The basic technological parameters of the preparation of nickel-filled hydrogel materials based on copolymers of polyvinylpyrrolidone with 2-hydroxyethyl methacrylate by the method of polymerization with simultaneous recovery of metal ions were considered. It was established by volumetric method that the process of chemical reduction of nickel ions at pH 7.5-8 is characterized by a high rate and a small induction period at a temperature of 60-70 0 C. The presence of polyvinylpyrrolidone was found to reduce the duration of the induction period and increase the rate of the reduction reaction. The duration of the induction period is 14 minutes when the content of polyvinylpyrrolidone in solution is 200 g/L. The kinetics of heat release during copolymerization of 2-hydroxyethyl methacrylate with polyvinylpyrrolidone initiated by benzoyl peroxide was investigated by a thermometric method. It was established that the exothermic effect of the polymerization can be used to ensure the required temperature conditions for Ni 2+ reduction. The versatile effect of the composition of the original polymer-monomer composition on the basic parameters of the exothermic process of copolymerization has been experimentally shown. The diversified effect of the composition of the initial polymer-monomer composition on the parameters of the exothermicity of the copolymerization was experimentally determined. The simplexlattice planning method was used to optimize the formula of polymer-monomer composition. The obtained regression equations allow establishing analytical dependences of the parameters of exothermic processes on the technological conditions of the reduction of Ni 2+ ions and the formula of the polymer-monomer composition.