A photocatalytic system for hydrogen production of iron-sulfur clusters mediated by graphene, its preparation method and application
A catalytic system, graphene technology, applied in the direction of organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of increasing the application cost of photoinduced hydrogen production Problems such as the green concept of hydrogen production and the violation of the green concept of photo-induced hydrogen
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Embodiment 1
[0080] Embodiment 1 Synthesis of iron-sulfur cluster compound A, the chemical formula of the iron-sulfur cluster compound A is [Fe 2 (μ-SC 3 h 6 S)(CO) 5 ][Fc(PPh 2 ) CHO], the preparation process is as follows:
[0081]
[0082] Concrete preparation steps are as follows:
[0083] 1) Under the protection of nitrogen, add 193mg (0.5mmol) Fe to a 100mL round-bottomed flask equipped with a magnetic stirrer to remove water and oxygen. 2 (μ-SC 3 h 6 S)(CO) 6 , 199mg (0.5mmol) Fc (PPh 2 ) CHO, 55.6mg (0.5mmol) Me 3 NO·2H 2 O and 20 mL of acetonitrile to obtain a mixed solution, and stirred at room temperature for 5 hours to obtain a reddish-brown solution.
[0084] 2) The solvent was dried by rotary evaporation, thin-layer separation was carried out with tetrahydrofuran and n-hexane at a volume ratio of 1:3, the second reddish-brown band was collected, and the solvent was dried to obtain a reddish-brown solid A (229.8 mg, yield 60.8%) .
[0085] The structural data o...
Embodiment 2
[0086] Example 2 Synthesis of the model substance B capable of intramolecular electron transfer, the chemical formula of the model substance B is 5-{[Fe 2 (μ-SC 3 h 6 S)(CO) 5 ] (PPh 2 Fc)}-10,15,20-triphenylporphyrin, the preparation process is as follows:
[0087]
[0088] Concrete preparation steps are as follows:
[0089] 1) Under nitrogen protection, add 540mg (0.7mmol) of compound A and 200mL of dichloromethane into a 250mL round-bottomed flask equipped with a stirring magnet to remove water and oxygen, and stir to dissolve to obtain a mixed solution.
[0090] 2) Add 0.21 mL (2.1 mmol) of benzaldehyde and 0.19 mL (2.8 mmol) of pyrrole to the above mixture, and stir at room temperature for 15 minutes to obtain a reaction solution.
[0091] 3) Add BF to the above reaction solution in the dark 3 ·Et 2 O 0.036mL (0.28mmol), react at room temperature for 16 hours.
[0092] 4) Next, 688.5 mg (2.8 mmol) of chloranil was added to the above reaction solution, and heate...
Embodiment 3
[0095] Embodiment 3 synthesis takes graphene as the intermediary nano material C, and the preparation process is as follows:
[0096]
[0097] Concrete preparation steps are as follows:
[0098] 1) Put 160mg of TPP-NHCO-GO into 300mL of dimethylformamide solution and sonicate for 1h to obtain a mixed solution.
[0099] 2) Pour the above mixed solution into a 500mL three-neck flask, install a condenser, add 33.3mg of compound A (0.044mmol), 35.6mg of CH 3 NHCH 2 COOH (0.4 mmol), heated and stirred at 120°C for 24 hours to obtain a reaction solution.
[0100] 3) Add 33.3mg A and 35.6mg CH to the above reaction solution 3 NHCH 2 COOH, followed by 48 hours of reaction.
[0101] 4) Continue to add 33.3mg of compound A and 35.6mg of CH to the reaction solution 3 NHCH 2 COOH, reacted for 48 hours.
[0102] 5) Cool to room temperature, wash with tetrahydrofuran and anhydrous methanol three times, and dry in a vacuum oven at 60° C. to obtain nanomaterial C.
[0103] product...
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