CN112237927B - Catalyst for electrocatalytic reduction of nitrate as well as preparation method and application thereof - Google Patents

Catalyst for electrocatalytic reduction of nitrate as well as preparation method and application thereof Download PDF

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CN112237927B
CN112237927B CN202011032642.1A CN202011032642A CN112237927B CN 112237927 B CN112237927 B CN 112237927B CN 202011032642 A CN202011032642 A CN 202011032642A CN 112237927 B CN112237927 B CN 112237927B
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nickel
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CN112237927A (en
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周凤玲
孙成华
李勤干
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Dongguan University of Technology
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    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/12—Oxidising
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    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
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    • C02F2101/10—Inorganic compounds
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Abstract

The invention relates to the technical field of catalyst preparation, in particular to a method for preparing a catalyst for electrocatalytic reduction of nitrate, which comprises the following steps: forming a nickel oxide layer on the surface of foam nickel by taking the foam nickel as a substrate to obtain a compound; and adopting ruthenium trichloride solution, and adopting electrochemical cyclic voltammetry to deposit ruthenium nano particles on the compound to obtain the Ni-Ru composite catalyst. The invention provides a preparation method of a catalyst for electrocatalytic reduction of nitrate, which has the advantages of simple preparation method process, low Ru load of the catalyst and low catalyst cost; the invention also provides application of the catalyst for electrocatalytic reduction of nitrate, which has higher current density, current Faraday efficiency and nitrate elimination rate of synthetic ammonia in a wide voltage range.

