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Paint applied as a single layer, and its spontaneous separation to form a primer and a top coat, is one of the newest concepts of the effective and economical application of two layers in one step. The influence of the molecular weight of epoxy oligomer and acrylic polymer and their ratio on self-stratification was investigated. The degree of stratification depending on molecular weight and their mutual ratio was determined using ATR-FTIR spectroscopy, differential scanning calorimetry, microscopy techniques, adhesion tests, and surface tension measurements. Phase separation and self-stratification of two-component homogenous mixtures were followed using FTIR technique and surface tension measurements. As a result of these investigations, optimal oligomeric/polymeric composition was selected. The obtained coating system showed good mechanical properties, gloss, and interlayer adhesion.