Sulfate Grafted Iron Stabilized Zirconia Nanoparticles as Efficient Heterogenous Catalysts for Solvent-Free Synthesis of Xanthenediones under Microwave Irradiation

Abstract

Sulfate grafted iron stabilized zirconia nanoparticles (SO 4 2− /xFe−Zr−O) are prepared by a coprecipitation method followed by sulfate ion grafting. The SO 4 2− /xFe−Zr−O materials have been characterized using XRD, UV−vis, FTIR, Raman, SEM, and TEM techniques. XRD study indicated incorporation of iron ions (up to 20 mol %) into the zirconia lattice, resulting in the formation of a substitutional solid solution. The vibrational features corresponding to the SO and S−O stretching of anchored sulfate species are observed in the FTIR study. The Raman study indicated the presence of nanosize hematite and tetragonal zirconia phase in the composite oxide. The presence of iron oxide in the zirconia lattice improves the sulfate retention capacity of the host zirconia. The SO 4 2− /xFe−Zr−O materials are found to be efficient catalysts for the synthesis of structurally diverse xanthenediones by one-pot condensation of dimedone with aryl aldehydes under solvent-free conditions and microwave irradiation.

Cytotoxicity and physicochemical characterization of iron–manganese-doped sulfated zirconia nanoparticles

“…A total lack of impact on the shape of the Zr 3d peak is very significant and suggests the different strengths and surroundings of the interfaces between the SO 4 2-species and the ZrO 2 for (NH 4 ) 2 SO 4 hydrothermal impregnation at the amount of 4% SO 4 2-. 45,46 The S 2p photoelectron lines appeared at approximately 168.4 eV ( Figure 1C) and indicate the presence of sulfur ions (+6) in agreement with the relative amount to S 6+ in sulfates anions and in agreement with a previous research article which performed analysis regarding sulfate group-doped ZrO 2 catalysts. 46 Figure 1D shows the X-ray photoelectron spectrum of iron(3+)-manganese-doped sulfated ZrO 2 in the region of iron 2p.…”

Synthesis of waste cooking oil-based biodiesel via effectual recyclable bi-functional Fe2O3MnOSO42−/ZrO2 nanoparticle solid catalyst

“…The higher binding energy species (185.5 eV) matched to the development of the zirconium (+4) component attached to a non-metal. The entire lack of influences on the profile of the 3d-orbital of the zirconium emission line has been extremely remarkable and suggestive of the different strength and environment of the interactions involved between ZrO 2 and the SO 4 2À anion [33,34]. The S2p emission was located at about 168.6 eV (Fig.…”

Sulfated Zirconia Synthesized in a One Step Solvent-Free Method for Removal of Olefins from Aromatics

“…Recently, sulfated zirconia (SZ) has also shown excellent performance toward olefin removal in aromatics . Due to its properties of superior acidity, sulfated zirconia is widely used in alkylation, , isomerization, , acylation, , condensation, , and esterification reactions. , Zirconium oxide (ZrO 2 ) possesses both acid sites and base sites and can convert to solid acid by supporting SO 4 2– in the inductive effect promoting by SO bonds. , The traditional synthesis method to prepare sulfated zirconia is an impregnation–immersion one, which dips zirconium hydroxide into ammonia sulfate or sulfuric acid followed by calcination at 650 °C . The most common raw material resource of Zr is zirconium oxychloride (ZrOCl 2 ·8H 2 O), which can be transferred into zirconium hydroxide (Zr­(OH) 4 ) in mixing with ammonium hydroxide (NH 3 ·H 2 O), while raw Zr in nature is in the form of azurite which includes ZrSiO 3 instead of ZrOCl 2 ·8H 2 O.…”