Samples of tungsten-modified borated zirconia were prepared to be used as catalyst in 2-phenoxyethanol acetylation. The borated zirconias were obtained by impregnation of two zirconias (S2 and S4) obtained by the micellar method using different zirconium precursor concentrations with boric acid solution containing 0.3 moles B/dm³. These solids and the parent zirconias were impregnated with two concentration levels of ammonium metatungstate solutions (0.11 and 0.22 moles W/dm³). The solids containing boron mainly have amorphous characteristics and strong acidity, while those that contain only tungsten showed stronger acidity and evidence of the presence of a crystalline phase.

The specific surface area and the pore volume slightly decreased in the solids obtained by adding tungsten to borated zirconia, and more markedly in those that contain only tungsten, and the mean pore size increased with respect to the parent support. It was observed that in the 2-phenoxyethanol acetylation using acetic acid as acylating agent and tungsten-modified borated zirconia as catalyst, the yield to acetylated product was high and it is correlated with the acid strength of the catalysts. In turn, the solids that contain only tungsten have a correlation with the acidity, but lead to low yield values due to a poorer dispersion of the tungsten species. The best yield was obtained with the catalyst prepared with the borated S4 zirconia containing 15% g B₂O₃/100 g support and 12.5% g W/100 g support. Using this catalyst and the same reaction conditions, the acetylation of different alcohols and phenols was studied, the reactivity order being as follows: primary alcohols > secondary alcohols > phenols.


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A particular advantage of the invention is that the silica used in digestion and subsequently filtered from the digested solution of ammonium metatungstate may be reused repeatedly, that is, its capacity to promote formation of AMT is not diminished with use. While the exact mechanism is not well understood at this time, the role of silica is to prevent the precipitation of insoluble APT and therefore to allow lowering of the pH to the AMT forming region, about 4 to 4.5.

After digestion is completed, the silica is removed, such as by filtering, and the solid AMT may be recovered in the conventional manner, such as by evaporation or spray drying.

The silica used in the invention may be any commercially available silica, provided that its impurities, both in kind and amount, are consistent with the final envisioned application for the AMT. For example, both sodium and phosphorus may be considered objectionable impurities for certain catalyst applications. Residual silica which cannot be removed from the digested AMT solution by filtering is generally below 1 percent by weight, and typically from 0.3 to 0.6 weight percent WO₃basis, and is compatible with many catalyst applications.


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At present both ammonium paratungstate (APT) and AMT are being used as tungsten sources in the catalyst industry. Since APT has a limited solubility in water (about 2 to 3 percent at room temperature), the user converts APT to a more soluble peroxytungstate form by means of reaction with hydrogen peroxide in order to prepare the catalyst. While AMT is highly water soluble, and thus need not be converted, it is in general more expensive than APT, due to the complexity and/or low yields of processes for producing it.

A process for producing ammonium metatungstate (AMT) from ammonium tungstate (AT) solution is described which involves the addition of about 3.6 percent by weight of silica to an AT solution, digestion for at least about 4 hours at a temperature of at least about 98°C, followed by filtration to remove the silica from the AMT solution. Typically about 0.4 percent by weight of silica remains after filtering. The resulting AMT solution may be further processed to recover solid AMT, such as by evaporation or spray drying.


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The purpose of this study is to establish the way in which different synthesis conditions influence on the structural and luminescent characteristics of europium activated calcium tungstate powder phosphor. CaWO₄:Eu³⁺ samples were prepared by thermal synthesis from mixtures consisting of precipitated-CaWO₄, equivalent amounts of Eu₂O₃ and WO₃ (activating system) and CaCl₂ or Na₂WO₄ as flux. Calcination was performed at 800 - 1000 degree(s)C for 2 h, in air. The crystalline structure (XRD-patterns) and luminescent characteristics (emission and excitation spectra of phosphor samples were determined and interpreted.


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