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Preparation method for electrocatalytic carbon dioxide reduction electrode, and application thereof

A technology of carbon dioxide and electrocatalysis, applied in the direction of electrodes, electrolysis process, electrolysis components, etc., can solve environmental pollution and other problems, and achieve the effect of excellent catalytic activity

Active Publication Date: 2018-11-23
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a catalyst, MOF materials can catalyze the reduction of carbon dioxide with high activity and high selectivity. However, Re-MOF thin film catalysts and many reported MOF catalysts contain noble metals, and the catalytic reaction is carried out in organic solvents, which is easy to pollute the environment.

Method used

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  • Preparation method for electrocatalytic carbon dioxide reduction electrode, and application thereof
  • Preparation method for electrocatalytic carbon dioxide reduction electrode, and application thereof
  • Preparation method for electrocatalytic carbon dioxide reduction electrode, and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation of embodiment 1 MOF catalyst

[0032] (1) Preparation of Zn-TCPP(Co)-MOF

[0033] Add cobalt nitrate hexahydrate (2.9mg, 10μmol), TCPP (7.9mg, 10μmol) and DMF (5mL) into a 10mL two-necked round bottom flask, sonicate for 30min and put it in an oil bath for reflux reaction under nitrogen protection for 3h. After the reaction was completed, it was naturally cooled to room temperature, and then 1.5 mL of absolute ethanol and zinc nitrate hexahydrate (5.9 mg, 20 μmol) were added to the flask, heated to 80° C. to continue the reaction for 24 h, and then naturally cooled to room temperature. The obtained red crystals were separated by a high-speed centrifuge, washed three times with DMF and ethanol, and dried in vacuum at 25°C for 12 hours to obtain a red solid Zn-TCPP(Co)-MOF.

[0034] (2) Preparation of Zn-TCPP(Zn)-MOF

[0035] DMF (6mL) and absolute ethanol (2mL) were added to a 20mL round bottom flask to obtain a mixed solvent, zinc nitrate (17.8mg, 60μm...

Embodiment 2

[0044] Example 2 Preparation of Zn-TCPP(Co)-MOF / CP electrode

[0045] Before preparing the Zn-TCPP(Co)-MOF / CP electrode, carbon paper (CP, 1×2.5cm 2 ) were washed with concentrated nitric acid, ethanol and ultrapure water to remove organic matter and metal impurities on the surface of carbon paper. Get 2.5mgZn-TCPP(Co)-MOF and add the mixed solution (V EtOH :V PEI :V Nafion =1000:1:2), sonicate for 30 minutes to obtain a uniform dispersion. Take 0.1mL of the dispersion and evenly drop it on the carbon paper (the active area is 1cm 2 ), and then dried in air overnight to obtain the Zn-TCPP(Co)-MOF / CP electrode. Zn-TCPP(Zn)-MOF / CP electrodes can be prepared by the same method.

Embodiment 3

[0046] Example 3 Test of electrochemical properties of Zn-TCPP(Co)-MOF / CP electrode

[0047] Cyclic voltammetry and electrochemical stability test of three-electrode system

[0048] In a closed electrolytic cell, a three-electrode system was used to test the half-reaction of electrochemical carbon dioxide reduction. The Zn-TCPP(Co)-MOF / CP electrode was used as the working electrode, the platinum wire electrode was used as the counter electrode, and Ag / AgCl (saturated KCl solution) The electrode is the reference electrode, 0.5M CsHCO 3 The aqueous solution (pH=8.6) is the electrolyte solution. First pass argon gas into the electrolyte for 0.5h to discharge the electrolytic cell and oxygen dissolved in the electrolyte, and then carry out cyclic voltammetry scanning (scanning rate 50mV / s) in nitrogen protection. Then, carbon dioxide was introduced into the electrolytic cell for 0.5h until the carbon dioxide was dissolved and saturated in the electrolyte (pH=7.3), and then a cyc...

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Abstract

The invention discloses a preparation method for an electrocatalytic carbon dioxide reduction electrode, and an application thereof, and belongs to the technical field of electrocatalysis. According to the preparation method for the electrocatalytic carbon dioxide reduction electrode, and the application thereof, Zn-TCPP(Co)-MOF is prepared in a two-step method, a complex formed by metallic cobaltand tetrakis(4-carboxylphenyl) porphyrin is an organic ligand of MOF, and zinc nitrate is a node. Zn-TCPP(Co)-MOF is loaded onto carbon paper to form a Zn-TCPP(Co)-MOF / CP electrode, and excellent catalytic activity and selectivity for a principal product carbon monoxide are shown in an electrocatalytic carbon dioxide reduction system taking 0.5 M CsHCO3 aqueous solution as an electrolyte.

Description

technical field [0001] The invention relates to a preparation method and application of an electrocatalytic carbon dioxide reduction electrode, belonging to the technical field of electrocatalysis. Background technique [0002] In the past two decades, a large number of catalysts for carbon dioxide reduction have been reported, and most of these catalysts are used in electrocatalytic carbon dioxide reduction half-reaction systems. In recent years, the research on the full battery system of electrocatalytic water splitting to produce hydrogen and oxygen has become more and more popular, but the full battery system of electrocatalytic carbon dioxide reduction coupled with water oxidation has rarely been reported. This is because the carbon dioxide molecule has a stable structure and will Its reduction requires more energy than splitting water to produce hydrogen, so it is more challenging to construct a full battery system with electrocatalytic carbon dioxide reduction coupled...

Claims

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Application Information

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IPC IPC(8): C25B1/00C25B11/06C25B11/12
CPCC25B1/00C25B11/043C25B11/051C25B11/095
Inventor 高岩路忠凯陈旭阳
Owner DALIAN UNIV OF TECH
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