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江苏大学化学化工学院
Published:2010
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赵谦, 陶蓉蓉, 荆俊杰, et al. Characterization and Microwave Synthesis of NiMCM-41 Mesoporous Molecular Sieves[J]. 2010, 31(6): 608-613.
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 surfa
ce 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.
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