Preparation of TiO2 Hollow-Fibers Using Supramolecular Assemblies
Source abstract
Abstract
trans-(1R,2R)-1,2-Cyclohexanedi(11-aminocarbonylundecylpyridinium) hexafluorophosphate (1) was synthesized. The sol−gel polymerization of Ti[OCH(CH3)2]4 using compound 1 as a self-assembled template afforded fibrous TiO2 materials with a “macaroni”-like structure. The unique structure of TiO2 could be created by the formation of a fibrous self-assembled aggregate and electrostatic interaction between anionic titania species and cationic 1 under basic conditions.
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Research context
OpenAlex topics: Mesoporous Materials and Catalysis · TiO2 Photocatalysis and Solar Cells · Polyoxometalates: Synthesis and Applications
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
Affiliations
Department of Functional Polymer Science, Faculty of Textile Science and Technology, Shinshu University, Ueda, Nagano 386-8567, Japan
Chemotransfiguration Project, Japan Science and Technology Corporation (JST), 2432 Aikawa, Kurume, Fukuoka 839-0861, Japan
References (26)
Show source-provided references
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25. trans-(1R,2R)-1,2-Cyclohexanedi(11-aminocarbonylundecylbromide). 12-Bromododecanoyl chloride (10.7 g, 3.60 mmol) was dissolved in 30 mL of tetrahydrofuran (THF). A mixture of 8.0 mL (57.4 mmol) of triethylamine and 2.05 g (1.80 mmol) oftrans-(1R,2R)-1,2-diaminocyclohexane in 50 mL of THF was added dropwise to the above solution and stirred overnight at 60 °C. After evaporation, the crude product was dissolved in 200 mL of hot ethanol and cooled to room temperature. The formed gel was filtered with suction and dried. This purification procedure with ethanol was repeated. Yield: 7.4 g (65%).trans-(1R,2R)-1,2-Cyclohexanedi(11-aminocarbonylundecylpyridinium)bromide.trans-(1R,2R)-1,2-Cyclohexanedi(11-aminocarbonylundecyl bromide) (0.50 g, 0.785 mmol) was dissolved in 30 mL of pyridine and refluxed for 12 h. After evaporation, the residue was dissolved in a minimum volume of ethanol. Acetone was added dropwise to the ethanol solution with stirring until white precipitation was generated. The solution was cooled at 0 °C, and then the gellike matter was filtered with suction and dried. Yield: 0.65 g (90%).trans-(1R,2R)-1,2-Cyclohexanedi(11-aminocarbonylundecylpyridinium)hexafluorophosphate (1).To a solution of 0.50 g (0.63 mmol) oftrans-(1R,2R)-1,2-cyclohexanedi(11-aminocarbonylundecylpyridinium) bromide in 50 mL of distilled water was added 0.46 g (2.5 mmol) of potassium hexafluorophosphate in 50 mL of distilled water, followed by stirring for 3 h. The precipitated matter was filtered off, washed with water, and dried in a vacuum. Yield: 0.55 g (92%).1H NMR (400.1 MHz, CD3CN): δ 1.26−1.67 (m, 36 H, CH2), 1.93 (t, 4 H, COCH2), 1.94−2.05 (m, 8 H, cyclohexane), 3.49 (d, 2 H, cyclohexane), 4.50 (t, 4 H, CH2), 6.53 (s, 2 H, NH), 8.03 (t, 4 H, pyridine), 8.50 (t, 2H, pyridine), and 8.66 (d, 4H, pyridine).13C NMR (100.6 MHz, CD3CN): δ 24.17, 25.23, 28.26, 28.59, 28.66, 28.77, 28.83, 30.54, 31.57, 35.81, 53.05, 61.52, 128.08, 144.07, 145.39, and 172.78. FT-IR (KBr): 3282 (ν NH) and 1637 cm-1(ν CO). Element analysis calculated for C40H66N4O2P2F16: C 51.9, H 7.2, N 6.1; found: C 52.2, H 7.4, N 6.1.
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