锆掺杂MCM-41介孔分子筛的水热合成与稳定性  

Stability and Hydrothermal Synthesis of Zirconium Incorporated MCM-41 Mesoporous Molecular Sieve

作　　者：赵谦[1] 李文静[1] 沈玉堂[1] 周旭平[1] 李梅[1] 姜廷顺[1] 

机构地区：[1]江苏大学化学化工学院,镇江212013

出　　处：《纳米技术与精密工程》2009年第5期397-402,共6页Nanotechnology and Precision Engineering

基　　金：镇江市工业攻关项目(GY2006017);江苏大学高级人才基金资助项目(JDG2006074)

摘　　要：水热条件下,以硅酸钠和硫酸锆为原料,十六烷基三甲基溴化铵(CTAB)为模板剂,按照初始的ZrO2与SiO2物质的量之比0.05、0.1、0.2和0.3合成了4种不同锆含量的含锆介孔分子筛(ZrMCM-41).采用X射线衍射(XRD)、红外光谱(FT-IR)、透射电子显微镜(TEM)和比表面积孔径测定等方法对样品的结构和形貌进行了表征.考察了不同ZrO2与SiO2物质的量之比、不同焙烧温度以及不同水热处理时间对样品孔结构的影响.结果表明:合成的样品具有典型的MCM-41介孔结构,其比表面积为448.6~891.9 m2/g.随着样品中锆含量的增加、焙烧温度的升高和水热处理时间的延长,所合成样品的介孔有序性下降,BET比表面积降低.According to the initial molar ratios of ZrO2∶SiO2(0.05,0.1,0.2 and 0.3,respectively),four zirconium incorporated MCM-41 mesoporous molecular sieves(ZrMCM-41) were synthesized under hydrothermal condition using cetyl trimethyl ammonium bromide(CTAB) as a template and sodium silicate and zirconium sulfate as raw materials.The structure and morphology of the samples were characterized via various physicochemical methods such as X-ray diffraction(XRD),transmission electron microscopy(TEM),Fourier transform infrared spectroscopy(FT-IR),thermal gravimetric-differential scanning calorimeter(TG-DSC) and N2 physical adsorption.The effects of the initial molar ratio of ZrO2∶SiO2,the thermal treatment temperature and the hydrothermal treatment time on the pore structure were also investigated.Experimental results reveal that the as-synthesized samples possess a typical mesoporous structure of MCM-41 and have specific surface area in the range of 448.6—891.9 m2/g.On the other hand,with the increase in the zirconium content of the synthesized ZrMCM-41 mesoporous molecular sieve and the rise of thermal treatment temperature and the prolonging of hydrothermal treatment time,the mesoporous ordering gradually deteriorates and the Brunauer-Emmett-Teller(BET) specific surface area gradually decreases.

关 键 词：MCM-41介孔分子筛 锆掺杂介孔分子筛 水热合成 表征 稳定性 

分 类 号：O643.36[理学—物理化学]