CN115057417A - Preparation of copper nitride nanosheet and application of copper nitride nanosheet in formate electrosynthesis - Google Patents

Preparation of copper nitride nanosheet and application of copper nitride nanosheet in formate electrosynthesis Download PDF

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CN115057417A
CN115057417A CN202210652471.5A CN202210652471A CN115057417A CN 115057417 A CN115057417 A CN 115057417A CN 202210652471 A CN202210652471 A CN 202210652471A CN 115057417 A CN115057417 A CN 115057417A
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copper nitride
formate
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nitride nanosheet
copper
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CN115057417B (en
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徐坤
赵磊
孙啟焦
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Anhui University
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
    • C01B21/0625—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with copper
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    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
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Abstract

The invention discloses a preparation method of copper nitride nanosheets and application thereof in formate electrosynthesis, and relates to the technical field of electrocatalysis, wherein the preparation method of the copper nitride nanosheets comprises the steps of dispersing zinc oxide in a copper nitrate solution, stirring for reaction, centrifugally separating out a solid, washing and drying to obtain a precursor; and then roasting the prepared precursor in an ammonia atmosphere to obtain the two-dimensional copper nitride nanosheet. The two-dimensional copper nitride nanosheet prepared by the method shows higher activity in preparing formate through selective conversion of electro-catalytic methanol, the Faraday efficiency of the formate generated by the two-dimensional copper nitride nanosheet exceeds 90%, and clean and efficient preparation of the formate is realized.

