摘要
首先采用sol gel法制备出ZrO(OH) 2 ,再分别用Ni2 + ,Al3 + ,Sn4+ ,Ag+ ,Sn2 + 金属盐溶液和H2 SO4稀溶液浸渍ZrO(OH) 2 的方法合成了一系列金属离子掺杂的SO2 -4/ZrO2 纳米固体超强酸。并用XRD ,TEM和IR技术考察了各样品的性能。结果发现 ,经不同金属掺杂的SO2 -4/ZrO2 颗粒具有固体超强酸的IR谱特征。经Ni2 + ,Sn4+ 掺杂的样品中Zr—O和 SO 键振动吸收峰明显蓝移 ,Zr—O的νZr—O由SO2 -4/ZrO2 的4 85cm-1增大到Ni2 + ,Sn4+ 掺杂样品的 5 0 0cm-1,SO的νas由 1390cm-1增大到 14 0 5和 14 0 0cm-1,而Sn2 + 掺杂的样品变化不大。说明Ni2 + ,Sn4+ 金属离子的掺杂增强了样品的超强酸性。同时还发现 ,随着样品焙烧温度的提高 ,经Ni2 + 和Al3 + 掺杂的SO2 -4/ZrO2 纳米颗粒 ,Zr—O和 SO 键振动吸收峰明显蓝移 ,而Ag+ 掺杂的样品在焙烧温度达到 10 73K时IR谱只是吸收强度减弱 ,振动频率不变。
In this paper, ZrO(OH)_2 was prepared with sol-gel method, then a series of metal-ions-doped SO 2-_4/ZrO_2 nanosolid superacids were prepared by impregnated ZrO(OH)_2 using diluted H_2SO_4 and Ni 2+, Al 3+, Sn 4+, Ag+, Sn 2+ etc. salt solutions. The samples were characterized by IR, XRD, TEM and chemical analysis method. The result shows that the IR spectra of samples are the characteristic spectra of the solid superacids. The stretching frequencies of Zr—O and SO in Ni 2+ and Sn 4+ doped samples are obviously increased, the ν_ Zr—O values of Zr—O increase from 485 cm -1 for SO 2-_4/ZrO_2 to 500 cm -1 for both Ni 2+ and Sn 4+ doped samples, the ν_ as values of SO increase from 1 390 cm -1 for SO 2-_4/ZrO_2 to 1 405 and 1 400 cm -1 for Ni 2+ and Sn 4+ doped samples respectively, but that in Sn 2+ doped sample increases a little. It is indicated that the samples doped by Ni 2+ and Sn 4+ show higher super acidity than SO 2-_4/ZrO_2. The IR spectra of samples were determined at different calcination temperatures. It was found that the stretching frequencies of Zr—O and SO in Ni 2+ and Al 3+ doped samples are obviously increased with the increase in calcination temperature, but that in Ag+ doped sample is not.
出处
《光谱学与光谱分析》
SCIE
EI
CAS
CSCD
北大核心
2005年第3期356-359,共4页
Spectroscopy and Spectral Analysis
基金
扬州大学科学基金 (D0 0 1 1 1 0 9)资助项目
