2004 Fiscal Year Final Research Report Summary
Study of Environmentally Benign Synthesis of Mesoporous Silicas with New Fluorous Surfactant
| Project/Area Number |
15590015
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| Research Category |
Grant-in-Aid for Scientific Research (C)
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| Allocation Type | Single-year Grants |
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| Section | 一般 |
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| Research Field |
Chemical pharmacy
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| Research Institution | Gifu Pharmaceutical University |
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Principal Investigator |
ITOH Akichika Gifu Pharmaceutical University, Associate Professor, 薬学部, 講師 (10203126)
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| Project Period (FY) |
2003 – 2004
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| Keywords | Environmentally Benign / Mesoporous Silicas / Silicas / Fluorous / Surfactant |
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| Research Abstract |
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.
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