The microchannel liquid-flow focusing and cryo-polymerization is an efficient method for the preparation of cryogel beads with a narrow diameter distribution. In order to prepare cryogel beads with expected diameters, it is necessary to get insights in the liquid-liquid immiscible flow characteristics of the flow-focusing fluid and the monomer solution in microchannels. In this work, the slug flow behaviors of two immiscible liquids regarding the preparation of poly(2-hydroxyethylmethacrylate) (pHEMA) cryogel beads in a rectangular cross-junction microchannel were investigated experimentally by the high-speed imaging method. Correlations of the immiscible liquid-liquid slug flow parameters like the aqueous slug velocity and length, the aqueous slug nose and tail lengths, the water-immiscible slug length as well as the aqueous droplet size were obtained. The pHEMA cryogel beads were prepared under certain flow conditions and the bead sizes were measured by laser particle size analyzer. The obtained correlations were then employed to estimate the bead sizes and compared with those obtained experimentally. The results showed that the present correlations gave reasonable estimations of the mean bead diameters at various conditions and thus, could be useful and helpful in the preparation of cryogel beads with expected size distributions in rectangular microchannels. (C) 2014 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.