Description

Catalyst for electrocatalytic reduction of nitrate as well as preparation method and application thereof
Technical Field
The invention relates to the technical field of catalyst preparation, in particular to a catalyst for electrocatalytic reduction of nitrate, and a preparation method and application thereof.
Background
In industrial processes, most industries produce nitrates directly or indirectly, for example: ammonia waste discharged from factories such as foods, fuel oil refining and the like is biologically and chemically converted to form nitrate; a large amount of nitrogen oxides generated in the combustion process of a thermal power plant, an automobile, a ship and the like are leached by precipitation to form nitrate; ammonium nitrate, calcium nitrate, potassium nitrate, sodium nitrate and urea and the like which are rich in the artificial fertilizer and the fuel of textile industry; nitric acid generated in the processes of acid washing, deplating, etching and the like in the electroplating industry. Nitrate is very soluble in water and is relatively stable and less prone to co-precipitation and adsorption, and therefore conventional water treatment techniques are not suitable for nitrate removal.
The conventional nitrate removal method mainly comprises a reverse osmosis method, an electrodialysis method, an ion exchange method, a catalytic denitrification method, a chemical denitrification method and a biological denitrification method. The reverse osmosis method, the electrodialysis method and the ion exchange method have the problems of high cost and low efficiency of the biological denitrification method. By electrochemical means, the reduction of nitric acid to ammonia under catalysis not only removes nitric acid, but also generates valuable ammonia. In the research of synthesizing ammonia by electrochemical catalytic reduction of nitric acid, ru-based catalyst has the highest performance. The preparation method comprises the steps of firstly preparing amorphous ruthenium oxychloride by an improved sol-gel method, then dripping the amorphous ruthenium oxychloride on a carbon paper substrate by a titration method, reducing the ruthenium oxychloride by electrochemical reduction, and finally reducing the amorphous ruthenium oxychloride in H 2 And heat-treating in the atmosphere for 6h. It can be seen that the method has the problem of complicated preparation procedures. And because the catalyst adopts a dripping method, the binding force between the catalyst and the carbon paper is poor, and the catalyst can run for a long time, so that the problem of insufficient stability can occur. In addition, because the carbon paper substrate is adopted, the substrate conductivity is not high, and the problem that the current collection effect is poor and the reaction can not be carried out under high current for a long time exists. (journal of the American chemical society,2020.142 (15): p.7036-7046.). Other catalysts include Cu-based, ti-based, and Co-based catalysts, but all have lower catalytic properties than Ru. In addition, ru is a noble metal, and there is a problem that the catalyst cost is high.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a catalyst for electrocatalytic reduction of nitrate, which has the advantages of simple preparation method process, low Ru loading amount of the catalyst and low catalyst cost.
The invention also provides application of the catalyst for electrocatalytic reduction of nitrate, which has higher current density, current Faraday efficiency and nitrate elimination rate of synthetic ammonia in a wide voltage range.
The invention adopts the following technical scheme:
a preparation method of a catalyst for electrocatalytic reduction of nitrate comprises the following steps:
forming a nickel oxide layer on the surface of foam nickel by taking the foam nickel as a substrate to obtain a compound;
and adopting ruthenium trichloride solution, and adopting electrochemical cyclic voltammetry to deposit ruthenium nano particles on the compound to obtain the Ni-Ru composite catalyst.
The technical scheme is further improved that in the step of forming a nickel oxide layer on the surface of the foam nickel by taking the foam nickel as a substrate to obtain a compound, the nickel oxide layer is obtained by performing heat treatment on the surface of the foam nickel in the air.
The technical scheme is further improved in that the temperature of the heat treatment is between room temperature and 700 ℃, and the atmosphere of the heat treatment is air atmosphere.
The technical scheme is further improved in that the content of ruthenium trichloride is 0.01-5 g/L, and the pH range is 0-14.
The technical scheme is further improved that in the step of adopting ruthenium trichloride solution to deposit ruthenium nano particles on a compound by adopting electrochemical cyclic voltammetry to obtain the Ni-Ru composite catalyst, the electrochemical cyclic voltammetry comprises the following steps:
a three-electrode electrochemical system is adopted, foam nickel with a nickel oxide layer is used as a working electrode, and cyclic voltammetry scanning is adopted on the working electrode.
The technical scheme is further improved that in the step of adopting a three-electrode electrochemical system and adopting foamed nickel with a nickel oxide layer as a working electrode and adopting cyclic voltammetry scanning on the working electrode, the voltage range is-1.0V-0.1V (vs RHE).
The technical scheme is further improved that in the step of adopting a three-electrode electrochemical system, taking foam nickel with a nickel oxide layer as a working electrode and adopting cyclic voltammetry scanning on the working electrode, the scanning speed is 1-100 mV/s.
The technical scheme is further improved in that in the step of adopting a three-electrode electrochemical system and adopting foamed nickel with a nickel oxide layer as a working electrode and adopting cyclic voltammetry scanning on the working electrode, the number of times of cyclic voltammetry scanning is 1-100 times, and the number of times of cyclic voltammetry scanning is controlled by an electrochemical workstation.
The catalyst for electrocatalytic reduction of nitrate is prepared by the preparation method.
The application of a catalyst for electrocatalytic reduction of nitrate in synthesizing ammonia by electrochemical catalytic reduction of nitrate.
The beneficial effects of the invention are as follows:
