Homogeneous Pt-catalyzed hydrosilylation is an industrially important process for the synthesis of organosilanes. Reusable heterophase (biphase) Pt-catalysts can solve economic and ecological issues arising from the high cost of Pt and its irretrievable “scattering”. Previously, we proposed a sustainable and convenient-to-handle heterophase Pt/EG-catalytic system (EG – ethylene glycol). In the current research heterophase Pt/EG-catalyzed hydrosilylation was transferred in a microfluidic regime that combined several advantages. A stable droplet or segmented Taylor flow with a well-defined contact area allow for the improvement of mass and heat transfer during the scaling of such a biphase and exothermic reaction, compared to batch mode. In situ Raman spectroscopy monitoring allows for fast and continuous data collection throughout the experiment and opens an opportunity for automation of conversion analysis. We demonstrate an efficient reaction of a range of reagents in the microfluidic reactor. In this work its universal components were constructed and modified using either commercially available units or via additive technologies (3D-printing). To the best of our knowledge, this is the first example of a semi-automatic recyclization device for a real heterophase catalytic process. These results open up new perspectives for scaling and automating industrially relevant heterophase hydrosilylation reactions.