In situ synthesis of copper nanowire array material and its preparation method and application

A technology of copper nanowires and in-situ synthesis, which is applied in nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problem of unstable catalysts, suitable deuterium donors, and the inability to accurately control the deuterium position and number, and deuterium rate No high problems, achieve the effect of maintaining shape and performance, low cost, and high deuterium substitution rate

Active Publication Date: 2022-05-24
TIANJIN UNIV
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  • Abstract
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Problems solved by technology

[0004] The present invention overcomes the deficiencies in the prior art. The existing deuterium reaction of organic matter has the problems of being unable to accurately control the position and number of deuterium, the rate of deuterium is not high, the catalyst is unstable and the catalyst is suitable for special deuterium donors, and provides a An in-situ synthesized copper nanowire array material and its preparation method and application. The present invention synthesizes a copper nanowire array (Cu NWAs) material through an in-situ conversion method, and uses the copper nanowire array (Cu NWAs) material as an electrochemical reaction The cathode of C-X / C-D was realized by a simple electrochemical reduction method using deuterated water as a deuterium source, and the preparation of deuterated drugs was realized by this method

Method used

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  • In situ synthesis of copper nanowire array material and its preparation method and application
  • In situ synthesis of copper nanowire array material and its preparation method and application
  • In situ synthesis of copper nanowire array material and its preparation method and application

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Embodiment 1

[0052] Step 1: The copper sheet (3cm*1cm*0.1mm) was ultrasonicated in acetone and 3.0M HCl solution for 15min respectively, then rinsed with distilled water and ethanol respectively, and dried with cold air in the air for subsequent use;

[0053] In step 2, two copper sheets obtained in step 1 were taken out and placed in a single-chamber reaction cell, respectively the anode and the cathode, and the electrodeposition reaction was carried out with 3M NaOH solution as the electrolyte. 2 The reaction was carried out for 6 min under the current density of 100 Å to form a dark blue copper hydroxide nanowire array precursor;

[0054] Step 3, placing the dark blue copper hydroxide precursor prepared in step 2 in a quartz tube with a diameter of 6 mm, calcining at 150° C. for 3 hours, and heating at a rate of 2° C. / min to obtain a copper oxide nanowire array;

[0055] Step 4, a two-chamber separated electrolytic cell was used, using the copper nanowire array as the working electrode,...

Embodiment 2

[0057] Step 1: The copper sheet (3cm*1cm*0.1mm) was ultrasonicated in acetone and 3.0M HCl solution for 15min respectively, then rinsed with distilled water and ethanol respectively, and dried with cold air in the air for subsequent use;

[0058] In step 2, two copper sheets obtained in step 1 were taken out and placed in a single-chamber reaction cell, respectively the anode and the cathode, and the electrodeposition reaction was carried out with 3M NaOH solution as the electrolyte. 2 The reaction was carried out for 6 min under the current density of 100 Å to form a dark blue copper hydroxide nanowire array precursor;

[0059] Step 3, placing the dark blue copper hydroxide precursor prepared in step 2 in a quartz tube with a diameter of 6 mm, calcining at 100° C. for 4 hours, and heating at a rate of 2° C. / min to obtain a copper oxide nanowire array;

[0060] Step 4, a two-chamber separated electrolytic cell was used, using the copper nanowire array as the working electrode,...

Embodiment 3

[0062] Step 1: The copper sheet (3cm*1cm*0.1mm) was ultrasonicated in acetone and 3.0M HCl solution for 15min respectively, then rinsed with distilled water and ethanol respectively, and dried with cold air in the air for subsequent use;

[0063] In step 2, two copper sheets obtained in step 1 were taken out and placed in a single-chamber reaction cell, respectively the anode and the cathode, and the electrodeposition reaction was carried out with 3M NaOH solution as the electrolyte. 2 The reaction was carried out for 6 min under the current density of 100 Å to form a dark blue copper hydroxide nanowire array precursor;

[0064] Step 3, placing the dark blue copper hydroxide precursor prepared in step 2 in a quartz tube with a diameter of 6 mm, calcining at 250° C. for 2 hours, and heating at a rate of 2° C. / min to obtain a copper oxide nanowire array;

[0065] Step 4, a two-chamber separated electrolytic cell was used, using the copper nanowire array as the working electrode,...

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Abstract

The invention provides an in-situ synthesized copper nanowire array material and its preparation method and application. The copper oxide nanowire array is placed in a separate two-chamber reaction electrolytic cell, and the copper oxide nanowire array is used as a working electrode in an air atmosphere. Mercury / mercury oxide is the reference electrode, the platinum sheet is the counter electrode, and the electrolytic solution is 0.5M K 2 CO 3 A mixed solution of acetonitrile and deuterated water, wherein the volume of acetonitrile accounts for 30-70% of the total volume of the mixed solution, the volume of deuterated water accounts for 30-70% of the total volume of the mixed solution, and the scanning speed is 8-12mV / s, the scanning voltage is in the range of -0.4--1.4V, and the cyclic voltammetry test is carried out until the reduction peak of copper oxide disappears, that is, the in-situ synthesized copper nanowire array material is obtained. The present invention synthesizes the copper nanowire array (Cu NWAs) material by the method of in-situ transformation, takes the copper nanowire array (Cu NWAs) material as the cathode of the electrochemical reaction, utilizes a kind of simple and convenient electrochemical reduction method to deuterate water The efficient conversion of C-X / C-D is realized for the deuterium source.

Description

technical field [0001] The present invention relates to the technical field of electrochemical catalyst materials, and more particularly to an in-situ synthesis of copper nanowire array material and its preparation method and application. Background technique [0002] Since the approval of the first deuterated drugs, research interest in the synthesis of deuterated drugs has grown rapidly. However, precise deuteration with controllable quantity and location remains a great challenge. Due to kinetic isotope effects, deuterium labeling plays a vital role in the synthetic chemistry, materials science and pharmaceutical industries. C-H / C-D exchange is a straightforward strategy to incorporate deuterium without prior functionalization, however C-H / C-D exchange usually requires noble metal catalysts and strong acids / bases to activate C-H bonds, but this method cannot precisely control the position and number of deuterium, and the deuterium Generation rate is not high. In contra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25C1/12B22F1/054C25B1/01C25B3/25C25B11/04C25B3/09C01G3/02B82Y30/00B82Y40/00
CPCC25C1/12C25B1/00C01G3/02B01J23/72B01J35/0033B82Y30/00B82Y40/00B22F1/0547Y02P10/20
Inventor 张兵韩舒艳刘翠波李孟阳
Owner TIANJIN UNIV
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