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Zinc porphyrin complex used for electrocatalysis oxygen evolution reaction, and preparation method thereof

A technology of oxygen evolution reaction and complexes, which is applied in organic chemical methods, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., to achieve high yield, easy access to solvents, and time-saving effects

Inactive Publication Date: 2017-09-15
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although metal-organic frameworks (MOFs) have shown promising application prospects in OER, there are few reports on the direct use of metal-organic framework crystals as OER catalysts.

Method used

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  • Zinc porphyrin complex used for electrocatalysis oxygen evolution reaction, and preparation method thereof
  • Zinc porphyrin complex used for electrocatalysis oxygen evolution reaction, and preparation method thereof
  • Zinc porphyrin complex used for electrocatalysis oxygen evolution reaction, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] This embodiment relates to a method for preparing 5,10,15,20-tetracyanophenylporphyrin, which specifically includes the following steps:

[0036] in N 2 Under atmosphere, add 0.565g p-cyanobenzaldehyde to 500mL anhydrous CH 2 Cl 2 , stirred for 20 minutes to remove the air contained in the solution. Then add 0.3ml of pyrrole to the above mixture and stir well. After refluxing at 130°C for 30 minutes, add 52.5 μL of BF 3 ·OEt 2 (0.85 nmol), and protect the reaction mixture from light with tin foil. After stirring for 2 hours, 0.78 g of p-chlorobenzoquinone (0.37 mmol) was added as a solid, and the solution was refluxed for 4 hours and slowly cooled to room temperature. The residue was separated and purified by silica gel column chromatography, and CHCl 3 Elution afforded (CNTCPP). The NMR data of the ligand obtained in this embodiment are as follows: 1 H NMR (CDCl 3 )δ8.83(s, 8H), 8.35(d, 8H), 8.10(d, 8H).

Embodiment 2

[0038] This embodiment relates to a preparation method for preparing a porphyrin zinc complex, specifically comprising the following steps:

[0039] Take 20mg (0.028mmol) of 5,10,15,20-tetracyanophenylporphyrin prepared in the examples, and 20mg (0.15mmol) of zinc chloride, mix in DMF and EtOH and prepare according to the volume ratio of 2:1 1 mL of mixed solvent, transferred to a glass tube, sealed, and reacted at 120°C for 3000 min to obtain dark brown crystals, which were collected and filtered, washed with EtOH, and dried at room temperature to obtain Zn-CNTCPP. The yield was 25%. The theoretical content of each element in Zn-CNTCPP is respectively: C, 74.09%, H, 3.11%, N, 14.40%; the measured values ​​are respectively C, 74.52%, H, 3.65%, N, 14.02%.

[0040] The crystal structure was collected at room temperature (293K) with an Agilent Xcalibur Eos Gemini single crystal diffractometer. With a graphite monochromator, λ is Absorption correction was performed using a multi...

Embodiment 3

[0050] Embodiment 3 This embodiment relates to the electrocatalytic activity research of porphyrin zinc complex

[0051] Since the zinc ion in the porphyrin center does not form a true coordination bond with the cyano groups in the other CNTCPP ligands, the central Zn 2+ The ion is unsaturated and coordinated, so it can function as a catalytically active center. Therefore, the electrocatalytic activity of Zn-CNTCPP was tested.

[0052] The oxygen evolution reaction activity of the porphyrin zinc complex prepared in Example 2 was detected, and as a comparison, the pure CNTCPP ligand, ZnCl 2 The mixture obtained by manual grinding and mixing with CNTCPP ligand (referred to as mixture A), ZnCl 2 and the CNTCPP ligand obtained by fully reflux mixing in hot DMF (referred to as the mixture B), and the Zn(OH) obtained by the conventional precipitation reaction 2 The electrocatalytic oxygen evolution reaction activity was tested. The specific experimental method is:

[0053] A gl...

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Abstract

The invention discloses a zinc porphyrin complex used for electrocatalysis oxygen evolution reaction, and a preparation method thereof. The molecular formula of the zinc porphyrin complex is Zn(CNTCPP), wherein Zn is a divalent ion, CNTCPP is 5,10, 15, 20-tetracyanide phenyl porphyrin ligand; the structure of the zinc porphyrin complex belongs to monoclinic system P2<1> / n space group; the crystal basic structure unit is obtained from an asymmetric unit via symmetry operation; symmetry operation codes are x, y, z; 0.5-x, 0.5+y, 0.5-z; -x, -y, -z; 0.5+x, 0.5-y, 0.5+z; the asymmetric unit is composed of a ligand CNTCPP and Zn<2+>, lattice parameters axial length a=9.7858(3) angstroms, b=9.3797(2) angstroms, c=21.3172(5) angstroms; axial angle alpha=90.00 DEG, beta=100.777(3) DEG, gamma=90.00 DEG; unit cell size V=1922.15(9) angstroms3, Z=2. The advantages are that: 1, the reaction solvent is easily available, cheap, and green, and no pollution is caused; 2, reaction conditions are simple, reaction can be realized quickly, energy is saved, and time is saved; and 3, yield is high, ligand using amount is low, and cost is low.

Description

technical field [0001] The invention belongs to the technical field of new materials, and specifically discloses a simple, high-efficiency, green metal-organic framework material (porphyrin zinc complex) constructed on the basis of porphyrin organic ligands at a relatively low temperature, a preparation method and its application in Application in electrocatalytic oxygen evolution reaction. Background technique [0002] As global energy demand increases, finding renewable and carbon-neutral energy alternatives to fossil fuels is becoming an urgent issue. In the past few decades, people have been working hard to find reliable ways to obtain hydrogen or oxygen through the splitting of water. In general, the splitting of water can be divided into two half-reactions: the production of hydrogen from the reduction of water, and the production of oxygen from the oxidation of water. The oxygen evolution reaction (OER) requires the oxidation process of four electrons from two water...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22B01J31/22C25B1/04C25B11/06
CPCC25B1/04C07D487/22B01J31/183C07B2200/13B01J2531/025B01J2531/26B01J35/33Y02E60/36
Inventor 戴昉纳林欢黄招娣袁雪王雨桐范卫东王霞
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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