Effect of preparative conditions on the surface characteristics of mixed zirconium and titanium oxides

Abstract

The surface characteristics of mixed zirconium and titanium oxides prepared from different starting materials are investigated. One mode of preparation entailed the use of zirconium sulfate and titanium oxysulfate as starting materials and ammonium hydroxide as precipitating agent. The produced oxides were washed to different extents to obtain samples with different sulfate content. A second preparative mode used zirconium oxychloride and titanous chloride as starting materials also with ammonium hydroxide as precipitating agent. The oxidation of the titanous to the titanic form for these oxides was carried out by means of oxygen gas. Resulting samples were heat treated at 400°C and 600°C, and textural characteristics determined from the adsorption of N 2 at 77 K, complemented by infrared and thermal studies.The samples precipitated from the oxychloride and chloride salts of zirconium and titanium, as well as those precipitated from the sulfate and oxysulfate salts and washed free of the sulfate ions displayed quite similar textural characteristics. The unheated samples and those heat-treated at 400°C were mesoporous, with some microporosity, and relatively large surface areas in the order of 200-300 m 2 /g. Heat treatment to 600°C led to a relative decrease in surface area, in the order of 100 m 2 /g, and to the disappearance of microporosity.The mixed zirconium and titanium oxides with a sulfate content of ≈17% displayed significantly lower surface areas, smaller than 10 m 2 /g, with a prevalence of micro and mesoporosity. Infrared and thermal studies indicated the presence of differently bounded sulfato groups, which seem to have a blocking effect on the pores, resulting in the observed smaller surface areas.

Materials Based on Titanium and Manganese Oxides for Selective Recovery of Lithium From Water Sources

“…The sorption capacity of the material correlates with the size of the hydrated cation, the rate of sorption is determined by the diffusion of cation to the OHgroup, not the ion exchange. However, in some samples during the calcination, increasing mesoporosity increases the availability of OH-groups for exchange, so the dependence of the sorption rate on the diffusion of hydrated ion is negligible, as in the case of non-porous gels [21].…”