This article describes the physico-chemical characterization of the sulfated zirconia catalysts prepared from zirconyl chloride, acetic acid and ammonium persulfate system under structure-directing-free and calcined a...This article describes the physico-chemical characterization of the sulfated zirconia catalysts prepared from zirconyl chloride, acetic acid and ammonium persulfate system under structure-directing-free and calcined at 650°C. The catalysts were characterized via an array of characterization techniques such as surface acidity and texture measurements, X-ray diffraction (XRD), ultraviolet-visible spectroscopy (UV-VIS), scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectroscopy (EDXS), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), infrared spectroscopy (IR), thermogravimetric measurement (TG) coupled with a quadrupole mass spectrometer (MS), inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and/or mass spectrometry (ICP-MS). It is clear from TG-MS, ICP-AES, and IR analyses that the precursor of the catalyst is a sulphur species-doped zirconium oxy-hydroxyl acetate complex. The presence of zirconium-bound sulfate groups results in the superacidity of the catalyst and hence high activity in n-hexane isomerization. It is shown from nitrogen adsorption and desorption, FESEM, and HRTEM measurements that the materials exhibit mesoporous and nanocrystalline structure.展开更多
文摘This article describes the physico-chemical characterization of the sulfated zirconia catalysts prepared from zirconyl chloride, acetic acid and ammonium persulfate system under structure-directing-free and calcined at 650°C. The catalysts were characterized via an array of characterization techniques such as surface acidity and texture measurements, X-ray diffraction (XRD), ultraviolet-visible spectroscopy (UV-VIS), scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectroscopy (EDXS), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), infrared spectroscopy (IR), thermogravimetric measurement (TG) coupled with a quadrupole mass spectrometer (MS), inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and/or mass spectrometry (ICP-MS). It is clear from TG-MS, ICP-AES, and IR analyses that the precursor of the catalyst is a sulphur species-doped zirconium oxy-hydroxyl acetate complex. The presence of zirconium-bound sulfate groups results in the superacidity of the catalyst and hence high activity in n-hexane isomerization. It is shown from nitrogen adsorption and desorption, FESEM, and HRTEM measurements that the materials exhibit mesoporous and nanocrystalline structure.
