It was previously found that the silica-supported rhodium catalyst prepared using water-in-oil microemulsion had rhodium particles partly, or wholly, embedded in silica. In this work, consequently, we investigated the effect of hydrolysis conditions of tetraethylorthosilicate, employed as the source of silica, on the atomic ratio of surface rhodium in contact with the gas phase, to total surface rhodium of nanoparticles. This ratio is denoted as R in this paper. R became higher when the catalyst was prepared under the following hydrolysis conditions: a shorter hydrolysis time and a smaller amount of tetraethylorthosilicate. On the other hand, R showed the minimum value when the water content in the preparation solution was 33 vol%. From these results, it is demonstrated that it was important to form silica as early as possible in hydrolysis of TEOS in order to increase R values. In addition, the effect of R on the catalytic behavior in CO hydrogenation was investigated. At R values below 30%, the turnover frequencies increased with a decrease in R.
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