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Asymmetric hydronitrogen-pyridine-nickel metal catalyst, and preparation method and application of catalyst

A metal catalyst, asymmetric technology, applied in the field of electrochemistry, to achieve the effect of stabilizing intermediates, promoting coordination, and benefiting the electrocatalytic reduction of carbon dioxide

Active Publication Date: 2018-06-08
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, few nickel-based nitrogen-ligand molecular catalysts can efficiently and selectively reduce carbon dioxide to carbon monoxide

Method used

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  • Asymmetric hydronitrogen-pyridine-nickel metal catalyst, and preparation method and application of catalyst
  • Asymmetric hydronitrogen-pyridine-nickel metal catalyst, and preparation method and application of catalyst
  • Asymmetric hydronitrogen-pyridine-nickel metal catalyst, and preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0108] An asymmetric nitrogen-hydrogen-pyridine-nickel-acetonitrile metal catalyst, namely 2 MeCN , its structural formula is as follows:

[0109]

[0110] The synthetic route of above-mentioned catalyst is as figure 1 As shown, the preparation includes the following steps:

[0111] 1) Synthesis of Compound 5:

[0112] In compound 4 (1.05g, 5.0mmol) in dry tetrahydrofuran, methylmagnesium bromide (3.0M in ether solution, 0.85mL, 2.5 equivalents, 12.5mmol) was added dropwise at -15°C, and reacted at -15°C Stirring was continued for 1 h at room temperature, and then stirring was continued for 2 h at room temperature to obtain an orange-red liquid. After the reaction was completed, saturated ammonium chloride was added dropwise under ice bath conditions to quench the reaction, the organic phase was extracted with tetrahydrofuran and dichloromethane respectively, the organic phase was combined, washed three times with saturated brine, dried over anhydrous sodium sulfate, the...

Embodiment 2

[0132] 2 prepared in Example 1 MeCN Perform electrochemical performance characterization:

[0133] In 2.5mL of 0.1M tetrabutylammonium hexafluorophosphate acetonitrile, add the 2 prepared in Example 1 MeCN , to get a mixed solution, wherein the concentration of the mixed solution is 2mM (that is, every L tetrabutylammonium hexafluorophosphate acetonitrile contains 2mmol of 1 MeCN ), after 10 min of Ar, the electrochemical CV was scanned at a scan rate of 50 mV / s; after that, after 10 min of carbon dioxide, the electrochemical CV was scanned at a scan rate of 50 mV / s.

[0134] Characterization results such as Figure 5 Shown, the compound's cyclic voltammetry curve (CV) Ar or CO in acetonitrile solution 2 Obtained under; Among them, under Ar, compound 1 MeCN exhibits two reversible electrochemical peaks E 1 / 2 =-0.35V (peak I) and -1.03V (peak II), peak I is electrochemically reversible, which is attributed to Ni(II) / Ni(I) electrochemical reduction electron pair, peak II is...

Embodiment 3

[0143] Test the generation of intermediate compound on the influence of asymmetric nitrogen-hydrogen-pyridine-nickel-acetonitrile metal catalyst electrochemical performance, the steps are as follows:

[0144] In 2.5mL of 0.1M tetrabutylammonium hexafluorophosphate in acetonitrile, add the 2 prepared in Example 1 MeCN, to get a mixed solution, wherein the concentration of the mixed solution is 5mM (that is, every L tetrabutylammonium hexafluorophosphate acetonitrile contains 2mmol of 1 MeCN ), after passing 20minAr, after saturation, electrolyze at -1.45V vs. NHE for 4h. Measure liquid infrared and observe the result. Compare the results of electrolysis and CO under Ar without electrolysis 2 Below is the electrolysis result.

[0145] The result is as Figure 7 and Figure 8 As shown, under Ar, 2 MeCN Three new peaks appeared, corresponding to the C═O double bond vibration and the C—O single bond vibration of carbon dioxide coordination. Explain that Ni compound and CO 2...

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Abstract

The invention discloses an asymmetric hydronitrogen-pyridine-nickel metal catalyst. The asymmetric hydronitrogen-pyridine-nickel metal catalyst is in a hexa-coordinate octahedral model structure, anda structural formula of the catalyst is shown as formula I as shown in the specification. According to the asymmetric hydronitrogen-pyridine-nickel metal catalyst, an asymmetric ligand complex is introduced into the structure; requirements of an electrochemical system on large pi-pi conjugated radicle groups to receive electrons are met; and the catalyst can be used for electric catalytic reduction of carbon dioxide into carbon monoxide.

Description

technical field [0001] The invention relates to the technical field of electrochemistry. More specifically, it relates to an asymmetric nitrogen-hydrogen-pyridine-nickel metal catalyst and its preparation method and application. Background technique [0002] At present, the content of carbon dioxide emitted by humans in the atmosphere is increasing year by year, leading to a serious greenhouse effect, global warming, melting glaciers, and rising sea levels. With the consumption of fossil fuels, CO in the air 2 The emissions are increasing, causing great pressure on the environment. CO 2 Reductive conversion into liquid fuels can not only balance the global atmospheric carbon balance, but also turn them into useful fuels to relieve environmental pressure. Currently, both electrochemical and photoelectrochemical methods can reduce CO 2 It is CO or formic acid, but there are many difficulties in controlling the specificity of the catalytic product. A major reason for CO ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07F15/04C25B11/06C25B1/00
CPCB01J31/1815B01J2531/0213B01J2531/0241B01J2531/847C07F15/045C25B1/00C25B11/075
Inventor 康鹏刘芳卫
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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