Alkene metathesis attracted recently much attention, especially with the 2005 Nobel prize awarded for the development of the metathesis method in organic synthesis. Supported molybdenum oxide catalysts are widely used in industrial petrochemical processes, including metathesis (e.g. Phillips triolefin process, Shell higher olefin process). The present work discloses new type of metathesis catalysts based on molybdenum oxide supported on mesoporous silica. The key idea is to improve the activity of molybdenum oxide catalyst in this reaction utilizing high surface area and narrow pore size distribution of the support material. For the preparation of the catalysts, innovative and environmentally friendly thermal spreading method was employed. The thorough characterization of the catalysts by physicochemical techniques is described. The analysis of activity/selectivity vs. composition/structure relationships should help shed some light on this new and exciting field of heterogeneous catalysis, and should be especially useful to professionals in metathesis chemistry, or anyone else who may be considering utilizing molybdenum oxide catalysts for another catalytic reaction.