CN115057417B - Preparation of copper nitride nano-sheet and application of copper nitride nano-sheet in formate electrosynthesis - Google Patents
Preparation of copper nitride nano-sheet and application of copper nitride nano-sheet in formate electrosynthesis Download PDFInfo
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- CN115057417B CN115057417B CN202210652471.5A CN202210652471A CN115057417B CN 115057417 B CN115057417 B CN 115057417B CN 202210652471 A CN202210652471 A CN 202210652471A CN 115057417 B CN115057417 B CN 115057417B
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- C01—INORGANIC CHEMISTRY
- 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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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
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- 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
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Abstract
The invention discloses a preparation method of a copper nitride nano-sheet and application thereof in formate electrosynthesis, and relates to the technical field of electrocatalysis, wherein the preparation method of the copper nitride nano-sheet comprises the steps of dispersing zinc oxide in a copper nitrate solution, stirring for reaction, centrifugally separating out solids, washing and drying to obtain a precursor; and then roasting the prepared precursor in an ammonia atmosphere to obtain the two-dimensional copper nitride nano-sheet. The two-dimensional copper nitride nano-sheet prepared by the invention has higher activity in preparing formate by electrocatalytic methanol selective conversion, the Faraday efficiency of formate generation exceeds 90%, and clean and efficient preparation of formate is realized.
Description
Technical field:
the invention relates to the technical field of electrocatalysis, in particular to preparation of a copper nitride nano-sheet and application thereof in formate electrosynthesis.
The background technology is as follows:
formate is taken as a basic organic micromolecule and is an indispensable chemical raw material in the actual production of various chemical products such as medicines, leather, dyes, rubber and the like. At present, the formate is produced mainly by the reaction of CO and sodium hydroxide at 160-200 ℃ and 1.4-1.8 MPa in the traditional industry, and the subsequent purification steps of the scheme still need to be complicated. The formate production scheme has high cost, poor quality of finished products, severe labor conditions and serious pollution, and is contrary to the current concept of green chemistry. Therefore, the development of a formate synthesis method with clean and zero pollution in the whole process and simple process becomes urgent. Considering a series of advantages of low price, wide sources, convenient storage and the like of the methanol, and the maturity of the existing green renewable energy sources (such as wind power generation, hydroelectric generation and the like), the development of an efficient and stable electrocatalyst for realizing the selective electrocatalytic conversion of the methanol into formate has important significance.
Transition metal nitrides have attracted 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 affected by a limited number of active sites and slow ion kinetics, making their final electrochemical performance more common. Designing nanosheet structured transition metal nitrides with tailored morphology has proven to be an effective strategy to address these issues, which can provide larger specific surface areas and richer active sites.
Patent CN 201711275090.5 discloses a method for preparing copper nitride nanocrystals, but it is not ideal to achieve controlled synthesis of copper nitride with specific platelet morphology. Patent CN 201210481128.5 discloses a write-once type multi-layer waveguide optical memory based on a copper nitride film and a manufacturing method thereof, patent CN 201310005350.2 discloses a write-once type double-sided optical disk based on a copper nitride film and a manufacturing method thereof, and patent CN 201310546250.0 discloses a manufacturing method of an integrated circuit board based on a copper nitride film, wherein the patents focus on the preparation and respective application fields of a film copper nitride sample, but the application range is relatively small. The preparation process provided by ACS Energy Lett.2019,4,3,747-754 still provides blocky copper nitride, and the two-dimensional nano-sheet with high exposed surface atomic percent has wider application value.
The invention comprises the following steps:
the invention aims to solve the technical problem of providing the preparation of the copper nitride nano-sheet with the anti-perovskite structure and the application of the copper nitride nano-sheet in formate electrosynthesis, wherein the prepared copper nitride nano-sheet shows excellent catalytic activity, conductivity, selectivity and stability, has Faraday efficiency of over 90 percent for formate products, and is expected to provide a new thought for developing perovskite catalytic materials for electrochemical conversion of small organic molecules while realizing clean and efficient conversion of methanol to formate.