in the first aspect, the preparation method has simple process, adopts foam nickel as a substrate, provides high electrochemical activity surface area for electrochemical reaction, introduces an oxide layer on the surface of the foam nickel, and effectively improves the catalytic performance of the catalyst on nitrate reduction; in the second aspect, an electrochemical cyclic voltammetry is adopted to deposit a catalyst, so that the catalyst with small-size nano particle size can be synthesized, and the content of deposited ruthenium and the content of ruthenium oxide can be regulated and controlled by regulating the circulation times in the electrochemical deposition process; in the third aspect, the Ru loading of the catalyst can be as low as 0.15wt%, so that the cost of the catalyst is effectively reduced; simultaneously has higher current density, current Faraday efficiency and ammonia synthesis elimination rate in a wide voltage range, and the obtained catalyst is directly used for electrochemical reduction of nitrate, and can obtain up to 110mAcm at low voltage -2 The ammonia synthesis efficiency is up to 100% and the yield is up to 1.4x10 -7 mol -1 s -1 cm -1 The method comprises the steps of carrying out a first treatment on the surface of the Over a wide voltage range, i.e. -1.0V-0V (vs RHE), the current efficiency of synthesizing ammonia can be maintained up to 100%, and the ammonia yield and nitrate radical elimination rate can be up to 1.56x10 -6 mol -1 s -1 cm -1 。
Drawings
FIG. 1 is a schematic diagram of the preparation principle of the method for preparing a catalyst for electrocatalytic reduction of nitrate and the synthesis of ammonia by catalytic reduction of nitric acid;
FIG. 2 is a plot of current versus voltage for the electrodeposition process of the catalyst preparation method of FIG. 1 for electrocatalytically reducing nitrates;
FIG. 3 is an electron micrograph, raman and XPS spectra of the catalyst of FIG. 1 for electrocatalytically reducing nitrates;
FIG. 4 is a schematic illustration of the catalytic performance of the catalyst of FIG. 1 for electrocatalytic reduction of nitrates;
FIG. 5 is a graph of performance of an application of the catalyst for electrocatalytic reduction of nitrates of the present invention;
FIG. 6 is another performance graph of an application of the catalyst of the present invention for electrocatalytically reducing nitrates.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below in connection with the embodiments of the present invention.
As shown in fig. 1 to 6, a method for preparing a catalyst for electrocatalytically reducing nitrate, comprising the steps of:
forming a nickel oxide layer on the surface of foam nickel by taking the foam nickel as a substrate to obtain a compound; and adopting ruthenium trichloride solution, and adopting electrochemical cyclic voltammetry to deposit ruthenium nano particles on the compound to obtain the Ni-Ru composite catalyst. The foam nickel is used as a substrate to provide high electrochemical activity surface area for electrochemical reaction; and an oxide layer is introduced on the surface of the foam nickel, so that the catalytic performance of the catalyst on nitrate reduction is effectively improved.
Forming a nickel oxide layer on the surface of foam nickel by taking the foam nickel as a substrate to obtain a compound, wherein the nickel oxide layer is obtained by performing heat treatment on the surface of the foam nickel in air; the temperature of the heat treatment is between room temperature and 700 ℃, and the atmosphere of the heat treatment is air atmosphere.
Preferably, the heat treatment temperature is room temperature to 300 ℃, and the heat treatment time is 30 minutes.
Ruthenium trichloride is added, and the content of the ruthenium trichloride is 0.01-5 g/L and the pH range is 0-14 in the process of adopting an electrochemical deposition catalyst.
Preferably, the ruthenium trichloride content is 2g/L and the pH is 0.
In the step of adopting ruthenium trichloride solution to deposit ruthenium nano particles on the compound by adopting electrochemical cyclic voltammetry to obtain the Ni-Ru composite catalyst, the electrochemical cyclic voltammetry comprises the following steps:
a three-electrode electrochemical system is adopted, foam nickel with a nickel oxide layer is used as a working electrode, and cyclic voltammetry scanning is adopted on the working electrode. The electrochemical cyclic voltammetry is adopted to deposit the catalyst, which is helpful for synthesizing the catalyst with small-sized nanometer particle size.
In the step of using a three-electrode electrochemical system, using foamed nickel with a nickel oxide layer as a working electrode, and using cyclic voltammetry scanning on the working electrode, the voltage range is-1.0V-0.1V (vs RHE).
Preferably, the electrochemical deposition cycle scans a voltage in the range of-0.6V to 0.1V (vs RHE).
In the step of adopting a three-electrode electrochemical system and adopting foamed nickel with a nickel oxide layer as a working electrode and adopting cyclic voltammetry scanning on the working electrode, the scanning speed is 1-100 mV/s.
In the step of adopting a three-electrode electrochemical system and adopting foamed nickel with a nickel oxide layer as a working electrode and adopting cyclic voltammetry scanning on the working electrode, the number of times of cyclic voltammetry scanning is 1-100 times, and the number of times of cyclic voltammetry scanning is controlled by an electrochemical workstation. The content of deposited ruthenium and the content of ruthenium oxide can be regulated and controlled by regulating the circulation times in the electrochemical deposition process.
The catalyst for electrocatalytic reduction of nitrate is prepared by the preparation method.
The application of a catalyst for electrocatalytic reduction of nitrate in synthesizing ammonia by electrochemical catalytic reduction of nitrate. Can obtain a voltage of up to 110mAcm at low voltage -2 The ammonia synthesis efficiency is up to 100% and the yield is up to 1.4x10 -7 mol -1 s - 1 cm -1 The method comprises the steps of carrying out a first treatment on the surface of the In a wide voltage range, i.e. -1.0V-0V (vs RHE), the current efficiency of synthesizing ammonia can be maintained up to 100%, and the ammonia yield and nitrate elimination rate can be up to 1.56x10 -6 mol -1 s -1 cm -1 。
As shown in figures 1 to 6, the preparation method of the invention has simple process, the Ru load of the catalyst can be as low as 0.15wt%, the cost of the catalyst is effectively reduced, and the catalyst has higher current density, current conversion efficiency and nitrate radical elimination rate of synthetic ammonia in a wide voltage range.
The foregoing examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (6)

