| Summary: | The demand for 1,3-butadiene, one of the most important raw materials in the rubber industry, is constantly increasing. The Lebedev process is a classical method of producing 1,3-butadiene from ethanol, which is to be optimized with regard to the mixed oxide catalysts used. In this work, the binary MgO/SiO<sub>2</sub> solid system was tested with regard to its optimum chemical composition for the catalytic conversion of ethanol to 1,3-butadiene. Furthermore, novel mesoporous mixed oxides were prepared to investigate their textural, structural, and surface chemical properties as well as the catalytic activity. Nitrogen physisorption, scanning electron microscopy (SEM), and temperature-programmed ammonia desorption (NH<sub>3</sub>-TPD) measurements were carried out and evaluated. It was shown that the optimum yield of 1,3-butadiene is achieved by using MgO/SiO<sub>2</sub> mixed oxide catalysts with 85–95 mol% MgO and not, as suggested by Lebedev, with 75 mol% MgO. The NH<sub>3</sub>-TPD measurements revealed that the maximum acid-site density is achieved with an equimolar up to magnesium-rich composition. During the synthesis of binary MgO/SiO<sub>2</sub> solid systems based on mesoporous MgO, a thermally stable and ordered structure was formed in the autoclave, depending on the carbonate used and on the duration of the treatment.
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