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Iron-containing graphene oxide modified graphite felt electrode and preparation method and application thereof

A graphite felt and graphene technology is applied in the field of graphite felt electrodes modified by iron-containing graphene oxide and its preparation, which can solve the problems of difficulty in guaranteeing stability, narrow pH range, inability to catalyze reduction, etc. The effect of shortening the reaction time and reducing the preparation cost

Active Publication Date: 2022-05-17
CHINA UNIV OF GEOSCIENCES (BEIJING)
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And during use, due to the lack of catalytic sites (often only focus on H 2 o 2 production), Fe(II) cannot be electrocatalytically reduced at the cathode in time, so that the two-electron oxygen reduction (ORR) performance and the acquisition of Fe(II) cannot be considered simultaneously
[0004] Chinese patent CN110862128A discloses a method for preparing an iron disulfide composite graphite felt electrode. This invention can well overcome the problems of narrow pH range of the traditional Fenton reaction, large amount of iron and hydrogen peroxide, and non-renewable problems, but the metal is directly exposed The surface of graphite felt is easily corroded and peeled off, leading to electrode deactivation and subsequent separation problems
Chinese patent CN109244402A discloses a graphene-coated ferric oxide composite electrode material and a preparation method thereof, which proves the protective effect of graphene materials on transition metal materials, and the preparation process is also simpler than Chinese patent CN110862128A, but the method The material is a composite powder material, which is actually an active material on the surface of the electrode and cannot directly use the powder as an electrode, and the contact area of ​​the granular ferric oxide is much smaller than the layered double hydroxide of the flake Fe used in the present invention. matter (Fe II Fe III -LDH), its stability after anchoring is difficult to guarantee

Method used

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  • Iron-containing graphene oxide modified graphite felt electrode and preparation method and application thereof

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preparation example Construction

[0032] The invention provides a kind of preparation method of the graphite felt electrode modified by iron-containing graphene oxide, comprising the following steps:

[0033] (1) immerse graphite felt in concentrated nitric acid and heat to obtain modified graphite felt;

[0034] (2) Fe(NO 3 ) 3 , FeSO 4 , The pore forming agent is dissolved in the graphene oxide solution to obtain a growth solution;

[0035] (3) placing the modified graphite felt in a growth solution for heat treatment to obtain a graphite felt electrode modified with iron-containing graphene oxide.

[0036]In the present invention, the graphite felt is washed and dried before being immersed in concentrated nitric acid. The washing is continuous ultrasonication in ethanol for 13 to 18 minutes, followed by water cleaning for 3 to 4 times, preferably continuous ultrasonication in ethanol for 14 to 4 minutes. 16 minutes, and then washed 3 times with water; the drying is drying in air at 55-65° C. for 10-14 h...

Embodiment 1

[0048] A preparation method for a graphite felt electrode modified with iron-containing graphene oxide, comprising the following steps:

[0049] (1) The electrode was prepared on the basis of graphite felt (160mm×45mm), and the preparation process was carried out in a reactor (effective volume: 450mL). Continuously ultrasonicate the graphite felt in ethanol for 13 minutes, wash it with water for 3 times, and then dry it in the air at 58°C for 11h, then immerse the dried graphite felt in concentrated nitric acid and heat it in a water bath at 98°C for 0.9h to obtain the modified graphite felt;

[0050] (2) After graphene oxide is placed in deionized water for ultrasonic dispersion, sodium dodecylbenzenesulfonate is added to obtain a graphene oxide solution, wherein the concentration of graphene oxide is 1g / L, and the concentration of sodium dodecylbenzenesulfonate Concentration is 0.5g / L, then Fe(NO 3 ) 3 , FeSO 4 1. Urea is dissolved in the graphene oxide solution to obtai...

Embodiment 2

[0053] (1) The electrode was prepared on the basis of graphite felt (160mm×45mm), and the preparation process was carried out in a reactor (effective volume: 450mL). Continuously ultrasonicate the graphite felt in ethanol for 16 minutes, wash it with water for 3 times, and then dry it in the air at 65°C for 14h, then immerse the dried graphite felt in concentrated nitric acid and heat it in a water bath at 100°C for 1.2h to obtain the modified graphite felt;

[0054] (2) After graphene oxide is placed in deionized water for ultrasonic dispersion, sodium dodecylbenzenesulfonate is added to obtain a graphene oxide solution, wherein the concentration of graphene oxide is 1.1g / L, sodium dodecylbenzenesulfonate The concentration is 0.5g / L, then Fe(NO 3 ) 3 , FeSO 4 , (NH 4 ) 2 CO 3 According to the ratio of 0.08:0.14:1, the molar ratio is dissolved in the graphene oxide solution to obtain the growth solution, graphene oxide and (NH 4 ) 2 CO 3 The molar ratio of mass is 1.1...

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Abstract

The invention relates to the technical field of electrode preparation, in particular to an iron-containing graphene oxide modified graphite felt electrode and a preparation method and application thereof. The preparation method of the iron-containing graphene oxide modified graphite felt electrode comprises the following steps: (1) immersing a graphite felt into concentrated nitric acid, and heating to obtain a modified graphite felt; (2) dissolving Fe (NO3) 3.9 H2O, FeSO4. 7H2O and a pore forming agent in the graphene oxide solution to obtain a growth solution; and (3) placing the modified graphite felt in a growth solution, and carrying out heating treatment to obtain the iron-containing graphene oxide modified graphite felt electrode. The graphite felt which is high in mechanical strength, low in price and easy to obtain is adopted as the carrier, the electrode is modified through the one-step hydrothermal method, the problems that Fe is corroded and leached into a solution, and the electrode performance is poor are solved, the reaction time is effectively shortened, the TOC and TN removal efficiency is improved, and the electrode preparation cost and the process operation cost are reduced to the maximum extent.

Description

technical field [0001] The invention relates to the technical field of electrode preparation, in particular to a graphite felt electrode modified with iron-containing graphene oxide, a preparation method and application thereof. Background technique [0002] Electro-Fenton technology can catalyze dissolved oxygen in water at the cathode and generate H in situ through two-electron reduction 2 o 2 , and then decomposed to generate hydroxyl radicals for the degradation of pollutants. This method does not require additional oxidants, does not produce toxic by-products, and is simple to operate, so it has excellent application prospects. The heterogeneous electro-Fenton technology is an environmentally friendly, mild and efficient electro-Fenton technology, which is used to degrade organic pollutants. Meanwhile, heterogeneous electro-Fenton can activate H in situ 2 o 2 Generate hydroxyl radicals, avoiding Fe 2+ release and dependence on pH. [0003] Active cathode material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F1/461C02F1/72
CPCC02F1/46109C02F1/4672C02F2001/46138C02F2305/026Y02E60/50
Inventor 陈男冯传平路望
Owner CHINA UNIV OF GEOSCIENCES (BEIJING)
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