The synthesis of a catalyst for a two-phase catalytic reaction, a millimeter-scale reactor experiment, and an analysis model for the prediction of reactor performance are presented in this paper. The catalyst nanoparticulate perovskite La0.8Sr0.2CoO3 was prepared by a modified sol-gel method, in which PAA (poly acrylic acid) was added to catalyst precursors. A millimeter-scale reactor experiment with the prepared catalyst was carried. Concentrated hydrogen peroxide was decomposed in the reactor and the characteristics of the reactor were measured in terms of temperature distributions and liquid production rates. The results indicated a flow regime transition, which caused the change of reactor performance. An analysis model for two-phase catalytic reaction based on the lumped flow reactor model and the diagnostic data obtained on the temperature distributions and liquid production rates is proposed. Temperature distributions and heat transfer characteristics of the reactor were predicted by a semi-empirical analysis. In this analysis, the model of the Nusselt number (Nu) was proposed as Nu = Nu(0)(1 + a(1)(a(2)(T) over tilde (-a3)) exp(a(4)(T) over tilde (-1)) exp(a(5)z)). This expression of the model reflects the effects of temperature and coordinate location on the heat transfer characteristics of the reactor. From the modeled reactor, characteristics such as the increase of heat transfer in the mid and rear parts of the reactor with the increase of reactant flow rate were obtained. with the obtained results, a tool for the design and analysis of a down-scaled catalytic reaction device was obtained. (C) 2009 Elsevier Ltd. All rights reserved.