The article deals with the creation of lightweight syntactic polymeric materials of new generation with the improved complex operational and special properties. The preparation of composition and technology polymeric syntactic foam based on cyanat resin having the higher operational and special properties, compared by analog material, was shown. The production of such material has the different steps: the synthesis of cyanat resin with request rheological properties; blending the cyanat resin with glass microsphere for prepare the material with request homogenous properties; the prepare of roll syntactic polymeric materials having the thickness 2 mm. For preparing the material with request thickness we used the calendric technology; cutting the roll spheroplastic material on sample workpeace; the molding of spheroplastic. The application spheroplastic can significantly increase both absolute and specific characteristics of multilayer structures compared to design with cell. Also, the preparation of polymeric phenolic foam, based on phenolic resin, modified by rubber, having close-cell structure and higher operational properties, was shown. For foaming process the foam obtained semifinished product are not prefabricated as individual pellets or crushed powder as generally accepted in the preparation of foams brand FC, and rolled in the form of solid sheets, the total mass chosen with a given density of the obtained foam. The resulting foam originally monolithic semi eliminated the possibility of forming foam at foaming various small areas between individual pellets (or powder particles). Thereby, it reduces the overall porosity in the resulting foam. It was found that resole resins (containing novolac oligomer) poor fit together with a nitrile rubber. In addition, a combination of product of nitrile rubber with phenol resoles SF-3021K and with a novolac resin in all investigated ratios doesn’t allow to obtain high quality foam structure having a density less than 150 kg / m3. Only by combining a mixture of nitrile rubber and oligomeric compositions (resole (SF-342A) with novolak (SF-010), it is possible to obtain foams with a density from 80 to 150 kg / m3. For citation:Chursova L.V., Sokolov I.I., Lukina A.I. Study of polymer syntactic and foam materials of new generation with improving operational characteristics. Izv. Vyssh. Uchebn. Zaved. Khim. Khim. Tekhnol. 2017. V. 60. N2. P. 67-73.