presence of catalyst selenium and cocatalyst NaHCO3. The effect order of different factors for the reduction was gotten by orthogonal experiments L9 (3^4 ) : amount of water 〉 pressure 〉 amount of selenium 〉 temperature. The optimum condition was 1-nitroanthraquinone 1. 265 g (5 mmol), Se 0. 0158 g (0. 2 mmol), H2O 30 mL; NaHCO30. 42 g (5 mmol), T = 150℃, PCO =5.0 MPa, reaction time 3 hours. The highest yield of 1-aminoanthraquinone was more than 98% and purity of product was 96. 53%.
Keywords:selenium  reduction  1-nitroanthraquinone  1-aminoanthraquinone  monoxide carbon  aqueous
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