研究了在乙酸中,用H2O2氧化1-萘胺合成1,4-萘醌的新方法.考察了反应温度、反应时间、1-萘胺与H2O2摩尔比、硫酸和H2O2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-萘胺与H2O2摩尔比为1∶10、H2O2质量分数为5％、硫酸质量分数为45％、反应温度为80℃、反应时间为3h.在此条件下,1,4-萘醌的收率为52.2％.该方法具有操作简单、反应时间短和产物易分离等优点.
参考文献
| [1] | WANG Shuqing.Research Progress of Oxidation of Alkylated Aromatic Hydrocarbon[J].J Petrochem Univ,1998,11(2):40-46(in Chinese).汪树清.烷基芳香烃氧化反应的研究进展[J].石油化工高等学校学报,1998,11(2):40-46. |
| [2] | M(o)ller K,Wienh(o)fer G,Schr(o)der K,et al.Selective Iron-Catalyzed Oxidation of Phenols and Arenes with Hydrogen Peroxide:Synthesis of Vitamin E Intermediates and Vitamin K3[J].Chem Eur J,2010,16(34):10300-10303. |
| [3] | Spotnitz R M.Mediated Electrosynthesis with Cerium(Ⅳ) in Methanesulphonic Acid[J].J Appl Electrochem,1990,20:209-215. |
| [4] | HAN Shiqing,YANG Zhenyun,ZHENG Lubin.Improvement of Preparative Method of Naphthquinone from Naphthalene Using Cerium(Ⅳ) Salt as Oxidant[J].Chem Reag,1998,20(3):189(in Chinese).韩世清,杨振云,郑禄彬.铈(Ⅳ)盐氧化萘制备萘醌的方法改进[J].化学试剂,1998,20(3):189. |
| [5] | Oehr Klaus H.Process for Producing Naphthoquinone:CA,1132996[P],1980-10-02. |
| [6] | Nanjing Chemical Industry Corporation Catalyst Company.Vanadium Catalyst[M].Beijing:Chemical Industry Press,1980:258-268 (in Chinese).南京化学工业公司催化剂厂.钒催化剂[M].北京:化学工业出版社,1980:258-268. |
| [7] | Ito S,Kuroda Y,Iwata M,et al.Duet Electrosynthesis Part Ⅱ:1,4-Naphthoquinone from Naphthalene[J].J Appl Electrochem,1993,23 (7):677-683. |
| [8] | JI Qingsong,YANG Jian,LIU Youquan.Synthesis of 1,4-Naphthquinone by Indirect Electro-oxidation[J].Chem World,1996,37(6):314-317(in Chinese).季青松,杨健,刘佑全.1,4-萘醌的间接电氧化合成[J].化学世界,1996,37(6):314-317. |
| [9] | XU Haisheng,ZHAO Jianhong.Research of Industrialization of Synthesis of Vitamin K3[J].Chem React Eng Technol,2002,18(4):334-338 (in Chinese).徐海升,赵建宏.维生素K3合成的工业化研究[J].化学反应工程与工艺,2002,18(4):334-338. |
| [10] | CAO Xiaoqun,LIU Xin,CHENG Yueshan.Study on Synthesis of 1,4-Naphthquinone[J].Fine Spec Chem,2006,14(12):18-20(in Chinese).曹晓群,刘欣,程岳山.1,4-萘醌的合成研究[J].精细与专用化学品,2006,14(12):18-20. |
| [11] | Ikeda Noriaki.Production of 1,4-Naphthquinone:JP,63270635[P],1987-04-30. |
| [12] | GAO Rong,TIAN Guang,WANG Jingguo,et al.Synthesis of 1,4-Naphthquinone from Naphthalene by Liquid-phase Oxidation:CN,85100335A[P],1985-04-01 (in Chinese).高榕,田光,王景国,等.萘液相氧化制1,4-萘醌的方法:中国,85100335A[P],1985-04-01. |
| [13] | Ройтер В А.Catalytic Oxidation of Naphthalene[M].TAO Hong,Trans.Beijing:China Industry Press,1965:101-113 (in Chinese).罗伊捷尔B A.萘的催化氧化[M].陶宏译.北京:中国工业出版社,1965:101-113. |
| [14] | Bernstein I,Cooper A.Catalytic Oxidation of Naphthalene:US,3776824[P],1973-07-04. |
| [15] | Wainwright M S,Bridgewater A J,Chaplin R P.The Formation of 1,2-Naphthoquinone in the Vanadia-catalysed Oxidation of Naphthalene[J].J Mol Catal,1986,38(3):383-385. |
| [16] | Walter Wettstein.Catalytic Masses for the Oxidation of Naphthalene to 1,4-Naphthoquinone:US,3095430[P],1963-06-25. |
| [17] | Nobuyuki I,Renard T L.Preparation of an Improved Catalyst for the Manufacture of Naphthoquinone:US,4533653[P],1985-08-06. |
| [18] | Matsuura Ryo,Yoshimura Shigeyuki.Process for Producing 1,4-Naphthoquinone:CA,1166263[P],1984-04-24. |
| [19] | Pausacjer K H,Scroggie J G.Oxidations with Lead Tetra-acetate:Part Ⅱ.The Oxidation of Primary Aromatic Amines[J].J Chem Soc,1954:4003-4006. |
| [20] | Bossmann S H,Oliveros E,G(o)b S,et al.New Evidence Against Hydroxyl Radicals as Reactive Intermediate in the Thermal and Photochemically Enhanced Fenton Reaction[J].J Phys Chem A,1998,102 (28):5542-5550. |
| [21] | Chen R,Pignatello J J.Role of Quinine Intermediates as Electron Shuttle in Fenton and Photoassisted Fenton Oxidations of Aromatic Compounds[J].Environ Sci Technol,1997,31 (8):2399-2406. |
上一张
下一张
上一张
下一张
计量
- 下载量()
- 访问量()
文章评分
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%