|Budget Amount *help
¥3,000,000 (Direct Cost : ¥3,000,000)
Fiscal Year 2004 : ¥1,000,000 (Direct Cost : ¥1,000,000)
Fiscal Year 2003 : ¥2,000,000 (Direct Cost : ¥2,000,000)
1. Synthesis of Fluorous Surfactant
Fluorous surfactant 1, a quaternary ammonium salt, was synthesized from commercially available alcohol through two steps in high yield.
2. Synthesis of FSM
Preparation of a mesoporous silica with fluorous surfactant 1 as template, named FSM-R_f11, was tried according to the synthesis of FSM-16. At first we studied the effect of reaction time and temperature in the reaction of 1 (0.1 M) with wet kanemite on a synthesis of FSM-R_f11. The results of a study of reaction temperature showed that FSM-R_f11, which possessed enough pore size and narrow pore distribution, could be prepared at reaction temperature of 60℃ to 90℃ we examined. Furthermore, the pore size of FSM-R_f11 proved to be larger than that of FSM-12, which was prepared with a surfactant with a longer C_<12>-alkyl chain.
3. Recovery and Re-use of Fluorous Surfactant 1
We designed a method to recover 1, which was used for actual FSM-R_f11 synthesis, from the aqueous waste after filtration of the product by extraction with perfluoro solvents. At first, we carried out a preliminary study for selective extraction of 1 from the aqueous 1 solution with several perfluoro solvents, and 2,2,2-trifluoroethyl trifluoroacetate (TFETFA) was found to be a good solvent for this purpose among the solvents examined. In the actual synthesis of FSM-R_f11, 1.1 g of 1 was recovered from the aqueous waste with TFETFA when 3.3g of 1 was used as a template. Surfactant 1 was not recovered completely because 1 was thought to remain in the mesopores of silicates. The recovered 1 was collected, and subjected to preparation of FSM-R_f11 again; however, the results were less satisfactory as the pore distribution of FSM-R_f11 with recovered 1 was much wider than that of FSM-R_f11 with freshly synthesized 1.