Liquid-phase cyclohexanone ammoximation over titanium silicate was carried out in a batch reactor. The influence of the solvent, duration of kinetic run, catalyst amount and reactant concentrations was investigated. Byproducts were formed in considerable amounts, leading to catalyst deactivation by pore blocking. The values of initial reaction rates were calculated taking into account deactivation phenomenon. These values indicated that within the range of studied concentrations (C-cyclohexanone = 0.4 to 1.70 mol/l; C-ammonia = 1 to 4 mol/l; C-hydrogen peroxide = 0.4 to 1.8 mol/l) the reaction rates plotted as a function of all the reagent concentrations go through a maximum. Special experiments on hydrogen peroxide decomposition and cyclohexanone oximation by hydroxylamine demonstrated that the rates of these reactions are essentially higher than the ammoximation rates.