Description

Preparation of copper nitride nanosheet and application of copper nitride nanosheet in formate electrosynthesis
The technical field is as follows:
the invention relates to the technical field of electrocatalysis, in particular to preparation of copper nitride nanosheets and application thereof in formate electrosynthesis.
Background art:
formate is used as a basic organic small molecule and is an indispensable chemical raw material in the actual production of chemical products such as various medicines, leather, dyes, rubber and the like. At present, in the traditional industry, formate is mainly produced by reacting CO and sodium hydroxide at 160-200 ℃ and 1.4-1.8 MPa, and the subsequent step of the scheme still needs complicated purification steps. The formate production scheme has the advantages of high cost, poor finished product quality, severe labor conditions and serious pollution, and is contrary to the current concept of green chemistry. Therefore, it is urgent to develop a formate synthesis method which is clean in the whole process, has no pollution and is simple in process. Considering that methanol has a series of advantages of low price, wide source, convenience in storage and the like, and the maturity of the existing green renewable energy sources (such as wind power generation, hydroelectric power generation and the like), the research and development of the efficient and stable electrocatalyst for realizing the selective electrocatalysis conversion of methanol into formate has important significance.
Transition metal nitrides have triggered great research interest by virtue of their unique electronic structure, high conductivity, excellent chemical and mechanical stability, showing great potential in electrocatalytic reactions. However, bulk transition metal nitrides are generally subject to a limited number of active sites and slow ion kinetics making their final electrochemical performance more common. Designing a nano-sheet structured transition metal nitride with a tailored morphology has proven to be an effective strategy to address these issues, providing a larger specific surface area and a richer number of active sites.
Patent CN 201711275090.5 discloses a method for preparing copper nitride nanocrystals, but it is not ideal to realize the controllable synthesis of copper nitride with specific sheet-like morphology. Patent CN 201210481128.5 discloses a write-once multilayer waveguide optical memory based on copper nitride film and its manufacturing method, patent CN 201310005350.2 discloses a write-once double-sided optical disc based on copper nitride film and its manufacturing method), and patent CN 201310546250.0 discloses a manufacturing method of integrated circuit board based on copper nitride film, these patents are focused on the preparation of thin film copper nitride sample and their respective application fields, but their application range is relatively small. The preparation process provided by the paper ACS Energy Lett.2019,4,3,747-754 still obtains bulk copper nitride, and the two-dimensional nanosheet with high exposed surface atomic percentage has a wide application value.
The invention content is as follows:
the invention aims to solve the technical problem of providing a preparation method of an anti-perovskite copper nitride nanosheet and an application of the anti-perovskite copper nitride nanosheet in formate electrosynthesis, wherein the prepared copper nitride nanosheet shows excellent catalytic activity, conductivity, selectivity and stability, the Faraday efficiency on formate products exceeds more than 90%, and a new thought is hopefully provided for researching and developing a perovskite type catalytic material for organic micromolecule electrochemical conversion while realizing clean and efficient conversion from methanol to formate.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
one of the purposes of the invention is to provide a preparation method of copper nitride nanosheets, which comprises the following steps:
(1) dispersing zinc oxide in a copper nitrate solution, stirring for reaction, centrifugally separating out solids, washing and drying to obtain a precursor;
(2) and roasting the prepared precursor in an ammonia atmosphere to obtain the two-dimensional copper nitride nanosheet.
In the step (1), the concentration of the copper nitrate solution is 0.01-1 mol/L, and the molar ratio of zinc oxide to copper nitrate is 1 (5-20).
In the step (2), the roasting temperature is 250-450 ℃, and the roasting time is 1-5 hours.
In the step (2), the particle diameter of the two-dimensional copper nitride nanosheet is 200-500 nm.
Step (1) synthesizes Cu according to Le Chatelier principle 2 (OH) 3 NO 3 The nanosheet precursor is characterized in that in the synthesis of the precursor, nitrate ions can be captured by copper ions and hydroxide ions released slowly to form Cu 2 (OH) 3 NO 3 Precipitation, in which zinc oxide is dispersed in water to provide hydroxide ions.
And (2) preparing the two-dimensional copper nitride nanosheet based on a precursor morphology guiding strategy.
The second purpose of the invention is to provide the copper nitride nanosheet prepared according to the preparation method.
The invention also aims to provide the application of the copper nitride nanosheet in preparing formate through electrocatalytic methanol conversion.
The invention has the beneficial effects that:
compared with the prior art, the invention provides the preparation method of the specific two-dimensional flaky copper nitride nanocrystal, and the controllable flaky morphology of the specific two-dimensional flaky copper nitride nanocrystal enables the specific two-dimensional flaky copper nitride nanocrystal to have a wider application prospect; meanwhile, the provided two-dimensional copper nitride nanosheet shows higher activity in preparation of formate through selective conversion of electrocatalytic methanol, the Faraday efficiency of the generated formate exceeds 90%, compared with the existing formate preparation scheme, the process avoids severe and harsh environment in formate preparation, eliminates emission of greenhouse gases such as carbon dioxide and harmful substances in the production process, and realizes clean and efficient preparation of formate.
Description of the drawings:
fig. 1 shows the structural characterization results of the precursor prepared in example 1 of the present invention: (a) an X-ray diffraction pattern; (b) scanning an electron microscope image; (c) an elemental analysis chart;
FIG. 2 shows Cu prepared in example 1 of the present invention 3 And (3) structural characterization results of the N nanosheets: (a) an X-ray diffraction pattern; (b) scanning an electron microscope image; (c) a transmission electron microscope image; (d) high resolution transmission electron microscopy images; (e) an elemental analysis chart;
FIG. 3 shows Cu prepared in example 1 of the present invention 3 The performance test result of the N nano sheet in preparing the formate through electro-catalysis methanol conversion is as follows: (a) linear sweep voltammetry curves in methanol electrolyte with or without 1 mol/L; (b) the required potential under different current densities is achieved; (c) analyzing the ion chromatography of the electrolyte product; (d) faraday efficiency of formate generation at different potentials; (e) a time current curve of 12 h; (f) multiple voltage step curves.
The specific implementation mode is as follows:
in order to make the technical means, the original characteristics, the achieved purposes and the effects of the invention easy to understand, the invention is further explained by combining the specific embodiments and the drawings.
Example 1
Preparing copper nitride nanosheets:
(1) 50mg of ZnO was dispersed in 50mL of 0.1M Cu (NO) 3 ) 2 And (3) in the solution, performing ultrasonic treatment to uniformly disperse the solution, performing magnetic stirring for 24 hours, performing centrifugal separation to obtain a solid, washing the solid with ultrapure water for three times, washing the solid with ethanol for one time, and drying the solid in a vacuum drying oven at 60 ℃ for 24 hours to obtain a precursor.
The precursor was subjected to structural characterization, and the results are shown in fig. 1.
FIG. 1(a) shows diffraction peaks of precursor and Cu 2 (OH) 3 NO 3 The cards are matched, so that the successful preparation of the target precursor is realized; FIG. 1(b) shows that the precursor is a two-dimensional sheet-like morphology with a length of about 400 nm; fig. 1(c) shows that the Cu element, the N element, and the O element are uniformly distributed in the precursor.
(2) Placing the prepared precursor into a quartz boat, placing the quartz boat into a tubular calcining furnace, heating the quartz boat to 300 ℃ from room temperature at the heating rate of 10 ℃/min in the ammonia atmosphere, maintaining the temperature for 2 hours, and naturally cooling the quartz boat to the room temperature to obtain Cu 3 And (4) N samples.
For Cu 3 The N samples were subjected to structural characterization, and the results are shown in fig. 2.
Cu in FIG. 2(a) 3 All the diffraction peaks of the N sample are corresponding to pure cubic Cu one by one 3 N diffraction peak, thereby proving that the invention realizes pure Cu 3 Successfully preparing N; FIGS. 2(b) and 2(c) show Cu 3 The N sample substantially retained the nanosheet morphology of the precursor, with a diameter of about 400 nm. Furthermore, it is worth noting that Cu compares to the precursor 3 The N sample has a rougher surface, and can provide more active centers in subsequent catalytic reaction; FIG. 2(d) shows that the lattice spacing at 0.22nm corresponds to cubic Cu 3 The (111) crystal face of N; FIG. 2(e) shows that Cu and N are present in Cu 3 And N is uniformly distributed in the sample.
The results prove that the Cu is successfully prepared and obtained based on the Le Chatelier's principle and the precursor morphology guiding strategy 3 N nano-sheet.
Example 2
Cu prepared in example 1 3 N sample asApplication study of the catalyst in electrocatalytic methanol conversion:
electrocatalytic testing of methanol conversion was performed on an electrochemical workstation using a standard three-electrode system. Takes 1M potassium hydroxide solution containing 1M methanol and not containing methanol as electrolyte to modify Cu 3 The glassy carbon electrode of the N catalyst is used as a working electrode (5 mg of Cu is added 3 Dispersing the N catalyst into 500 mu L ethanol containing 10uL of 5 wt% Nafion, and preparing Cu by ultrasonic treatment for 1h 3 N printing ink; then 10. mu.L of Cu 3 Dropping N ink onto the polished glassy carbon electrode to obtain a working electrode), using a carbon rod as a counter electrode and using an Hg/HgO electrode as a reference electrode.
As shown in FIG. 3a, Cu was present in two 1M KOH solutions containing 1M methanol and no methanol, respectively 3 The polarization curves of the N samples were significantly different. Wherein, Cu 3 The N electrode shows conventional electrocatalytic performance in 1M KOH electrolyte and reaches 10mA cm under 1.64V vs. RHE -2 The current density of (1). In contrast, this potential requirement was significantly reduced to 1.35V upon addition of 1M methanol. Further comparison data shows that in FIG. 3b, the current densities reached 30, 60, 90 and 120mA cm, respectively, compared to water oxidation -2 The potential of the methanol oxidation reaction was decreased by 334, 368, 402 and 431mV, respectively.
The methanol oxidation product formate was then tested at different potentials using ion chromatography (FIG. 3c) and calculations revealed that faradaic efficiencies exceeded 90% over the potential range of 1.4-1.8V vs. RHE (FIG. 3d), indicating Cu-and that 3 The N sample showed very high electrochemical selectivity in the electrocatalytic methanol oxidation reaction.
Applying chronopotentiometry to Cu 3 The electrochemical stability test of the N sample shows that the current density generated in 12h is hardly attenuated (FIG. 3e), and the multi-potential transition curve (FIG. 3f) further shows that the Cu is added 3 The N sample has extremely high electrochemical stability in the electrocatalytic methanol oxidation reaction.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (6)

