摘要
采用XRD及其Rietveld全谱拟合、低温N2吸附-脱附、XPS、TEM(包括EFTEM和HRTEM)、UV-Vis等手段对失活HTS分子筛的晶胞参数、骨架结构、颗粒形貌和Ti物种的位置与状态进行分析。结果表明,HTS分子筛失活后,其拓扑结构保存完整,且晶胞参数未发生明显变化,但部分微孔结构发生溶解,介孔体积增大,比表面积略有下降。HTS分子筛失活后,部分骨架Ti物种转变为非骨架Ti物种,富集且高度分散于分子筛颗粒形成小碎片,可以初步判定该碎片为高度分散的无定型TiO2或TiO2-SiO2氧化物。
Multiple characterization methods, including XRD and its Rietveld whole pattern fitting, low-temperature N2 adsorption-desorption, XPS, TEM ( EFTEM, HRTEM ) and UV-Vis spectroscopy, were introduced to investigate the characteristics, such as framework structure, crystal parameters, the morphology and chemical state of Ti species, of deactivated HTS zeolite from industrial cyclohexanone ammoxidation processing. The results showed that the MFI topological structure and crystal volume of deactivated HTS zeolite remained almost the same as that of fresh one, while some micropores of zeolite transformed into mesopores, resulting in the increase of mesopore volume and the decrease of specific surface area. At the same time the framework Ti transformed into non-framework Ti, forming highly scattered Ti aggregates on zeolite particle, which were considered as amorphous TiO2 or TiO2-SiO2 oxides.
出处
《石油学报(石油加工)》
EI
CAS
CSCD
北大核心
2014年第4期595-601,共7页
Acta Petrolei Sinica(Petroleum Processing Section)
基金
国家重点基础研究发展计划"973"项目(2006CB202500.7-22)资助