Mesoporous mesophase materials (MMM) with well-expressed porous hexagonal structures and dimension range 2-10 nm are used as inorganic sorbents, catalysts and catalyst carriers. Therefore, the production of mesoporous synthetic materials with controllable pore dimensions, large surface area is of current importance. One of the most effective methods for the production of nano-scale materials as a basis of metal oxide catalysts is the chemical liquid-phase condensation due to various conditions. Literary sources on the matter are inconsistent, therefore the optimization of technological procedures for the production of mesoporous silica appeared necessary. In this paper the influence of synthesis conditions, of the ratio between reaction components CTAB/TEOS, NaOH/TEOS, water/TEOS, of the use of organic additives such as 2-cyanoethyltriethoxysilane, 2-aminopropyltriethoxysilane and for the first time tris-trimethylsiloxysilane on textural and structural characteristics of the finished material during production of mesoporous silica has been studied. The structural characteristics have been investigated by BET measurement, Raman spectroscopy, Fourier-transform infrared spectroscopy and X-ray diffraction techniques. Optimization of technological procedures allows to produce the material with high specific surface (1400 m2/g), total pore volume over 1 cm3/g and average pore diameter approximately 4 nm.