NaY分子筛负载金属Salen催化剂催化α-蒎烯环氧化

Preparation of NaY Molecular Seive Loaded with Salen-metal Complexes for Catalyzing the Epoxidation of α-Pinene

采用普通热溶剂法和微波加热法将SalenMnCl成功负载于NaY分子筛的超笼中,通过FT-IR、XRD、TG和比表面分析方法对催化剂进行了表征。以此负载型催化剂催化低浓度过氧乙酸氧化α-蒎烯制备α-环氧蒎烷,比较了2种方法制备的催化剂性能,然后用响应曲面法探索最佳反应条件,并在该条件下研究负载型催化剂循环使用情况。结果表明,2种方法制备的分子筛负载型SalenMnCl催化剂均可催化α-蒎烯环氧化反应,且催化效果微波法优于普通热溶剂法。微波法制备的SalenMnCl/Y-MW催化剂催化反应的最优条件为:过氧乙酸与α-蒎烯物质的量之比值为1.43,反应温度为10℃,反应时间为3.75 h,在此条件下产物产率达91.60%。同时,该负载型催化剂重复使用5次,产物产率仍达76%以上,其具有较好的稳定性,可循环利用。

Immobilization of Mn（ salen） complex into the super-cage of Zeolite Y was achieved via traditional solvothermal method（ SalenMnCl/Y） and microwave heating method（ SalenMnCl/Y-MW）,respectively. And FT-IR,XRD,TG and Specific surface area analysis were used to characterize the catalysts which were employed to catalyze the epoxidation of α-pinene to getα-poxypiene by peracetic acid under the low catalyst concentration. Comparative study of the performance of catalysts prepared by two methods was carried out. The optimal reaction condition was investigated by response surface methodology and used to evaluate the performance of the recycle catalyst. The results showed that although the catalysts prepared by two methods can both successfully catalyse α-pinene epoxidation,microwave heating method however is priority to traditional solvothermal method. The yield can reach 91. 60 % with the catalyst of SalenMnCl /Y-MW under the following conditions,i. e.,peroxide and α-pinene mole ratio 1. 43,the reaction temperature 10 ℃ and the reaction time 3. 75 h. Meanwhile,this type of catalyst can be recycled for5 times and the yield also can reach 76 %. It indicates that this type of catalyst has good stability and can be recycled.