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A kind of preparation method of composite metal oxide functional electrode

A composite metal and oxide technology, applied in chemical instruments and methods, water pollutants, water/sludge/sewage treatment, etc., can solve problems such as limited loading of cobalt tetroxide, loss of precious metals, complicated preparation steps, etc., and achieve efficient realization Reduction removal, low concentration of intermediate by-products, and broad engineering application prospects

Active Publication Date: 2021-03-19
YANSHAN UNIV
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  • Claims
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Problems solved by technology

[0003] Patent CN 108341467 A discloses a preparation method of Ag / GO / Ti electrode and its application in electrochemical reduction of nitrate, in which a certain proportion of GO and Ag are electroplated on Ti substrate by electrodeposition method to obtain Ag / GO / Ti electrode, which is used as the cathode, and the chlorine analysis electrode is used as the anode, and the nitrate is reduced to nitrogen in the presence of chloride ions, but the removal efficiency of the electrode for high-concentration nitrate is low, and there is no mention of side effects The production of products such as nitrite and ammonium salt; in addition, the electrode uses noble metal Ag as the electrode material, which is expensive, and there is no corresponding recovery step after the electrochemical reaction is completed, which will cause the loss of precious metals
[0004] Patent CN 105198046A mentions a method for removing nitrate in water by a Ti-graphene electrode, which involves immersing the pretreated Ti plate into a graphene oxide solution and drying it naturally to obtain a Ti-graphene electrode. The Pt electrode is used as the anode, the concentration of nitrate nitrogen drops from 50mg / L to 29mg / L, the degradation rate of nitrate is low, and the stability of the electrode prepared by this method is poor, and the thin layer of graphene oxide after repeated electrolysis Easy to fall off
[0005] Patent CN 105858818 A discloses a method for removing nitrate by a Zn / Cu / Ti multi-metal nanoelectrode. The electrode is based on a Ti plate, and a Ti nanolayer is formed on the surface of the Ti plate by a constant voltage anodic oxidation method, and then Cu The nanolayer and Zn nanolayer are electrodeposited on the Ti nanolayer, and the preparation steps are complicated. After the electrochemical reaction, the concentration of nitrate nitrogen still exceeds 15mg / L, and the removal efficiency of nitrate nitrogen is low, and the electrochemical reduction product is mainly ammonia nitrogen.
[0006] In addition, some studies have also reported that cobalt nitrate is coated on the surface of titanium metal, and then cobalt tetroxide is obtained by heat treatment, and the electrochemical reduction treatment of nitrate is realized by using it as the cathode. The concentration of salt by-products is high, and its engineering application efficiency still needs to be improved

Method used

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  • A kind of preparation method of composite metal oxide functional electrode
  • A kind of preparation method of composite metal oxide functional electrode
  • A kind of preparation method of composite metal oxide functional electrode

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Experimental program
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Embodiment 1

[0033] This embodiment provides a method for preparing a composite metal oxide functional electrode, which includes:

[0034] (1) Carbon cloth base pretreatment:

[0035] First, cut out a carbon cloth with a size of 2×2 cm, and then perform ultrasonic cleaning on it with acetone and absolute ethanol to remove surface stains. The ultrasonic cleaning time is 30 minutes, and the power is 90W; the cleaned carbon cloth is rinsed with deionized water 3 times to remove residual acetone and absolute ethanol on the surface; then soak the carbon cloth in 3mol / L nitric acid solution for 12 hours to remove impurities such as inorganic oxides on the surface of the carbon cloth, and then rinse it with deionized water; finally, the carbon cloth Arranged in a vacuum drying oven, vacuum-dry at 60°C for 12 hours, and the vacuum degree is -0.1MPa;

[0036] (2) Co(OH) used in the preparation of functional electrodes 2 / Cu(OH) 2 Precursor preparation:

[0037] ①Chemical raw materials used:

...