1. A preparation method of copper nitride nanosheets is characterized by comprising the following steps:
(1) dispersing zinc oxide in a copper nitrate solution, stirring for reaction, centrifugally separating out solids, washing, and drying to obtain a precursor;
(2) and roasting the prepared precursor in an ammonia atmosphere to obtain the two-dimensional copper nitride nanosheet.
2. The method of claim 1, wherein: in the step (1), the concentration of the copper nitrate solution is 0.01-1 mol/L, and the molar ratio of zinc oxide to copper nitrate is 1 (5-20).
3. The method of claim 1, wherein: in the step (2), the roasting temperature is 250-450 ℃, and the roasting time is 1-5 hours.
4. The method of claim 1, wherein: in the step (2), the particle diameter of the two-dimensional copper nitride nanosheet is 200-500 nm.
5. Copper nitride nanosheets produced by the production method according to any one of claims 1 to 4.
6. Use of copper nitride nanoplates as described in claim 5 in the preparation of formate salts by electrocatalytic conversion of methanol.
CN202210652471.5A 2022-06-08 2022-06-08 Preparation of copper nitride nano-sheet and application of copper nitride nano-sheet in formate electrosynthesis Active CN115057417B (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102211763A (en) * 2011-04-14 2011-10-12 中国科学院长春应用化学研究所 Method for preparing copper nitride nano crystalline
CN102491290A (en) * 2011-12-12 2012-06-13 沈阳化工大学 Method for preparing copper nitride powder
WO2014119748A1 (en) * 2013-01-31 2014-08-07 独立行政法人産業技術総合研究所 Fine copper nitride particles and production method therefor
CN108063249A (en) * 2017-12-06 2018-05-22 江汉大学 A kind of preparation method of high-purity copper nitride nano crystalline
CN109499495A (en) * 2018-12-13 2019-03-22 吉林大学 A kind of zinc oxide/hydroxide aeroge and preparation method thereof
CN110102325A (en) * 2018-12-26 2019-08-09 武汉理工大学 Porous nano chip architecture cupro-nickel nitride material and its preparation method and application
CN111450867A (en) * 2020-05-09 2020-07-28 青岛科技大学 Cu for electrocatalytic carbon dioxide reduction3Preparation method of N nano catalyst
CN113136598A (en) * 2021-04-26 2021-07-20 华电重工股份有限公司 Carbon-supported nickel-zinc nitride bifunctional catalyst and preparation method and application thereof
WO2021243971A1 (en) * 2020-06-03 2021-12-09 深圳先进技术研究院 Composite nanomaterial, preparation method therefor and catalyst

