Ring metal iridium photosensitizers, synthesis thereof and application thereof in hydrogen preparation by photocatalytic reduction of water

A technology of photosensitizer and ring metal, which is applied in the field of chemical energy, can solve the problems of low activity, dual-core iridium photosensitive development has not been reported in the literature, etc., and achieve high activity, good photocatalytic reduction of water hydrogen production performance, and simple post-treatment Effect

Inactive Publication Date: 2013-10-23
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In 2009, Stefan Bernhard's research team first published an iridium photosensitizer based on C^N^N on Inorg.Chem. Its structure is as follows. This photosensitizer has high stability, but at the same time it has a low activity shortcoming
[0006] But so far, the development of iridium photosensitizers has been concentrated on mononuclear iridium photosensitizers, while the development of dual-nuclear iridium photosensitizers has not been reported in the literature.

Method used

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  • Ring metal iridium photosensitizers, synthesis thereof and application thereof in hydrogen preparation by photocatalytic reduction of water
  • Ring metal iridium photosensitizers, synthesis thereof and application thereof in hydrogen preparation by photocatalytic reduction of water
  • Ring metal iridium photosensitizers, synthesis thereof and application thereof in hydrogen preparation by photocatalytic reduction of water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1: Synthesis of P1 and P2

[0028] Add iridium trichloride hydrate and 4-trifluoromethylphenylpyridine in a ratio of 1:2.2 to 40 ml of ethylene glycol monoethyl ether: water = 3:1, and react at 140 °C for 24 hours under nitrogen protection. After the reaction, the reaction solution was cooled to room temperature, and 100 ml of deionized water was added, at which time a large amount of yellow solids would precipitate. The reaction solution was filtered under reduced pressure to obtain a yellow solid. Dissolve the yellow solid again with dichloromethane, pass through the column with ethyl acetate:n-hexane=1:1, collect the yellow liquid, and obtain pure chlorine bridge dimer [Ir(tfppy)(μ-Cl)] 2 .

[0029] The chlorine-bridged dimer [Ir(tfppy)(μ-Cl)] 2 (300 mg) and bisbenzimidazole (128.7 mg) were added to the mixed solvent CH at a ratio of 1:2.2 2 Cl 2 : CH 3 OH =1:1, add Na 2 CO 3 396 mg, reflux reaction at 70 °C under nitrogen protection for 24 hours. Af...

Embodiment 2

[0033] In a homogeneous photocatalytic system, iridium photosensitizer photocatalytically reduces water to produce hydrogen: add 1 ml 1mol / L iridium photosensitizer P1 or P2, 2.5 ml triethanolamine, 0.33 mM catalyst, 1 g LiCl, 0.75 ml concentrated hydrochloric acid to 100 ml In the solvent (acetone in the solvent: water = 4:1), the air in the reactor was pumped dry, and the hydrogen gas generated by the reaction was quantitatively analyzed by gas chromatography under the irradiation of a 300 W xenon lamp (λ> 420 nm). The amount of hydrogen produced by the photosensitizer under the action of different catalysts is shown in Table 1:

[0034] Table 1

[0035]

[0036] It can be seen from the chart that among the four catalysts, except for CoCl 2 In addition, other catalysts combined with the photosensitizer used have the ability to catalyze the reduction of water to produce hydrogen. Among the many water reduction catalysts used, Rh(dtbpy) 3 3+has the best effect.

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Abstract

The invention discloses ring metal iridium photosensitizers, synthesis thereof and application thereof. The synthesis of the iridium photosensitizers comprises: placing chlorine-bridge dipolymer [Ir(tfmppy)(mu-Cl)]2 and bis(benzimidazole) into a mixed solvent of methanol and dichloromethane, and then adding Na2CO3 for reflux reaction; after the reaction, cooling, drying the solvent by rotary evaporation, then obtaining a target product through column chromatography. The column chromatography developing agent is a mixture of ethyl acetate and hexane, and the ratio of the ethyl acetate to the hexane is between 1:1 and pure ethyl acetate. Through use of the synthesis method, single-core and dual-core iridium photosensitizers can be simultaneously obtained, and post-treatment is simple, and the pure product can be obtained through simple column chromatography method. Compared with hydrogen preparation by photocatalytic reduction of water with a conventional single-core iridium photosensitizer, the single-core iridium photosensitizer of the invention has good performance of hydrogen preparation by photocatalytic reduction of water, and the dual-core iridium photosensitizer is more active than the single-core iridium photosensitizer.

Description

technical field [0001] The invention relates to an iridium photosensitizer, its synthesis and its application in photocatalytic reduction of water to produce hydrogen, and belongs to the field of chemical energy. Background technique [0002] The consumption of fossil energy not only causes an energy crisis, but also seriously damages our living environment. Finding clean, renewable new energy sources to replace fossil energy sources has become a current research hotspot. Hydrogen, as an environmentally friendly and clean secondary energy carrier, has attracted increasing attention. But so far, the most important way to prepare hydrogen is still to decompose water into hydrogen by electrolysis. The biggest defect of this method is that it will consume a lot of electric energy, and the consumed electric energy is greater than the obtained hydrogen energy, so the gain outweighs the gain. Finding energy-efficient ways to split water into hydrogen and oxygen has become a resea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00C01B3/02
Inventor 蔡建光李峰
Owner NANJING UNIV OF SCI & TECH
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