含双杂原子(Ti,V)新型中孔分子筛的合成与表征

SYNTHESIS AND CHARACTERIZATION OF A NOVEL BIHETEROATOM(Ti AND V)CONTAINING MESOPOROUS MOLECULAR SIEVE

合成出一种含双杂原子（Ｔｉ，Ｖ）的新型中孔（Ｍｅｓｏｐｏｒｏｕｓ）分子筛材料，ＸＲＤ谱图与文献报道的Ｍ４１ｓ族中孔分子筛材料不同，表明可能是一种新分子筛物相。骨架红外、顺磁共振、紫外漫反射、固体魔角核磁２９Ｓｉ谱、激光拉曼光谱、电子能谱等测试结果表明，Ｖ在分子筛中主要以分散的不流动的Ｖ离子形式四配位存在于骨架上，Ｔｉ处在骨架位的配位数４～６之间，在苯酚羟基化催化反应中显示出一定的选择性的催化氧化活性。考察了分子筛的合成条件、吸附性能及热稳定性。

A novel biheteroatom(Ti and V)containing mesoporous molecular sieve has been synthesized.Its XRD pattern is different from that of M41s materials,which indicates that it would be a novel mesoporous molecular sieve structure.The intensity of 960 cm-1 bands in IR spectra of the samples increased with increasing of the vanadium or titanium contents respectively.The ESR spectrum shows that V exists in 4+ oxidation state,is monoatomically dispersed,and not mobile.Ti atoms isolate in the framework,and their coordination number are 4 or 6 from the results of diffuse reflectance spectra in the UVVIS region.Raman spectra show the absence of extraframework Ti and V;29Si MAS NMR spectra and XPS techniques provide additional evidences for the incorporation of Ti and V in mesoporous framework.Selective oxidation results of phenol hydroxylation in the samples were reported.The adsorption capacity and thermal stability of the sample have also been elucidated.