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102211763A (en) * 2011-04-14 2011-10-12 中国科学院长春应用化学研究所 Method for preparing copper nitride nano crystalline
CN102491290A (en) * 2011-12-12 2012-06-13 沈阳化工大学 Method for preparing copper nitride powder
WO2014119748A1 (en) * 2013-01-31 2014-08-07 独立行政法人産業技術総合研究所 Fine copper nitride particles and production method therefor
CN108063249A (en) * 2017-12-06 2018-05-22 江汉大学 A kind of preparation method of high-purity copper nitride nano crystalline
CN109499495A (en) * 2018-12-13 2019-03-22 吉林大学 A kind of zinc oxide/hydroxide aeroge and preparation method thereof
CN110102325A (en) * 2018-12-26 2019-08-09 武汉理工大学 Porous nano chip architecture cupro-nickel nitride material and its preparation method and application
CN111450867A (en) * 2020-05-09 2020-07-28 青岛科技大学 Cu for electrocatalytic carbon dioxide reduction3Preparation method of N nano catalyst
WO2021243971A1 (en) * 2020-06-03 2021-12-09 深圳先进技术研究院 Composite nanomaterial, preparation method therefor and catalyst
CN113136598A (en) * 2021-04-26 2021-07-20 华电重工股份有限公司 Carbon-supported nickel-zinc nitride bifunctional catalyst and preparation method and application thereof

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