1. The application of the catalyst for electrocatalytic reduction of nitrate in the aspect of synthesizing ammonia by electrochemically catalyzing and reducing nitrate is characterized in that the preparation method of the catalyst for electrocatalytic reduction of nitrate comprises the following steps:
forming a nickel oxide layer on the surface of foam nickel by taking the foam nickel as a substrate to obtain a compound;
depositing ruthenium nano particles on the compound by adopting a ruthenium trichloride solution and adopting an electrochemical cyclic voltammetry to obtain a Ni-Ru composite catalyst;
the electrochemical cyclic voltammetry comprises the following steps:
adopting a three-electrode electrochemical system, taking foam nickel with a nickel oxide layer as a working electrode, and adopting cyclic voltammetry scanning on the working electrode;
in the step of adopting a three-electrode electrochemical system and adopting foam nickel with a nickel oxide layer as a working electrode and adopting cyclic voltammetry scanning on the working electrode, the voltage range is-1.0V-0.1V vs RHE;
at low voltage up to 110mAcm -2 The ammonia synthesis efficiency is up to 100% and the yield is up to 1.4x10 -7 mol -1 s -1 cm -1 The method comprises the steps of carrying out a first treatment on the surface of the In a wide voltage range, namely-1.0V-0V vs RHE, the current efficiency of synthesizing ammonia can be maintained to be up to 100%, and the ammonia yield and nitrate elimination rate can be up to 1.56x10 -6 mol -1 s -1 cm -1 。
2. The use of the catalyst for electrocatalytic reduction of nitrate according to claim 1 for electrochemical catalytic reduction of nitrate synthesis ammonia, wherein in the step of forming a nickel oxide layer on the surface of the nickel foam with the nickel foam as a substrate to obtain a composite, the nickel oxide layer is obtained by heat-treating the air on the surface of the nickel foam.
3. The use of the catalyst for electrocatalytic reduction of nitrate according to claim 2, wherein the temperature of the heat treatment is room temperature to 700 ℃, and the atmosphere of the heat treatment is an air atmosphere.
4. The use of the catalyst for electrocatalytic reduction of nitrate according to claim 1, wherein the content of ruthenium trichloride is 0.01-5 g/L and the pH range is 0-14.
5. The use of the electrocatalytic reduction nitrate catalyst according to claim 1, wherein in the step of using a three-electrode electrochemical system, using foam nickel with a nickel oxide layer as a working electrode and using cyclic voltammetry scanning on the working electrode, the scanning speed is 1-100 mv/s.
6. The use of the catalyst for electrocatalytic reduction of nitrate according to claim 5, wherein in the step of using a three-electrode electrochemical system, foamed nickel with nickel oxide layer as a working electrode and cyclic voltammetry scanning on the working electrode, the number of cyclic voltammetry scanning is 1-100, and the number of cyclic voltammetry scanning is controlled by an electrochemical workstation.
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CN113005469B (en) * 2021-01-27 2022-04-08 浙江大学衢州研究院 Ruthenium-loaded amorphous nickel hydroxide/nickel phosphide composite electrode and preparation method and application thereof
CN112981451B (en) * 2021-02-07 2022-02-18 安徽农业大学 Preparation method of catalytic electrode for preparing ammonia by electrochemical reduction of nitrate or nitrite
CN113403633B (en) * 2021-05-10 2022-05-10 杭州师范大学 Preparation method of Cu-C-N metal organic framework electrocatalyst for reducing nitrate into ammonia
CN113668001A (en) * 2021-07-27 2021-11-19 北京化工大学 Method for synthesizing ammonia by electrocatalysis nitrate radical reduction using hydrogen evolution reaction catalyst
CN113637989B (en) * 2021-08-10 2023-07-07 湖南大学 Method for synthesizing ammonia by electrocatalytic nitrate or nitrite
CN114574895B (en) * 2022-03-18 2023-06-20 南京师范大学 Ru-NiO hydrogen evolution reaction catalyst loaded by foam nickel and preparation method thereof
CN116083952B (en) * 2023-03-28 2023-06-13 西南石油大学 Cu (copper) alloy 3 Ti nano-sheet loaded Ti-doped CuO/Ru hydrogen evolution reaction catalyst and preparation method thereof

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