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Photoinduced hydrogen production catalytic system taking graphene as electron mediator and containing iron-sulfur cluster compound and preparation method and application of catalytic system

A catalytic system and cluster technology, applied in the field of photo-induced hydrogen production catalytic system, can solve the problems of violating the green concept of photo-induced hydrogen production, violating the green concept of photo-induced hydrogen production, low hydrogen production effect, etc.

Active Publication Date: 2016-04-13
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, the aforementioned method for photoinduced hydrogen production has the following disadvantages: (1) the platinum metal used is a noble metal, which increases the application cost of photoinduced hydrogen production because of its relatively expensive price.
(2) Tetraphenylporphyrin is insoluble in water, so that the photo-induced hydrogen desorption experiment cannot be carried out in pure water, thus violating the green concept of photo-induced hydrogen in water
(3) Most hydrogenase model substances are slightly soluble or insoluble in water, so their photo-induced hydrogen desorption experiments must be carried out in organic solutions or organic aqueous solutions, which also violates the green concept of photo-induced hydrogen production in pure water
(4) The efficiency of electron transfer from the photosensitizer to the catalyst determines the efficiency of hydrogen production. The effect of hydrogen production is not ideal

Method used

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  • Photoinduced hydrogen production catalytic system taking graphene as electron mediator and containing iron-sulfur cluster compound and preparation method and application of catalytic system
  • Photoinduced hydrogen production catalytic system taking graphene as electron mediator and containing iron-sulfur cluster compound and preparation method and application of catalytic system
  • Photoinduced hydrogen production catalytic system taking graphene as electron mediator and containing iron-sulfur cluster compound and preparation method and application of catalytic system

Examples

Experimental program
Comparison scheme
Effect test

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 O0.036mL (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 heated...

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 mixture into a 500mL three-necked flask, install a condenser tube, 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 33.3mgA and 35.6mgCH 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 a...

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Abstract

The invention provides a photoinduced hydrogen production catalytic system taking graphene as an electron mediator and containing an iron-sulfur cluster compound and a preparation method and application of the catalytic system, and belongs to the field of photoinduced hydrogen production catalysts. Particularly, the photoinduced hydrogen production catalytic system taking graphene as the electron mediator and containing the iron-sulfur cluster compound comprises a metal-sulfur cluster compound and a benzoporphyrin derivative which are connected with graphene oxide (GO). According to the photoinduced hydrogen production catalytic system taking graphene as the electron mediator and containing the iron-sulfur cluster compound and the preparation method and application of the catalytic system, the defect that most of hydrogenase model compounds are not dissolved in water is overcome, and obtained graphene oxide serves as a nano material to be connected with a medium; the hydrogen yield of the system taking the nano material as the catalyst is obviously higher than other systems; in addition, the nano material does not use a noble metal catalyst, and the production cost is further reduced.

Description

technical field [0001] The invention relates to a photoinduced hydrogen production catalytic system using graphene as an electron transfer medium and an iron-sulfur cluster as a catalyst, its preparation method and application, and belongs to the field of photoinduced hydrogen production catalysts. Background technique [0002] As we all know, the energy problem is one of the problems facing mankind in the new century. Until now, the main source of global energy still relies on fossil fuels. However, as a non-renewable energy source, fossil fuels cannot always meet the increasing energy needs of mankind. As a clean, pollution-free and almost inexhaustible form of energy, solar energy has become one of the main energy sources developed by human beings. However, the problem of how to directly store solar energy has become the biggest obstacle to the effective use of solar energy. As one of the most ideal energy sources, hydrogen energy has high energy density and can be dir...

Claims

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Application Information

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IPC IPC(8): B01J31/22C01B3/04
CPCC01B3/042B01J31/1625B01J2531/842B01J2531/0211B01J35/39Y02E60/36
Inventor 闫敬李瑞霞尹一冰梅顺康
Owner TIANJIN UNIV
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