The technical problems to be solved by the invention are realized by adopting the following technical scheme:
the invention aims at providing a preparation method of a copper nitride nano sheet, which comprises the following steps:
(1) Dispersing zinc oxide in a copper nitrate solution, stirring for reaction, centrifugally separating out solid, washing and drying to obtain a precursor;
(2) And roasting the prepared precursor in an ammonia atmosphere to obtain the two-dimensional copper nitride nano-sheet.
In the step (1), the concentration of the copper nitrate solution is 0.01-1 mol/L, and the mol ratio of zinc oxide to copper nitrate is 1 (5-20).
In the step (2), the roasting temperature is 250-450 ℃ and the time is 1-5 h.
In the step (2), the particle size of the two-dimensional copper nitride nano-sheet is 200-500nm.
Step (1) Cu is synthesized according to the LeChatelier principle 2 (OH) 3 NO 3 Nanosheet precursor, wherein during the synthesis of the precursor, copper ions can capture nitrate ions and slowly released hydroxide ions to form Cu 2 (OH) 3 NO 3 Precipitation, wherein zinc oxide is dispersed in water to provide hydroxide ions.
And (2) preparing the two-dimensional copper nitride nano-sheet based on a precursor shape guiding strategy.
The second object of the present invention is to provide a copper nitride nano-sheet prepared by the aforementioned preparation method.
The invention further aims to provide an application of the copper nitride nano-sheet in preparing formate by electrocatalytic methanol conversion.
The beneficial effects of the invention are as follows:
compared with the prior art, the invention provides a preparation method of a specific two-dimensional flaky copper nitride nanocrystal, which has controllable flaky morphology and wider application prospect; meanwhile, the provided two-dimensional copper nitride nano-sheet shows higher activity in preparing formate by electrocatalytic methanol selective conversion, and the Faraday efficiency of generating formate is over 90 percent.
Description of the drawings:
FIG. 1 shows the structural characterization result of the precursor prepared in example 1 of the present invention: (a) an X-ray diffraction pattern; (b) scanning electron microscopy images; (c) an elemental analysis map;
FIG. 2 shows Cu prepared in example 1 of the present invention 3 Structural characterization results for N nanoplatelets: (a) an X-ray diffraction pattern; (b) scanning electron microscopy images; (c) a transmission electron microscope image; (d) high resolution transmission electron microscopy; (e) elemental analysis map;
FIG. 3 shows Cu prepared in example 1 of the present invention 3 Performance test results of N nanoplatelets in electrocatalytic methanol conversion to formate: (a) Linear sweep voltammetry curves in methanol electrolyte with or without 1 mol/L; (b) achieving the desired potential at different current densities; (c) ion chromatography of the electrolyte product; (d) Faraday efficiency of formate formation at different potentials; (e) a time current profile of 12 h; (f) a multiple voltage step curve.
The specific embodiment is as follows:
the invention is further described below with reference to specific embodiments and illustrations in order to make the technical means, the creation features, the achievement of the purpose and the effect of the implementation of the invention easy to understand.
Example 1
Preparation of copper nitride nano-sheets:
(1) 50mg ZnO was weighed and dispersed in 50mL of 0.1M Cu (NO) 3 ) 2 In the solution, uniformly dispersing the solution by ultrasonic, magnetically stirring the solution for 24 hours, centrifugally separating out solid, washing the solid by using ultrapure water for three times, washing the solid by using 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 structurally characterized, and the result is shown in fig. 1.
Diffraction peaks of the precursor in FIG. 1 (a) with Cu 2 (OH) 3 NO 3 Cards are matched, so that the successful preparation of the target precursor is realized; FIG. 1 (b) shows a precursor having a two-dimensional platelet morphology with a length of about 400 nm; fig. 1 (c) shows that Cu element, N element and O element are uniformly distributed in the precursor.
(2) Placing the prepared precursor in a quartz boatAnd placing into a tube calciner, heating from room temperature to 300 ℃ at a heating rate of 10 ℃/min under an ammonia atmosphere, maintaining for 2h, and naturally cooling to room temperature to obtain Cu 3 N samples.
For Cu 3 The N samples were structurally characterized and the results are shown in FIG. 2.
