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Ruthenium water oxidation catalyst based on electronegative ligand and preparation method thereof

An oxidation catalyst and electronegative technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of insufficient stability and fast decay rate of catalytic current density etc. to achieve good photoelectrochemical performance, simple preparation method and high yield

Inactive Publication Date: 2018-06-22
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the catalytic current density decay rate of this composite electrode is very fast, and the stability is not good enough. After 1 hour of reaction, its current density drops to 2mA / cm 2 , after 5 hours, its current density dropped to 1mA / cm 2 the following

Method used

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  • Ruthenium water oxidation catalyst based on electronegative ligand and preparation method thereof
  • Ruthenium water oxidation catalyst based on electronegative ligand and preparation method thereof
  • Ruthenium water oxidation catalyst based on electronegative ligand and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation of embodiment 1 carbazole derivative I

[0032]

[0033] Add carbazole (5.02g, 30mmol) and 100mL CH to a 250mL two-necked bottle 2 Cl 2 , added anhydrous aluminum trichloride (9.33g, 70mmol) in batches under stirring at room temperature, continued stirring for 90 minutes, cooled the reaction to 0°C in an ice-water bath, slowly added dodecanoyl chloride (15.30g, 70mmol) dropwise ), after the dropwise addition, the reaction temperature was raised to room temperature, and the stirring reaction was continued for 14 hours. The reaction solution was poured into 200mL ice water, the precipitate was collected by filtration, rinsed with deionized water and methanol respectively, the crude product was collected and recrystallized with methanol / acetone, and dried in vacuo to obtain white pure product 3,6-bis(dodecanoyl) Carbazole (11.20 g, 70% yield). 1 H NMR (400MHz, CDCl 3 ,): δ (ppm) 8.98 (br, 1H), 8.79 (s, 2H), 8.14 (d, J = 8.8Hz, 2H), 7.49 (d, J = 8.8Hz...

Embodiment 2

[0038] Example 2 Preparation of Metal Complex Ru with Carbazole Dicarboxylic Acid Derivatives as Skeleton

[0039]

[0040] Compound Ⅰ and Ru(DMSO) 4 Cl 2 in Et 3 N and anhydrous DMF, heated to 110 ° C for 12 h. Then 4-picoline was added, and the reaction was continued at 90°C for 10 hours. The reaction was stopped, cooled to room temperature, and the solvent was spin-dried to obtain a dark green powder product. Compound Ⅰ and Ru(DMSO) 4 Cl 2 The molar ratio of 1:1, 4-picoline is in excess. The above steps are all carried out under anhydrous and oxygen-free conditions.

[0041] Finally, with CH 2 Cl 2 / CH 3 OH=100:1 (V:V) was used as the eluent for silica gel column separation to obtain a green solid product (yield 45%). TOF-MS: m / z=[M+H] + calcd:970.4910;found,970.4941.m / z=[M+Na] + calcd:992.4730;found:992.4754.Elem.anal:calcd.for C 56 h 75 N 4 o 4 Ru(%): C 69.32, H 7.74, N 5.78; found, C 69.23, H 7.72, N 5.88.

Embodiment 3

[0042] Crystal growth and analysis of embodiment 3 metal complex Ru

[0043] The crystal cultivation method of the complex: Slowly add 0.1 mL of deionized water to 5 mL of the methanol solution in which the complex (15 mg) is dissolved, store it in a sealed container, and let it stand at room temperature for five days. The entire system is supersaturated through the interdiffusion of methanol and water , a green crystal suitable for single crystal testing was precipitated.

[0044] The structure of the complex was tested by X-ray single crystal diffraction, and its X-ray single crystal diffraction data were obtained. For specific test instruments and methods, see Section 2.2.3 of Chapter II. The crystallographic parameters and test parameters of the complexes are listed in Table 1.

[0045] Table 1 Crystal test data and related parameters of complex Ru

[0046]

[0047] Through the X-ray single crystal diffraction test, the precise spatial structure of the complex Ru was...

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Abstract

The invention discloses a ruthenium water oxidation catalyst based on an electronegative ligand and a preparation method thereof, and belongs to the technical field of catalyst preparation. The overpotential of the molecular catalyst can be reduced through the electronegative ligand, so that the electronegative tridentate ligand with a conjugated system is designed and synthesized, simultaneouslya long carbon chain is also introduced into the molecular catalyst, and the electronegative tridentate ligand can be preferably combined with a carboxylated multi-wall carbon nanotube. Therefore, thewater oxidization catalyst has preferable electrochemical performance inside electro-catalysis water oxidation, so that the catalyst provides an effective half-reaction for water oxidation, and an effective approach is provided for solving environmental problems and energy problems.

Description

technical field [0001] The invention relates to a ruthenium water oxidation catalyst based on an electronegative ligand and a preparation method thereof, belonging to the technical field of catalyst preparation. Background technique [0002] Molecular catalysts for water oxidation have developed rapidly in recent years, and one of their advantages is that the electrochemical properties of the catalyst can be changed by adjusting the ligands. The introduction of electronegative ligands is beneficial to reduce the potential energy of high-valence reaction intermediates, which can effectively reduce the overpotential of the catalyst and accelerate the water oxidation reaction. However, the current research is still far from the real realization of artificial photosynthesis, and electrochemical water oxidation molecular devices can improve the practical application of water oxidation molecular catalysts. The ultimate goal of artificially simulating photosynthesis is to convert ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07F15/00C25B1/04C25B11/06
CPCB01J31/1815B01J31/2217B01J2531/0213B01J2531/0241B01J2531/821C07F15/0053C25B1/04C25B11/075Y02E60/36
Inventor 高岩路忠凯陈旭阳
Owner DALIAN UNIV OF TECH
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