考察了系列氧化剂、催化剂和溶剂对环己胺液相氧化制备环己酮肟的影响,发现以乙腈为溶剂,过氧化氢为氧化剂,NaY型沸石分子筛对该反应具有优良的催化性能.对该反应体系进行了五因素四水平的正交实验,确定了适宜的催化剂用量、溶剂用量、反应时间、反应温度和氧化剂用量,比较分析了各因素对环己胺转化率和环己酮肟选择性的影响.确定了环己胺液相氧化反应的最佳工艺条件为:环己胺为3 mL,催化剂为0.3g,环己胺、溶剂和氧化剂的体积比为1∶3∶3,65℃反应2h.讨论了环己胺液相催化氧化的反应机理.
参考文献
| [1] | Suzuki K,Nagahara H.Process for Preparation of Cyclohexanone Oxime:US 0176592 A1[P].2004-9. |
| [2] | Ichihashi H,Sato H.The Development of New Heterogeneous Catalytic Processes for the Production of ε-Caprolactam[J].Appl Catal,2001,221(1/2):359-366. |
| [3] | Corma A,Sema P.Chemoselective Hydrogenation of Nitro Compounds with Supported Gold Catalysts[J].Science,2006,313:332-334. |
| [4] | MAO Liqiu,LV Xing,YIN Dulin,et al.Hydrogenation of Nitrocyclohexane to Cyclohexanone Oxime Catalyzed by Pd/C[J].Chem Ind Eng Prog,2009,28(6):1024-1026(in Chinese).毛丽秋,吕兴,尹笃林,等.Pd/C催化硝基环己烷氢化制备环己酮肟[J].化工进展,2009,28(6):1024-1026. |
| [5] | WU Bohua,MAO Liqiu,YIN Dulin,et al.One-step Synthesis of Caprolactam by Liquid-phase Nitrosation Reaction of Cyclohexane[J].Chinese J Appl Chem,2008,25(4):502-504(in Chinese).吴伯华,毛丽秋,尹笃林,等.环己烷液相亚硝化一步合成己内酰胺反应的研究[J].应用化学,2008,25(4):502-504. |
| [6] | Rakottyay K,Kaszonyi A.Oxidation of Cyclohexylamine over Modified Alumina by Molecular Oxygen[J].Appl Catal A,2009,367(1/2):32-38. |
| [7] | GAO Meixiang,LUO Dong,MAO Liqiu,et al.Oxidation of Cyclohexylamine to Cyclohexanone Oxime Catalyzed by Al2O3-SiO2[J].Chinese J Appl Chem,2013,30 (1):28-31 (in Chinese).高美香,罗东,毛丽秋,等.Al2O3-SiO2催化环己胺氧化制备环己酮肟[J].应用化学,2013,28(1):28-31. |
| [8] | Gu F N,Wei F,Yang J Y.New Strategy to Synthesis of Hierarchical Mesoporous Zeolites[J].Chem Mater,2010,22:2442-2450. |
| [9] | Orthogonal Test Drafting Group.Orthogonal Test[M].Beijing:Publishing House of Defense Industry,1976:7-25 (in Chinese).正交试验编写组.正交试验法[M].北京:国防工业出版社,1976:7-25. |
| [10] | XU Ruren,PANG Wenqin,YU Jihong,et al.Chemistry-Zeolites and Porous Materials[M].Beijing:Science Press,2004:170-175 (in Chinese).徐如人,庞文琴,于吉红,等.分子筛与多孔材料化学[M].北京:科学出版社,2004:170-175. |
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%