Issues of industrial waste recycling are very relevant for the entire global scientific community. The search for technological solutions that would allow the production of high-quality materials using industrial waste will not only reduce the environmental load, but also expand the raw material base for the production of gypsum materials. The study examined the possibility of improving the surface quality of molded gypsum samples by replacing the metal mold with a plastic one and introducing a surfactant into the raw mixture. As a result of the research, it was found that the use of a surfactant and a plastic mold allows to avoid defects on the surface of the samples. At the same time, the use of a plastic mold, which has low adhesion to the citrogypsum-based binder, helps to reduce the amount of adhesion friction and optimize the raw mixture compaction process. This makes it possible to obtain samples with improved physical and mechanical characteristics (compressive strength increases by 30–85.5%, average density - by 1.7–2.7% and water absorption decreased by 1.7–16%) or lower consumption of binder up to 20% compared to samples prepared in metal mold.