Water oxidation catalyst using metal organic frame material for immobilization and preparation method thereof
A metal-organic framework and organic framework technology, applied in the field of water oxidation heterogeneous catalysts and its preparation, can solve the problems of uncontrollable, uncertain water oxidation rate slowdown, etc., to prevent deactivation, good morphology and structure , the effect of high catalytic performance
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Embodiment 1
[0036] A method for preparing a water oxidation catalyst immobilized with a metal organic framework material, comprising the following steps:
[0037] (1) Preparation of metal-organic framework material MIL-101(Cr): This process was carried out in a 100mL polytetrafluoroethylene hydrothermal kettle, and Cr(NO 3 ) 3 9H 2 O (400mg, 1mmol), and 1 equivalent of terephthalic acid (H 2 BDC, 164mg, 1mmol) was dissolved in 4.8mL water, and ultrasonicated in an ultrasonic cleaner for 4min. Add hydrofluoric acid (HF, 1 mmol) into the above solution, and continue to sonicate until it is well mixed to obtain a reaction precursor solution. Then put the reaction precursor solution into an electric constant temperature blast drying oven, set the reaction program: 1°C / min to 220°C for 8h, 1h to 150°C and then keep for 12h, then 1°C / min to room temperature.
[0038] After the reaction is over, use the following filtration methods to remove impurities:
[0039] First, vacuum filter with a ...
Embodiment 2
[0055] A method for preparing a water oxidation catalyst immobilized with a metal organic framework material, comprising the steps of:
[0056] (1) The synthesis method of MIL-101 (Cr) is the same as (1)) step in Example 1. The ultrasonic time is 5 min.
[0057] (2)MIL-101(Cr)-N 3 Preparation: 100mg MIL-101(Cr) was added to the mixture of 7mL concentrated nitric acid and 5mL concentrated sulfuric acid, and reacted in ice bath for 6h. After the reaction, the reaction solution was raised to room temperature and then poured into 50 mL of crushed ice. After the temperature rises to room temperature, filter and wash with a large amount of deionized water until neutral. The solid was activated with water (30 mL) and ethanol (30 mL) at 80° C. for 6 h, respectively. The filtered solid was vacuum-dried at 120°C for 12 hours to remove small solvent molecules in the pores to obtain MIL-101(Cr)-NO 2 .
[0058] Next, 100mg MIL-101(Cr)-NO 2 and 3.26g SnCl 2 2H 2 O was ultrasonicall...
Embodiment 3
[0066] A method for preparing a water oxidation catalyst immobilized with a metal organic framework material, comprising the steps of:
[0067] (1) The synthesis method of MIL-101 (Cr) is the same as (1)) step in Example 1. The ultrasonic time is 10min.
[0068] (2)MIL-101(Cr)-N 3 Preparation: 200mg MIL-101(Cr) was added to a mixture of 14mL concentrated nitric acid and 10mL concentrated sulfuric acid, and reacted in ice bath for 7h. After the reaction, the reaction liquid was raised to room temperature and then poured into 100 mL of crushed ice. After the temperature rises to room temperature, filter and wash with a large amount of deionized water until neutral. The solid was activated with water (30 mL) and ethanol (30 mL) at 80° C. for 6 h, respectively. The filtered solid was vacuum-dried at 120°C for 12 hours to remove small solvent molecules in the pores to obtain MIL-101(Cr)-NO 2 .
[0069] Next, 200mg MIL-101(Cr)-NO 2 and 6.25g SnCl 2 2H 2 O was ultrasonically...
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