Co (II) based metal organic framework as well as preparation method and application thereof
A metal-organic framework and organic ligand technology, applied in organic chemistry, cobalt-organic compounds, chemical instruments and methods, etc., can solve the problems of high cost, unrecyclable catalyst, and complicated operation.
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Embodiment 1
[0059] Embodiment 1: the preparation of organic ligand L
[0060] Concrete preparation steps are as follows:
[0061] (1) 4,4-dibromobenzil (10.00g, 27.17mmol), ammonium acetate (41.89g, 543.45mmol), paraformaldehyde (1.63g, 54.34mmol), join in 100mL glacial acetic acid solution, stir Heat to reflux for 5 hours, adjust to neutral with saturated sodium carbonate solution after the reaction, extract with 200mL ethyl acetate, wash with sodium carbonate solution, extract the aqueous phase with ethyl acetate, combine the organic phases, and wash with anhydrous magnesium sulfate Dry, filter, and remove the solvent under reduced pressure to obtain 10.07 g of a yellow solid with a yield of 98.00%.
[0062]
[0063] (2)N 2 Under protection, intermediate A (10.58mmol, 4.00g) and sodium hydride (11.64mmol, 0.28g) were placed in a 100ml three-necked flask, and 50ml of anhydrous THF was slowly added as a solvent, heated to 80°C, and stirred at a constant temperature of 80°C for 1h , ...
Embodiment 2
[0068] Embodiment 2: Synthesis of Co-MOF-1
[0069] The organic ligand L (4.06mg, 0.01mmol) prepared in Example 1, terephthalic acid (1.66mg, 0.01mmol), cobalt acetate (0.01mmol, 2.13mg), were dissolved in 2mL of methanol, placed in a 5ml small In the test tube, the temperature was kept at 120°C for 72 hours, and the temperature was lowered to room temperature after 50 hours of programming to obtain purple-red blocky crystals {Co 3 L(BDC) 2.5 (OAc)(MeOH)}, yield 3.3 mg, yield 34% (based on L).
[0070] We characterized the compound by IR, TGA, and the infrared spectrum results of Co-MOF-1 are shown in Figure 7 , see the TGA spectrum Figure 8 .
Embodiment 3
[0071] Example 3: Synthesis of Co-MOF-2
[0072] The crystal of Co-MOF-1 prepared in Example 2 was placed in the air at room temperature for 24 hours, and then kept at 70°C for 2 hours to obtain the compound Co-MOF-2. We characterized the compound by IR and TGA, and the results are shown in Figure 9 , 10 .
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