Fe-hydrogenase model compound, its preparation method, photo-catalytic hydrogen production system containing it, and hydrogen preparation method of system

A technology of simulating compounds and iron hydrogenase, which is applied in the direction of iron organic compounds, organic compound/hydride/coordination complex catalysts, hydrogen production, etc., can solve the problems of loss of catalytic activity, catalyst instability, cost increase, etc.

Active Publication Date: 2013-02-13
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above research results are of great significance for the development of photocatalytic hydrogen production systems, but most systems still have the following problems: First, the catalyst is unstable under light conditions, and most photocatalytic hydrogen production systems lose their catalytic activity after 1 hour of light irradiation ; Second, most systems are constructed in a mixed system of water and acetonitrile, and the TON value is generally less than 5; third, most systems use noble metals as photosensitizers, which increases the cost of the system

Method used

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  • Fe-hydrogenase model compound, its preparation method, photo-catalytic hydrogen production system containing it, and hydrogen preparation method of system
  • Fe-hydrogenase model compound, its preparation method, photo-catalytic hydrogen production system containing it, and hydrogen preparation method of system
  • Fe-hydrogenase model compound, its preparation method, photo-catalytic hydrogen production system containing it, and hydrogen preparation method of system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0130] Preparation of water-soluble ADT type iron hydrogenase mimetic compound (I), such as figure 1 The synthetic roadmap shown, wherein n=3 of SI-3, comprises the following steps:

[0131] 1) Add 0.6g C 14 h 8 Fe 2 INO 6 S 2 (hereinafter referred to as SI-1) and 0.15g of 4-ethynylbenzoic acid were dissolved in 20ml of tetrahydrofuran, then added 7ml of anhydrous triethylamine, degassed with argon for 25 minutes, and added 0.015g of Pd(PPh 3 ) 2 Cl 2 and 0.008g CuI, refluxed for 5 hours, after monitoring the completion of the reaction, separated with a silica gel column, rinsed with a mixed solution of methanol / dichloromethane=1 / 10 (v / v) to obtain the product SI-2;

[0132] 2) Add 7.50g of SI-3, 2.55g of propylenediamine protected by tert-butoxycarbonyl (hereinafter referred to as: Boc) at one end, and 7.75g of benzotriazol-1-yl-oxy hexafluorophosphate in 45ml of DMF Tripyrrolidinyl phosphorus (hereinafter referred to as: PyBOP) and 18ml triethylamine, stirred the mix...

Embodiment 2

[0137] Preparation of water-soluble ADT type iron hydrogenase mimetic compound (I), such as figure 1 The synthetic roadmap shown, wherein n=3 of SI-3, comprises the following steps:

[0138] 1) Dissolve 0.6g SI-1 and 0.15g 4-ethynylbenzoic acid in 30ml tetrahydrofuran, then add 9ml anhydrous triethylamine, degas with argon for 50 minutes, add 0.020g Pd(PPh 3 ) 2 Cl 2 and 0.010g CuI, refluxed for 7 hours, after monitoring the completion of the reaction, separated with a silica gel column, rinsed with a mixed solution of methanol / dichloromethane=1 / 10 (v / v) to obtain the product SI-2;

[0139] 2) Add 7.70g SI-3, 2.65g propylenediamine protected by Boc at one end, 7.80g PyBOP and 22ml triethylamine in 55ml DMF, stir the mixture at room temperature for 3 hours, then pour the mixture into 160ml water, and use Dichloromethane extracted 4 times, kept the organic layer, and then extracted 9 times with saturated brine to remove DMF in the mixed system, kept the organic layer, added N...

Embodiment 3

[0142] Same as Example 1, the only difference is that n=4 in SI-3, and the consumption of SI-3 is 10.6g.

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Abstract

The invention discloses an Fe-hydrogenase model compound, its preparation method, a photo-catalytic hydrogen production system containing it, and a hydrogen preparation method of the system. The Fe-hydrogenase model compound can be used for the photocatalytic hydrogen production system, and has a high catalytic activity. The photo-catalytic hydrogen production system containing the Fe-hydrogenase model compound comprises the Fe-hydrogenase model compound, a photo-sensitizer, an electronic donor, a proton source and a solvent; the catalytic activity of the system can be stably maintained for a plurality of hours under an illumination condition; the system can be constructed in pure water, or in a mixed system of water and an organic solvent, and the TON value of the system is large; and the photo-sensitizer used in the system comprises CdSe quantum dot, CdTe quantum dot, Ru(III) tri(terpyridine) and zinc porphyrin, so the cost of the system is reduced. Hydrogen can be generated through using visible light having a wavelength lambda of above 400nm to irradiate the system.

Description

technical field [0001] The invention relates to a photocatalytic hydrogen production system, in particular to an ADT type and a PDT type iron hydrogenase analog compound and a preparation method thereof, a photocatalytic hydrogen production system containing the same and a method for preparing hydrogen. Background technique [0002] Using solar energy to split water to produce hydrogen is one of the most ideal ways to solve the energy crisis faced by mankind. Because the solar energy involved in the whole reaction process is inexhaustible, and the water reserves on the earth are abundant and the cost is low; the product after hydrogen is used as an energy carrier is water, the process is clean and the result is environmentally friendly, and water can enter the next light The process of decomposing water constitutes a closed energy cycle. [0003] At present, people have developed several types of photocatalysts for solar photolysis of water, such as Pt sol catalysts, Co com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/02C07K5/107B01J31/26C01B3/02
Inventor 吴骊珠李成博王锋汪晶晶
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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