Cu in FIG. 2 (a) 3 All diffraction peaks appearing on the N samples were uniform-corresponding to pure cubic Cu 3 N diffraction peaks, thus demonstrating that the present invention achieves pure Cu 3 Successful preparation of N; FIGS. 2 (b) and 2 (c) show Cu 3 The N sample substantially maintains the nanoplatelet morphology of the precursor, with a diameter of about 400nm. Furthermore, it is worth noting that Cu, in comparison to the precursor 3 The N sample has a rougher surface, which can provide more active sites in the subsequent catalytic reaction; FIG. 2 (d) shows that the lattice spacing of 0.22nm corresponds to cubic Cu 3 The (111) crystal plane of N; FIG. 2 (e) shows that the Cu element and the N element are in Cu 3 Evenly distributed in the N samples.
The result proves that the Cu is successfully prepared based on the LeChatelier's principle and the precursor shape guiding strategy 3 N nano-sheets.
Example 2
Cu prepared in example 1 3 Application study of N samples as catalysts in electrocatalytic methanol conversion:
electrocatalytic testing of methanol conversion was performed on an electrochemical workstation using a standard three electrode system. 1M potassium hydroxide solution containing 1M methanol and no methanol is used as electrolyte to modify Cu 3 The glassy carbon electrode of the N catalyst was the working electrode (5 mg Cu was used 3 N catalyst was dispersed in 500. Mu.L ethanol containing 10uL 5wt% Nafion and sonicated for 1h to prepare Cu 3 N ink; then 10. Mu.L of Cu 3 And (3) dripping the N ink onto the polished glassy carbon electrode to obtain a working electrode), wherein a carbon rod is used as a counter electrode, and a Hg/HgO electrode is used as a reference electrode.
As shown in FIG. 3a, cu in two 1M potassium hydroxide solutions containing 1M methanol and no methanol, respectively 3 There was a significant difference in the polarization curve of the N samples. Wherein Cu is 3 N electrode shows conventional electrocatalytic activity in 1M KOH electrolytePerformance at 1.64V vs. RHE to 10mA cm -2 Is used for the current density of the battery. In contrast, this potential requirement was significantly reduced to 1.35V after the addition of 1M methanol. Further comparative data are shown in FIG. 3b, current densities of 30, 60, 90 and 120mA cm, respectively, compared to water oxidation -2 At this time, the potential of the methanol oxidation reaction was reduced by 334, 368, 402 and 431mV, respectively.
Next, the formate of methanol oxidation products at different potentials was tested by ion chromatography (FIG. 3 c), and the Faraday efficiencies were more than 90% in the range of 1.4-1.8V vs. RHE potential (FIG. 3 d), indicating Cu 3 The N sample shows extremely high electrochemical selectivity in the electrocatalytic methanol oxidation reaction.
Cu is treated by adopting a chronopotentiometric method 3 The N samples were subjected to electrochemical stability testing, which showed little decay in current density generated over 12h (fig. 3 e), and the multi-potential transition curve (fig. 3 f) further indicated Cu 3 The N sample has extremely high electrochemical stability in the electrocatalytic methanol oxidation reaction.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. The preparation method of the copper nitride nano sheet is characterized by comprising the following steps of:
(1) 50mg of zinc oxide is dispersed in 50mL of 0.1M copper nitrate solution, stirred for reaction, centrifugally separated to obtain solid, washed and dried to obtain a precursor;
(2) Roasting the prepared precursor in an ammonia atmosphere to obtain a two-dimensional copper nitride nano sheet;
in the step (2), the roasting temperature is 300 ℃ and the time is 2 hours.
2. The method of manufacturing according to claim 1, characterized in that: in the step (2), the particle size of the two-dimensional copper nitride nano-sheet is 200-500nm.
3. The copper nitride nanoplatelets prepared by the preparation method according to claim 1 or 2.
4. Use of the copper nitride nano-sheet according to claim 3 for preparing formate by electrocatalytic methanol conversion.
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Citations (9)
| 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 |
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- 2022-06-08 CN CN202210652471.5A patent/CN115057417B/en active Active
Patent Citations (9)
| 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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