Preparation method of fluorinated ZIF-90 modified PDMS film
A ZIF-90, fluorination technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of limited research, few types, difficult preparation of fluorinated organometallic framework materials, etc. The effect of enhanced compatibility and good separation performance
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Embodiment 1
[0030] 1) Synthesis of imidazole fluoride: Dissolve 2-formylimidazole (2.5g, 26mmol) and 2,3,4,5,6-pentafluoroaniline (4.8g, 26mmol) in 40mL of absolute ethanol, add titanium Acetate tetraisopropyl ester (7.38g, 26.0mmol), then reacted at 65°C, TLC tracking showed that the reaction raw materials disappeared, the solvent was removed by rotary evaporation, and ethyl acetate was used as the eluent to dissolve the product. Then separated by column chromatography to obtain 4.1 g of flocculent white solid. NMR characterization results such as figure 1 shown. 1 H NMR(400MHz,DMSO)δ13.44(s,1H),8.59(s,1H), 7.40(s,2H). 19 F NMR (376MHz, DMSO) δ-153.84(m, 2F), -161.68(t, J=22.8Hz, 1F), -163.67(m, 2F).
[0031] 2) Synthesis of fluorinated ZIF-90: Zinc nitrate hexahydrate (740 mg, 2.5 mmol), imidazole fluoride (2.62 g, 10 mmol) and sodium formate (680 mg, 10 mmol) were dissolved in 400 mL of methanol by sonication. Then the reaction solution was put into a polytetrafluoroethylene-lined ...
Embodiment 2
[0034] 1) Synthesis of imidazole fluoride: Dissolve 2-formylimidazole (2.5g, 26mmol) and 2,3,4,5,6-pentafluoroaniline (5.7g, 31mmol) in 40mL of absolute ethanol, add titanium Acetate tetraisopropyl ester (8.86g, 31mmol) was then reacted at 80°C. TLC tracking showed that the reaction raw materials disappeared, the reaction solution was cooled and filtered, and the resulting solid was recrystallized from ethanol to obtain 3.6g of a white solid. The nuclear magnetic data is identical with embodiment 1.
[0035] 2) Synthesis of fluorinated ZIF-90: Anhydrous zinc chloride (340 mg, 2.5 mmol), imidazole fluoride (2.62 g, 10 mmol) and sodium formate (680 mg, 10 mmol) were dissolved in 400 mL of methanol by sonication. Then the reaction solution was put into a polytetrafluoroethylene-lined stainless steel reactor and heated at 85 °C for 24 h. The reaction solution was cooled and filtered to obtain a light yellow powder, which was washed three times with anhydrous methanol, and then va...
Embodiment 3
[0038] 1) Synthesis of imidazole fluoride: Dissolve 2-formylimidazole (2.5g, 26mmol) and 2,3,4,5,6-pentafluoroaniline (5.7g, 31mmol) in 40mL of absolute ethanol, add titanium Acetate tetraisopropyl ester (8.86g, 31mmol) was then reacted at 80°C. TLC tracking showed that the reaction raw materials disappeared, the reaction solution was cooled and filtered, and the resulting solid was recrystallized from ethanol to obtain 3.6g of a white solid. The nuclear magnetic data is identical with embodiment 1.
[0039] 2) Synthesis of fluorinated ZIF-90: Zinc nitrate hexahydrate (740 mg, 2.5 mmol), imidazole fluoride (1.31 g, 5 mmol) and sodium formate (680 mg, 10 mmol) were dissolved in 400 mL of methanol by sonication. Then the reaction solution was put into a polytetrafluoroethylene-lined stainless steel reactor and heated at 85 °C for 24 h. The reaction solution was cooled and filtered to obtain a light yellow powder, which was washed three times with anhydrous methanol, and then va...
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