Studies on functionalized mesoporous materials—Part I: characterization of silylized mesoporous material of type MCM-41

The synthesis of organic–inorganic composite materials was performed by the surface modification of mesoporous material type MCM-41 by chlorodimethylphenylsilane and dichloromethylphenylsilane. Applying IR spectroscopy, low temperature nitrogen adsorption/desorption (isotherms BET), thermogravimetric measurements and technique of competitive adsorption of toluene and water it was shown that the degree of silylation, hydrophobicity, surface and volume properties (pore size distribution, pore volume) strongly depends on the nature of silylation agent and the ratio of calculated amount of silanol groups to the modifier. Two types of condensation reaction take place: (1) the reaction of the modifier with surface silanol groups, and (2) an inter-molecular condensation of the modifier, resulting in additional pore blocking. Only 24–36 % of the surface silanol groups react with modifier agent. The materials are stable up to temperatures of about 170 °C that is higher than the corresponding polymeric resins. The TG/DTA data allowed concluding that the degree of grafting depends on the ratio silylation agent to SiOH groups. As shown by Fourier transform diffuse reflectance mode spectroscopy only free silanol groups react with modifier.