Preparation of electrocatalysis electrode of Nano carbon fiber in use for organic electrochemical synthesis process

A technology of nano-carbon fiber and chemical synthesis, applied in electrolysis process, electrodes, electrolysis organic production, etc., can solve problems such as human health hazards, electrode inactivation, affecting production efficiency and product quality

Inactive Publication Date: 2007-05-09
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, traditionally, heavy metals such as Pb and Cd with high hydrogen evolution overpotential are generally used as electrode materials in organic electrosynthesis, which is harmful

Method used

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  • Preparation of electrocatalysis electrode of Nano carbon fiber in use for organic electrochemical synthesis process

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Experimental program
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Effect test

Embodiment 1

[0022] Weigh 0.1 gram of tubular carbon nanofibers, add water, make the mass percent of the nanocarbon fiber mixed liquid A obtained through ultrasonic dispersion be 25%, weigh 0.25 grams of polytetrafluoroethylene solution with a mass percent of 60%, add 2.25 grams of water , diluted to 6% polytetrafluoroethylene solution B in mass percent. In a water bath at 80°C, put the mixed liquid A into a beaker, and gradually add solution B under vigorous stirring. Continue to stir until a gel forms. Afterwards, the obtained jelly was uniformly coated on the nickel foam, and then pressed into a tablet at 250° C. under a pressure of 5 MPa to prepare a carbon nanofiber electrocatalyst.

[0023] The prepared carbon nanofiber electrocatalyst was embedded in 0.05mol / L Pb(NO 3 ) 2 in solution. The constant potential deposition was carried out under the conditions of a deposition temperature of 25° C. and a potential of −0.85 V (relative to a saturated calomel electrode), and the depositi...

Embodiment 2

[0028] Weigh 1 g of herringbone carbon nanofibers and weigh 0.5 g of polyethylene glycol with a purity of 100% in a ratio of 2:1. Fully mix the carbon nanofibers and polyethylene glycol, press into a tablet under a pressure of 5MPa at room temperature, and then add 0.05mol / L of Pb(AC) 2 in solution. The cyclic voltammetry scan was carried out under the conditions of a temperature of 10°C and a potential range of -0.35--0.95V to deposit metal, and the scan time was 30 minutes. Afterwards, the obtained electrocatalyst electrode was washed with ultrapure water until the pH was neutral.

[0029] Put the obtained carbon nanofiber electrocatalyst electrode into the oxalic acid solution of 0.5mol / L, in the negative electrode in the H-type electrolyzer, with 1500A / m 2 constant current electrolysis. After 6h electrolysis, the average current efficiency is 75%.

Embodiment 3

[0031] Weigh 5 mg plate-type carbon nanofibers and add 1 ml of 0.5 wt% Nafion solution (Dupont Corp.). After ultrasonic dispersion, 10 μL of the mixed liquid was dropped on a glassy carbon electrode with a diameter of 3 mm with a pipette gun, and then dried naturally in an air atmosphere for 1 h, and then placed in 0.05 mol / L Pb(COO) 2 In the solution, constant potential electrodeposition was carried out in the potential range of -0.95V for 5 minutes. Afterwards, the obtained electrocatalyst electrode was washed with ultrapure water until the pH was neutral, and the morphology of the electrode was observed with HRTEM.

[0032] Put the obtained carbon nanofiber electrocatalyst electrode into the electrolyte solution containing 20% ​​acrylonitrile, with 2000A / m 2 The current density of constant current electrolysis is carried out in the cathode of the H-type electrolyzer. After 6h electrolysis, the average current efficiency is 70%.

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Abstract

This invention discloses a method for preparing carbon nanofiber electrode used in organic electrochemical synthesis. The method comprises: immersing carbon nanofibers in a solution containing metal precursor, and electrodepositing metal nanoparticles onto carbon nanofibers to obtain carbon nanofiber electrode. Compared with traditional high hydrogen-evolution overpotential metals such as Pb and Cd, the electrode has such advantages as high current efficiency, high chemical selectivity and low electrolytic tank voltage, and is environmentally friendly.

Description

technical field [0001] The invention relates to a new preparation method of a nano-carbon fiber electrode used in an organic electrochemical synthesis process. Background technique [0002] Organic electrosynthesis, as a method and technology aimed at green synthesis, has made great contributions to the production of basic organic chemical raw materials and fine chemicals. Organic electrosynthesis uses electrons as "reaction reagents", abandons traditional catalysts, and can realize organic synthesis reactions at normal pressure, normal temperature or lower temperature, and low voltage, eliminates pollution from the process itself, and truly realizes green chemistry and green chemical processes . However, traditionally, heavy metals such as Pb and Cd with high hydrogen evolution overpotential are generally used as electrode materials in organic electrosynthesis, which is harmful to human health. Moreover, electrodes such as Pb and Cd are seriously deactivated in industrial...

Claims

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Application Information

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IPC IPC(8): C25B11/12C25B11/06C25B3/00
Inventor 郑俊生张新胜王明霞袁渭康
Owner EAST CHINA UNIV OF SCI & TECH
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