The suitability of mixed solubilization compositions for template synthesis of mesoporous molecular sieves of various designations was demonstrated by analysis of published data and by the authors' experimental results.Scientific approach and experimental methods in physical and colloid chemistry of surfactants are developed and improved mostly for individual substances, idealized models, and simple systems. In practice, it is more expedient, however, to use surfactant-based compositions, as, e.g., in production of detergents, flotation reagents, defoliants, emulsifiers, pharmaceuticals, and cosmetics [137].The use of individual micelle-forming surfactants in template synthesis of mesoporous sorbents has been studied since 1992 [8,9]. Beck et al. [8] and Huo et al.[9] suggested a number of basic schemes of interaction between a skeleton-forming inorganic reagent (I) and a micelle-forming surfactant (S), template. These authors assumed that the assembly (selfassembly) is controlled by electrostatic interaction of the ions in solution, namely, between charged polar groups of the surfactant and inorganic counterions. This interaction is the most efficient in the case of long-chain surfactants based on quaternary ammonium cations (S + ) and anionic silicate precursors (I 3 ), yielding hexagonal, cubic, of lamellar mesostructures. More recently, this concept was extended to include the views on the synthesis routes involving inversely charged reagents (S 3 I + ), anionic surfactants such as sulfonates and phosphonates, as well as carboxylates and cations of inorganic precursors, buffer ions (S + X 3 I + , S 3 M + I 3 , where X is halogen, and M + , alkali metal cation).Irrespective of the scheme chosen, mesoporous sorbents are synthesized using insoluble/poorly soluble organic substances as auxiliary forming reagents. For example, Beck et al. [8] used trimethylbenzene (TMB) exerting a swelling (expanding) effect when added to a freshly synthesized template-containing mesophase: The diameter of the mesoporous molecular sieves (MMSs) increased from 4.0 to 6.5 nm. There is a good reason to assume that TMB is incorporated into the oil core of the micelle of the cationic surfactant.Nonpolar aliphatic and aromatic hydrocarbons, for the most part, efficiently promote structure formation when introduced into freshly synthesized materials. Hydrocarbons with linear and branched radicals (C 5 3 C 12 ) yield an M41S phase mixture and/or cause the pore size to increase. At the same time, polar organic substances, in particular, alcohols, aldehydes, ketones, ethers, and esters, generally did not efficiently increase the pore size of the MCM-41 mesophase and, moreover, often yielded amorphous materials [10].Kleitz et al. [11] prepared heat-resistant mesoporous oxides of transition metals (Ti and Zr) using binary organic additives, namely, 1-octanol as cosurfactant and toluene or TMB as swelling reagent. Both additives were introduced simultaneously with all the components (cetyltrimethylammonium bromide, CTMABr, acted as the basic t...