二次晶化法修饰改性钛硅分子筛及催化环己酮氨氧化反应  

Study of Ammoximation of Cyclohexanone over Titanium Silicalites Zeolite Catalyst Synthesized by Secondary Crystallized Method

作　　者：黄先亮[1] 周继承[1] 

机构地区：[1]湘潭大学化工学院,湖南湘潭411105

出　　处：《化学反应工程与工艺》2007年第6期553-559,共7页Chemical Reaction Engineering and Technology

摘　　要：采用无机钛硅原料合成了钛硅分子筛TS-1,经酸处理后对合成的钛硅分子筛TS-1进行二次晶化修饰改性。用X射线衍射仪(XRD)、傅立叶红外光谱(FT-IR)和扫描电子显微镜(SEM)对二次晶化后的钛硅分子筛进行表征,发现晶粒变小,钛进入了分子筛的骨架中。考察了二次晶化后的催化剂对环已酮氨氧化反应的催化性能。结果表明,二次晶化法可提高TS-1分子筛的催化性能,在氨、环己酮和过氧化氯的物质的量之比为2.0:1.0:1.5、催化剂用量为18g/mol和75℃的条件下,反应4h后,过氧化氢的转化率、环己酮的转化率和环己酮肟的收率分别为98.12%,97.07%和93.33%。The TS-1 zeolite, synthesized from inorganic titanosilicate and pretreated with acid, was modified by secondary crystallization method and was characterized by X-ray diffraction （XRD）, Fourier transformation infrared （FT-IR） spectrometer and scanning electron microscopy （SEM）. It was found that titanium could be incorporated into zeolite framework when the grain of TS-1 zeolite catalyst changed smaller. The catalytic performance of modified TS-1 zeolite for ammoximation of cyclohexanone was investigated. The results showed that the catalystic properties were improved. Under the optimized conditions of molar ratio of ammonia to cyclohexanone and hydrogen peroxide 2.0： 1.0： 1.5 and catalyst dosage 18 g/mol, the conversion of H2O2 and cyclohexanone and selectivity of cyclohexanone oxime were 98.12%, 97.07% and 93.33%, respectively, after reaction 4 h at 75 ℃.

关 键 词：钛硅分子筛 环己酮 环己酮肟 过氧化氢 氨氧化 

分 类 号：O643.32[理学—物理化学] TQ203.5[理学—化学]