TS分子筛的催化氧化性能研究Ⅴ.环己酮氨肟化反应  

Study on Catalytic Oxidation Activity of TS Zeolite V . Ammoximation of Cyclohexanone

作　　者：李平[1] 卢冠忠[1] 罗勇[1] 代亚男 

机构地区：[1]华东理工大学工业催化研究所,上海200237

出　　处：《化学学报》2000年第2期204-208,共5页Acta Chimica Sinica

基　　金：上海市"优秀学科带头人"资助计划(97DX14004);国家教委"跨世纪优秀人才培养计划"基金资助

摘　　要：研究了自制的钛硅分子筛(TS-1)催化H_2O_2参与的环己酮氨肟化反应.结果表明,降低反应溶液中H_2O_2的浓度、增加NH_3用量有利于H_2O_2利用率、环己酮肟收率和选择性的提高,适宜的n(H_2O_2):n(酮)<1.0,n(NH_3):n(酮)>2.0.反应时间应控制在3.5h左右.对溶剂的研究显示,叔丁醇在溶剂中所占的体积对反应有较大的影响,在叔丁醇体积分数为0.2到0.8之间,实验获得了较好的结果.当n(NH_3):n(H_2O_2):n(酮)=2.0:1.0:1.0,叔丁醇体积分数为0.5,反应时间2.5h,反应温度353K时,H_2O_2利用率、环己酮肟收率和选择性分别达95%,94%和97%以上.并对空白实验结果和TS-1的重复性试验进行了讨论.Ammoximation of cyclohexanone with ω(H2O2) = 30% aqueous hydrogen peroxide and ammonia in the presence of a titanium silicalite (TS - 1) catalyst was studied. Decreasing the content of H2O2 and increasing the amount of NH3 in the reaction solution, increase the utilization of H2O2 and the yield as well as the selectivity of cyclohexanone to oxime. The favorable reaction time is about 3. 5h. The effect of the volume fraction of t - butyl alcohol in the solvent on the ammoximation is discussed in detail. The experiment results show that when the molar ratio of n(NH3) : n(H2O2) : n(ketone) is 2.0:1.0:1.0, the volume fraction of t -butyl alcohol is 0.5, and the reaction time is 2. 5h at 353K, the utilization of H2O2 and the yield and selectivity of cyclohexanone oxime can reach 95% , 94% and 97% respectively.

关 键 词：钛硅分子筛 催化氧化 环己酮 氨肟化 生产工艺 

分 类 号：O643.3[理学—物理化学]