Embodiment 2

[0058] This embodiment provides a method for preparing a composite metal oxide functional electrode, which includes:

[0059] (1) Carbon cloth base pretreatment:

[0060] First, cut out a carbon cloth with a size of 2×2 cm, and then perform ultrasonic cleaning on it with acetone and absolute ethanol to remove surface stains. The ultrasonic cleaning time is 40 minutes, and the power is 90W; the cleaned carbon cloth is rinsed with deionized water 3 times to remove residual acetone and absolute ethanol on the surface; then soak the carbon cloth in 3mol / L nitric acid solution for 12 hours to remove impurities such as inorganic oxides on the surface of the carbon cloth, and then rinse it with deionized water; finally, the carbon cloth Arranged in a vacuum drying oven, vacuum-dry at 65°C for 12 hours, and the vacuum degree is -0.1MPa;

[0061] (2) Co(OH) used in the preparation of functional electrodes 2 / Cu(OH) 2 Precursor preparation:

[0062] ①Chemical raw materials used:

...

experiment example

[0075] Experimental procedure is basically consistent with embodiment 1, and difference is:

[0076] (1) The concentration of nitrate nitrogen in the electrolyte solution is 50mg / L, the concentration of sodium sulfate is 0.1g / L, and the concentration of sodium chloride is 2g / L.

[0077] (2) When using the constant current mode to reduce the nitrate in the solution, the cathode current is controlled at 0.08A, and the reduction treatment time is 180min.

[0078] Experimental results: Figure 5 Be CoO / Cu in embodiment 2 2 O functional electrode, Cu 2 Nitrate removal rate and product concentration diagram of O electrode and CoO electrode, CoO / Cu 2 The removal rate of nitrate by O functional electrode is 91.4%, and its performance on nitrate removal is better than that of CoO electrode, Cu 2 O electrode, during the reaction process, the concentration of intermediate products nitrite and ammonium salt first increases and then decreases, and finally decreases to 0.

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Abstract

The invention provides a production method of a composite metal oxide functional electrode. The production method comprises the following steps: dissolving cobalt nitrate hexahydrate, copper nitrate trihydrate and urea in methanol to obtain a precursor solution, impregnating a carbon cloth in the precursor solution, and carrying out a hydrothermal reaction on the mixture of the carbon cloth and the precursor solution at 160-200 DEG C for 2-4 h to obtain an electrode precursor; and calcining the electrode precursor at 250-350 DEG C for 2-4 h to obtain a Co3O4 / CuO electrode loaded on the carboncloth, impregnating and reducing the carbon cloth loaded with the Co3O4 / CuO electrode in a sodium borohydride solution for 5-15 min to obtain a carbon cloth loaded with a CoO / Cu2O functional electrode, and performing vacuum drying. The CoO / Cu2O functional electrode obtained by the production method has the advantages of excellent reduction catalysis performance, efficient realization of reductionremoval of nitrates, low concentration of intermediate byproducts, and wide engineering application prospect.

Description

technical field [0001] The invention relates to a preparation method of a composite metal oxide functional electrode. Background technique [0002] In recent years, with the advancement of science and technology and economic development, people's living standards have been continuously improved, and the process of industrialization has been accelerated. Human activities have damaged the environmental ecosystem to a certain extent, and the impact of nitrate pollution on surface water and groundwater has become increasingly serious. At present, there are three main methods for the removal of nitrate in water: biological method, physical chemical method, and chemical method. Electrochemical reduction of nitrate is the combination of electrochemical technology and catalytic technology, using electrons as reducing agents, and an electrochemical redox reaction occurs under certain conditions, thereby reducing nitrate nitrogen to nitrogen gas. In recent years, electrochemical redu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C02F1/461C02F1/467C02F101/16
CPCC02F1/46109C02F1/4678C02F2001/46142C02F2101/16
Inventor 宋来洲许乔波杨淑琴牛倩倩宋梓陌张晓
Owner YANSHAN UNIV
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