NiMCM-41介孔分子筛的微波合成与表征  

Characterization and Microwave Synthesis of NiMCM-41 Mesoporous Molecular Sieves

作　　者：赵谦[1] 陶蓉蓉[1] 荆俊杰[1] 张蓉仙[1] 

机构地区：[1]江苏大学化学化工学院,江苏镇江212013

出　　处：《中北大学学报（自然科学版）》2010年第6期608-613,共6页Journal of North University of China(Natural Science Edition)

基　　金：江苏大学高级人才基金(06JDG074);镇江市工业攻关项目(GY2006017)

摘　　要：以硅酸钠（Na2SiO3.9H2O）、氯化镍（NiCl2.6H2O）等无机盐为原料,十六烷基三甲基溴化铵（CTAB）为模板剂,通过微波辐射方法合成不同镍含量的NiMCM-41介孔分子筛.采用X射线粉末衍射（XRD）、红外光谱（FT-IR）、透射电子显微镜（TEM）、等离子发射光谱（ICP-OES）、程序升温还原（TPR）和N2吸附-脱附等技术,分别对经550℃焙烧后的样品进行表征.同时研究金属镍添加量与比表面积、孔体积之间的关系.结果显示：合成的样品具有典型的MCM-41介孔分子筛结构,表明在微波辐射条件下成功合成出4种不同镍含量的NiMCM-41介孔分子筛,其比表面积在625.8~1 161.3 m2/g之间,平均孔径大约2.7 nm.随着介孔分子筛中金属镍含量的增加,介孔分子筛的比表面积、孔体积变小,介孔有序性变差.其中原料配比n（SiO2）∶n（NiO）=1∶0.05时,合成的NiMCM-41介孔分子筛的介孔有序性最好.NiMCM-41 mesoporous molecular sieves with different content of nickel incorporated in the framework were synthesized from sodium silicate,nickel chloride and using cetyltrimethyl ammonium bromide as a template by a novel microwave irradiation method.The calcined samples were characterized by X-ray diffraction（XRD）,transmission electron microscopy（TEM）,inductive coupled plasma（ICP-OES）,Fourier transform infrared spectroscopy（FT-IR）,temperature programmed reduction（TPR） and N2 physical adsorption,respectively.The experimental results show that the synthesized samples have a typical mesoporous structure of MCM-41,indicating that NiMCM-41 mesoporous molecular sieves are successfully synthesized under microwave irradiation condition,and have specific surface area in a range of 625.8~1 161.3 m2/g and an average pore size of ca. 2.7 nm.On the other hand,specific surface area and pore volume of the synthesized NiMCM-41 mesoporous molecular sieve decrease with the increase of the amount of nickel doped,and the mesoporous ordering becomes poor.Also,when the molar ratio of SiO2 to NiO in the original material is 1∶0.05,the ordering of the synthesized NiMCM-41 mesoporous molecular sieve is the best among the four doping contents.

关 键 词：NiMCM-41介孔分子筛 微波法 合成 表征 

分 类 号：O643[理学—物理化学]