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The FSM-16, MCM-41 and SBA-15 type hexagonal mesoporous silica materials having a highly arrange in order of the 2-dimensional structure were synthesized by using different silicon sources and surfactants. In the 2-dimensional silicate framework, pore size can be uniformly controlled by the combined use of the surfactants having different alkyl chains length and swelling agents (triisopropyl benzene). Pore-diameter of FSM-16 and MCM-41 can be expanded to 100 A, SBA-15 is 150 A. Crystal regularity decreased with increasing the pore-diameter in the FSM-16 derived from Kanemite (silicon source) and MCM-41 from water glass, its anionic char-acteristics on the pore wall may be higher than SBA-15 derived from oligomeric tetramethoxysilane (TMOS) is also reported. We have successfully used FSM-16 and MCM-41 as immobilizing agents of enzyme having cationic residues under isoelectric point. The level of adsorption of enzymes in the FSM-16 and MCM-41 was relatively high, but was low in the SBA-15 support. The mechanism of enzyme adsorption in mesopore was suggested to be the ionic interactions. In aqueous solutions, horseradish peroxidase (HRP) immobilized in FSM-16 containing 89A mesopore showed the highest loaded amounts(183mg/mg FSM),then a FSM-16 of pore-diameter 30 A only loaded a litter amounts (28mg/mg FSM) on the outside surface. The catalytic activity in organic solvent is high when HRP was immobilized in FSM-16 and MCM-41, but is low in case of SBA- 15.