以介孔分子筛KIT-6为载体,采用溶液浸渍法将乙酰丙酮锰(III)的糠醇溶液灌注到KIT-6的孔道内,一定条件下将糠醇碳化后再焙烧脱除碳,制得Mn-KIT-6催化剂.通过X射线衍射(XRD);氮气物理吸附-脱附;紫外-可见吸收光谱(UV-Vis);傅里叶变换红外光谱(FT-IR);电感耦合等离子发射光谱(ICP-AES);透射电镜(TEM);氨气-程序升温脱附(NH3-TPD)及X射线光电子能谱(XPS)等方法对样品进行了表征.结果表明锰在KIT-6孔道内部高度分散,同时催化剂保持高度有序的孔道结构、较大的比表面积和孔容.正丁醇和乙酸的催化酯化反应结果表明,该催化剂具有很高的催化活性,反应4 h后乙酸正丁酯的产率高达97.3%,使用5次后催化剂依然具有较高的活性.
In this paper,highly dispersed Mn-KIT-6 catalysts were prepared via a simple incipient wetness co-impregnation route by casting furfurylalcohol(FA) solution of manganese(III) acetylacetonate,which were used as carbon and Mn sources,respectively,into the channels of KIT-6,followed by the subsequent removal of the carbon resulted from carbonized FA.The catalysts were characterized by X-ray diffraction(XRD),N2 adsorption-desorption,UV-visible absorption spectroscopy(UV-Vis),Fourier transform infrared spectroscopy(FT-IR);inductively coupled plasma emission spectroscopy(ICP-AES),transmission electron microscope(TEM),temperature programmed desorption of ammonia(NH3-TPD) and X-ray photoelectron spectroscopy(XPS).The results showed that Mn species were highly dispersed onto the pore surface of KIT-6 with the well maintenance of the highly ordered meso-structure of KIT-6.The catalysts exhibited high catalytic activity in the etherification of N-butanol and acetic acid,with the yield of butyl acetate as high as 97% after 4 h reaction.The reusability and stability were demonstrated with the high activity after 5 runs.