含锆介孔分子筛的微波合成与表征(英文)

MICROWAVE SYNTHESIS AND CHARACTERIZATION OF ZIRCONIUM-CONTAINING MESOPOROUS MOLECULAR SIEVES

在微波辐射条件下,以硅酸钠和硫酸锆为原料、十六烷基三甲基溴化铵为模板剂合成含锆介孔分子筛(zirconium-containing mesoporous molecular sieves,Zr-MCM-41)。用X射线粉末衍射、红外光谱、透射电子显微镜、等离子发射光谱和比表面积孔径测定等测试手段表征经550℃焙烧后样品,同时研究锆添加量与分子筛比表面积及孔体积之间的关系。结果表明:利用微波技术合成Zr-MCM-41介孔分子筛,操作便利,节能省时,所得产物具有典型的MCM-41介孔分子筛结构,其比表面积为598.1～971.4m^2/g,平均孔径大约为2.46～3.43nm。随着介孔分子筛中锆含量的增加,介孔分子筛的比表面积、孔体积变小,介孔有序性变差。

Zirconium-containing mesoporous molecular sieves （Zr-MCM-41） were synthesized from sodium silicate and zirconium sulfate, using cetyltrimethyl ammonium bromide as a template under microwave irradiation conditions. The calcined samples were characterized by the X-ray diffraction, transmission electron microscope, inductive coupled plasma technique, Fourier transform in-frared spectroscopy, and N2 physical adsorption technique. The experimental results show that the reaction time and energy required in the synthesis of Zr-MCM-41 mesoporous molecular sieves by the microwave irradiation method are greatly reduced in contrast with those needed by the the conventional hydrothermal method. The obtained products possess a typical mesoporous structure of MCM-41and have specific surface areas in the range of 598.1 m^2/g to 971.4 m^2/g and average pore sizes in the range of circa 2.46 nm to 3.43 nm. On the other hand, the specific surface area and pore volume of the synthesized Zr-MCM-41 mesoporous molecular sieve decrease with the increase of the amount of Zr incorporated, and the mesoporous ordering deteriorates.