Results of the studies on the use of hydrolytic lignin as a raw material for the production of carbon adsorbents are given. A thermochemical method using sodium hydroxide as an activating agent was chosen as a method of activation of hydrolytic lignin. The experiment was aimed at finding out the influence of operating conditions on the yield and properties of the active carbon obtained. Synthesis of adsorbents was carried out using a uniform second order rotatable central composite design for three variables at five levels. Temperatures of prepyrolysis and pyrolysis, and a dosage of the activating agent represented changing parameters. For samples of active carbon obtained, the adsorption activity was investigated with respect to three adsorbates: methylene blue (MB), iodine, and hexane. Based on the output parameters, the coefficients of equations of regression were calculated and the assessment of their significance was carried out. The conclusion on the degree of the effect of factors and curvature of space studied could be made using absolute values and signs of the coefficients. The effect of operating parameters on the yield and sorption activity of the coal obtained was studied by constructing graphic dependencies and response surfaces. As a result of the analysis of the data obtained, a conclusion was made on the effectiveness of the method used for the synthesis of adsorbents, since the active carbon obtained had a developed porous structure.