FePc-loaded metal-organic framework composite nano material, preparation method thereof and application thereof for chemiluminiscence detection
A technology of metal-organic frameworks and composite nanomaterials, which is applied in the direction of chemical reaction of materials, chemiluminescence/bioluminescence, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of conjugated rigid macrocycles The structure is insoluble in aqueous solution, limited catalytic activity, and difficult to be practically applied, etc., to achieve the effect of convenient industrial scale production, high catalytic activity, and simple reaction steps
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Embodiment 1
[0053] Synthesis of FePc@ZIF-90:
[0054] Heat and stir imidazolyl-2-carboxaldehyde (40.0mg, 0.416mmol) and 20mL DMF at 50℃ until the imidazolyl-2-carboxaldehyde is completely dissolved, then cool to room temperature; add zinc nitrate hexahydrate (31.5mg, 0.106mmol) ) And FePc (4.0mg, 0.0070mmol) were dissolved in 20mL DMF; 172μL trioctylamine was dissolved in 10mL DMF; then imidazolyl-2-formaldehyde solution and Zn(NO 3 ) 2 ·6H 2 The O solution is kept in the refrigerator (4℃) for 20 minutes; under the condition of vigorous stirring, pour the imidazolyl-2-formaldehyde solution into the Zn(NO 3 ) 2 ·6H 2 O solution, then add trioctylamine solution. After stirring for 1 min, the reaction was quenched by adding 20 mL of ethanol. Then, the mixed solution was centrifuged at high speed at 12000 rpm for 20 minutes to obtain a blue solid powder, and a large amount of DMF was used to wash away excess imidazolyl-2-formaldehyde, zinc nitrate, FePc, etc. Finally, they were washed with abso...
Embodiment 2
[0066] Synthesis of FePc@ZIF-90:
[0067] The imidazolyl-2-carboxaldehyde (80.0mg, 0.832mmol) and 40mL DMF were heated and stirred at 50℃ until the imidazolyl-2-carboxaldehyde was completely dissolved, and then cooled to room temperature; the zinc nitrate hexahydrate (89.2mg, 0.300mmol) ) And FePc (8.0mg, 0.014mmol) were dissolved in 40mL DMF; 390μL trioctylamine was dissolved in 20mL DMF; then imidazolyl-2-formaldehyde solution and Zn(NO 3 ) 2 ·6H 2 The O solution is kept in the refrigerator (4℃) for 30 minutes; under the condition of vigorous stirring, pour the imidazolyl-2-formaldehyde solution into the Zn(NO 3 ) 2 ·6H 2 O solution, then add trioctylamine solution. After stirring for 1 min, 40 mL of ethanol was added to quench the reaction. Then, the mixed solution was centrifuged at a high speed of 12000 rpm for 30 minutes to obtain a blue solid powder, and a large amount of DMF was used to wash off excess imidazolyl-2-formaldehyde, zinc nitrate, FePc, etc. Finally, they wer...
Embodiment 3
[0070] The synthesis procedure of FePc@ZIF-90 is the same as in Example 1.
[0071] Synthesis of FePc@ZIF-90-Lum:
[0072] At room temperature, add FePc@ZIF-90 (9mg) and luminol (10mg) into 3mL methanol and stir, add diethylamine (100μL), stir and react for 3h, centrifuge to obtain green powder, wash off with a large amount of DMF The reaction of luminol. Finally, they were washed with absolute ethanol and ether, and the product was dried in a vacuum drying oven at 40°C for 12 hours to obtain a green powder called FePc@ZIF-90-Lum.
[0073] As mentioned in the background art, although iron phthalocyanine (FePc) is used as an artificial peroxidase mimic enzyme to catalyze hydrogen peroxide, the large and rigid conjugated molecular structure of FePc makes FePc hardly soluble in water and easy to aggregate, which greatly reduces The catalytic activity of FePc is reduced, which limits its application as a chemical sensor in the water phase.
[0074] In view of this, the present invention...
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