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

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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

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

Example Embodiment

[0031] Example 1 Preparation of MOF catalyst

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

[0033] Cobalt nitrate hexahydrate (2.9 mg, 10 μmol), TCPP (7.9 mg, 10 μmol) and DMF (5 mL) were added to a 10 mL two-necked round-bottomed flask, sonicated for 30 min, placed in an oil bath, and refluxed for 3 h under nitrogen protection. 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 hours, 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, respectively, and vacuum-dried at 25 °C for 12 h to obtain a red solid Zn-TCPP(Co)-MOF.

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

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

Example Embodiment

[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 × 2.5 cm 2 ) were washed with concentrated nitric acid, ethanol and ultrapure water to remove organic matter and metal impurities on the surface of carbon paper. Take 2.5mg Zn-TCPP(Co)-MOF into the mixed solution (V EtOH : V PEI : V Nafion =1000:1:2), ultrasonic for 30min 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 a Zn-TCPP(Co)-MOF / CP electrode. Zn-TCPP(Zn)-MOF / CP electrodes can be prepared by the same method.

Example Embodiment

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

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

[0048] A three-electrode system was used to test the electrochemical carbon dioxide reduction half-reaction in a closed electrolytic cell. The Zn-TCPP(Co)-MOF / CP electrode was used as the working electrode, the platinum wire electrode 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 an electrolyte solution. First, argon gas was introduced into the electrolyte for 0.5h to discharge the electrolytic cell and the oxygen dissolved in the electrolyte, and then cyclic voltammetry was performed under nitrogen protection (scanning rate 50mV / s). Then, carbon dioxide was introduced into the electrolytic cell for 0.5 h until the carbon dioxide was dissolved and saturated in the electrolyte (pH=7.3), and then th...

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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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