分子筛固载型Cosalen的制备、表征及其应用研究  

Preparation of molecular sieve immobilized Cosalen and its characterization and application

作　　者：单高峰[1] 袁霞[1] 吴剑[1] 

机构地区：[1]湘潭大学化工学院,湖南湘潭411105

出　　处：《现代化工》2009年第S1期164-167,共4页Modern Chemical Industry

基　　金：国家自然科学基金重点项目资助(20736009)

摘　　要：分别采用NaY分子筛、γ-氨丙基三乙氧基硅烷修饰的MCM-41分子筛固载双水杨醛缩乙二胺合钴(Cosalen)配合物,制备了固载型Cosalen/NaY、Cosalen/MCM-41催化剂。采用傅里叶变换红外光谱、热重-差热、X射线衍射、比表面积测定等方法对固载型分子筛催化剂的结构进行表征。结果表明,Cosalen已成功地进入分子筛孔道内。在以氧气为氧源的环己烷氧化反应中,Cosalen/MCM-41催化剂具有较好的活性和对环己醇、环己酮的选择性。该催化反应体系产物中环己基过氧化氢(CHHP)的量很少,表明Cosalen/MCM-41催化剂能加速CHHP的分解。在初始氧气压力0.80MPa、温度130℃、环己烷用量30g、Cosalen/MCM-41用量0.30g、叔丁基过氧化氢0.10g的条件下反应2h,环己烷的转化率达到5.96%,醇酮选择性87.03%。N,N′-bis(salicylidene)ethylenediiminocobalt (Cosalen) is encapsulated into both the supercage of microporous NaY zeolite and the mesoporous molecular sieve (MCM-41) which modified by 3-triethoxysilylpropylamine.The prepared samples are characterized by FT-IR,TG-DSC,XRD,BET.The results show that Cosalen has incorporated into matrix of the both samples.The catalytic performance of the samples for the cyclohexane liquid-phase oxidation into cyclohexanone and cyclohexanol by oxygen is investigated in the absence of solvents.Only small amount of cyclohexyl hydroperoxide(CHHP) analyzed in products indicates that Cosalen/MCM-41 catalyst can accelerate decomposition of CHHP.The oxidation reaction of cyclohexane is studied and the optimum reaction conditions are obtained as follows:0.8 MPa of initial oxygen pressure,130℃ of temperature,30 g of cyclohexane,0.30 g of Cosalen/MCM-41 used as the catalyst,0.10 g of TBHP and 2 h of reaction time.The conversion of cyclohexane can reach 5.96% and the selectivity of cyclohexanone and cyclohexanol can be up to 87.03%.

关 键 词：环己烷氧化 氧气 Cosalen 分子筛 

分 类 号：O643.32[理学—物理化学]