Preparation method and electrocatalytic application of nickel bimetallic nanometer material

A bimetallic nano-electrocatalysis technology, applied in the field of electrochemistry, can solve the problems of inability to popularize industrial applications, complicated reaction conditions, etc., and achieve the effects of excellent electrochemical properties and chemical catalytic properties, cheap and easily available raw materials, and simple synthesis process.

Active Publication Date: 2019-03-12
EAST CHINA NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in most of the above-mentioned studies, the reaction conditions of the methods for synthesizing metal and bimetallic nanomaterials are relatively complicated, and cannot be popularized in industrial applications. Therefore, a simple and mild synthesis method is explored to prepare a cheap and easy-to-obtain metal with excellent catalytic performance. And bimetallic nanomaterials are a major difficulty in their research and application

Method used

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  • Preparation method and electrocatalytic application of nickel bimetallic nanometer material
  • Preparation method and electrocatalytic application of nickel bimetallic nanometer material
  • Preparation method and electrocatalytic application of nickel bimetallic nanometer material

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Experimental program
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Effect test

Embodiment 1

[0024] Take 1.4540g Ni(NO 3 ) 2 ·6H 2 O and 0.5097g AgNO 3 Dissolve in a mixed solution of 10mL deionized water and 20mL absolute ethanol and keep stirring, then slowly add dropwise a mixed solution of 30mL NaOH with a concentration of 1mol / L and 20mL with a concentration of 50vol% hydrazine hydrate, and react at 60°C for 3h , and then ultrasonically wash the product with deionized water and absolute ethanol, respectively, until the supernatant is clear and transparent, and finally vacuum-dry at 60°C to obtain a Ni / Ag 5 / 3 bimetallic nanomaterial.

[0025] See attached figure 1 , the above products are characterized by XRD curves, Ni / Ag 5 / 3 bimetallic nanomaterials have (111), (200) and (220) characteristic peaks of nickel and silver (111), (200), (220) and The characteristic peak of (311) shows that the product of embodiment 1 is the pure metal nanomaterial of nickel and silver.

[0026] See attached figure 2 , the above product was characterized by a scanning electron ...

Embodiment 2

[0028] Take 0.1g of the above-prepared Ni / Ag 5 / 3 bimetallic nanomaterial and add 0.2mL sodium carboxymethylcellulose sol, ultrasonically disperse and evenly coat both sides of 2cm×2.2cm carbon paper, and dry naturally to obtain Ni / Ag 5 / 3 solid electrodes made of bimetallic nanomaterials.

[0029] Add 20 mL of anhydrous N,N-dimethylformamide (DMF), 1 mmol of acetophenone, 2 mmol of tetra-n-butylammonium iodide (TBAI), 0.05 mmol of cinchonidine ( CD), 0.05mmol n-butanol, continuous and slow introduction of CO 2 and stir. Then insert a solid electrode made of Ni / Ag 5 / 3 bimetallic nanomaterials as the cathode, and a polished magnesium rod as the anode, and connect it to a galvanostat to form a circuit path, select a constant direct current of 10mA, and a current density of 2.5mA / cm 2 , until the end of the electrocarboxylation reaction. After the solvent was removed by rotary evaporation, 10 mL of 1 mol / L HCl was added to acidify, extracted three times with 30 mL of anhydrou...

Embodiment 3

[0031] Add 20 mL of anhydrous N,N-dimethylformamide (DMF), 1 mmol of acetophenone, 2 mmol of tetra-n-butylammonium iodide (TBAI), 0.05 mmol of L-(+) - Tartaric acid (L-(+)-TA) and 0.05mmol n-butanol, continuous slow passage of CO 2 and stir. Then insert a solid electrode made of Ni / Ag 5 / 3 bimetallic nanomaterials as the cathode, and a polished magnesium rod as the anode, and connect it to a galvanostat to form a circuit path, select a constant direct current of 10mA, and a current density of 2.5 mA / cm 2 , until the end of the electrocarboxylation reaction. After removing the solvent by rotary evaporation, add 10 mL of 1 mol / L HCl to acidify, and extract with 30 mL of anhydrous ether three times, then wash once with 10 mL of saturated NaCl solution, add anhydrous magnesium sulfate to dry for 1 hour, and then remove the ether by rotary evaporation to obtain the target Product 2-hydroxyl-2-phenylpropionic acid (2-hydroxy-2-phenylpropionic acid), its productive rate is 17%, ee ...

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Abstract

The invention discloses a preparation method and electrocatalytic application of a nickel bimetallic nanometer material. The preparation method of the nickel bimetallic nanometer material is characterized by synthesizing common nickel salts and other metal salts under normal-pressure heated conditions into the nickel bimetallic nanometer material with different molar ratios through a one-step process; the nickel bimetallic nanometer material can be manufactured into a solid electrode after being washed and vacuum-dried, which can serve as the anode of a pit type electrolytic tank to work together with a magnesium rod cathode for implementing asymmetric reactions such as acetophenone asymmetric electrocarboxylation. Compared with the prior art, the nickel bimetallic nanometer material is high in magnetism and high-temperature thermal stability, good in electrochemical property and electrocatalytic performance and easy to apply to modification of chiral compounds, processes are simple and easy to implement, and raw materials are low in price and easy to acquire; when applied to asymmetric reactions such as acetophenone asymmetric electrocarboxylation, the nickel bimetallic nanometermaterial presents high stability and catalytic activity to produce target products with high ee (enationmetric excess) values, thereby being an ideal electrocatalytic material with a good applicationprospect.

Description

technical field [0001] The invention relates to the technical field of electrochemistry, in particular to a preparation method of a nickel-based bimetallic nanometer material and its electrocatalytic application in the asymmetric electrocarboxylation reaction of acetophenone and carbon dioxide. Background technique [0002] In recent years, due to the important role of metal and bimetallic nanomaterials in the field of catalysis to replace noble metal catalysts, improve catalytic activity and selectivity, etc. (Stamenkovic VR, Mun BS, Arenz M, et al. Nat Mater, 2007, 6 :241–247.), control and synthesize different bimetallic materials around the composition of bimetallic materials, study the performance of the above-mentioned different bimetallic materials in different catalytic reactions, and try to find a catalyst with higher activity, selectivity and stability. Catalyst materials, and trying to explore new catalytic reactions and catalytic reaction mechanisms has become a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/745B01J23/75B01J23/89C25B11/06C25B3/00
CPCB01J23/745B01J23/75B01J23/892B01J35/0033C25B3/00C25B11/04
Inventor 陆嘉星曾胜王慧王烁杨丽荣王欢
Owner EAST CHINA NORMAL UNIV
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