CN114538510A - Bismuth carbonate nano material and preparation method and application thereof - Google Patents
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Abstract
The invention relates to the technical field of electrochemistry, in particular to a bismuth carbonate nano material as well as a preparation method and application thereof. The invention discloses a bismuth carbonate nano material which is composed of uniformly distributed bismuth carbonate nano particles, has a large specific surface area, greatly improves the catalytic reduction capability of the bismuth carbonate nano material, and can be used for electrocatalysis of CO2In the process of preparing formic acid by reduction, the catalyst shows higher catalytic activity and selectivity under room temperature and mild conditions. In addition, the bismuth carbonate nano material also comprisesHas a large current density of>100mA cm‑2)。
Description
Technical Field
The invention relates to the technical field of electrochemistry, in particular to a bismuth carbonate nano material and a preparation method and application thereof.
Background
The hydrogen fuel cell has the advantages of high fuel energy conversion rate, low noise, zero emission and the like, and can be widely applied to vehicles such as automobiles, airplanes and trains, fixed power stations and the like. Since the fuel cell is applied to manned space, underwater submarines and distributed power stations, the fuel cell is always concerned by governments and enterprises of various countries, and under the condition that the coal-electricity occupation ratio is relatively low in the future, the power supply structure of the whole upstream becomes cleaner and cleaner due to the increase of the technical scale of renewable energy sources such as wind energy, solar energy and the like.
Therefore, how to safely and simply prepare hydrogen and store the hydrogen becomes an important direction for developing the research of the fuel cell. In addition to the hydrogen fuel cell, the formic acid fuel cell is widely studied because of its high energy density and safety. It would therefore be possible to solve the problem of product supply for fuel cells if hydrogen and formic acid could be readily produced using renewable energy sources.
Furthermore, the carbon dioxide concentration on the earth is continuously increasing and warming the earth due to the large-scale use of fossil energy. The global warming can cause a lot of damages, such as ice thawing, hot wave invasion, storm, flood and drought, and other natural disasters to become very frequent. Therefore, the emission reduction and resource utilization of carbon dioxide are a major problem to be solved urgently by human beings at present. In recent years, techniques such as carbon capture, carbon sequestration, etc. have been developed for capturing and concentrating carbon dioxide in the buried atmosphere, however, these techniques are resource intensive and the technological progress is slow and therefore are not currently the optimal choice. The conversion of carbon dioxide into hydrocarbons with economic benefits, such as high value-added products of methane, formic acid, ethylene, ethanol and the like, by biochemical methods, thermochemical methods, photochemical methods, electrochemical methods and the like is a promising method at present. However, biochemical and photochemical methods are inefficient in conversion, and thermochemical methods require severe reaction conditions such as high temperature and high pressure, and thus are not suitable for large-scale use. In view of the vigorous development of China in the field of new energy, the power generation capacity of renewable clean energy (wind energy and solar energy) is considerable, however, clean energy such as wind energy, solar energy and the like is difficult to be merged into a power grid because of strong intermittence, randomness, volatility and inverse peak shaving performance on the power grid, so that great waste is caused to the electric energy. If the electric energy is converted into chemical energy in a mild way, the resource is well utilized. Therefore, the renewable electric energy is used for converting carbon dioxide in the atmosphere into hydrogen storage materials with high energy density, such as formic acid, and the like, so that the emission of the carbon dioxide can be reduced, the resource waste can be avoided, and the renewable electric energy can be used as a reactant supply end of a formic acid fuel cell and a hydrogen fuel cell, and has important practical significance for relieving double pressure of energy and environment. Therefore, the technical problem to be solved is to provide a carbon dioxide electrochemical catalyst with high selectivity to formic acid.
Disclosure of Invention
In view of this, the invention provides a bismuth carbonate nano material, a preparation method and an application thereof.
The specific technical scheme is as follows:
the invention provides a bismuth carbonate nano material which is composed of bismuth carbonate nano sheets, wherein the bismuth carbonate nano sheets are formed by stacking bismuth carbonate nano particles.
In the invention, the bismuth carbonate nano material is in a flower ball shape; the width of the bismuth carbonate nano sheet is 10-20 um, the thickness is 0.04-0.06um, and the length is 20-30 um; the particle size of the bismuth carbonate nano-particles is 10nm-20 nm.
In the present invention, bismuth carbonate has a suitable band gap of 3.3eV and is a layered oxide having a specific Aurivillius/Sillen structure composed of (Bi)2O2)2+Layer and CO3 2-The ion layers are alternately formed into a layered structure, so that a bismuth carbonate nano material catalyst consisting of uniformly distributed nano particles is formed, and CO is electrically catalyzed2The application of the formic acid shows good performance, realizes higher activity and selectivity and larger current, and has low price and environmental protection.
The invention also provides a preparation method of the bismuth carbonate nano material, which comprises the following steps:
mixing the alkaline solution with a bismuth source dissolved in an ethylene glycol solution, and reacting to obtain a bismuth carbonate nano material;
the alkaline solution is sodium acetate trihydrate solution or urea.
The invention adopts hydrothermal reaction to prepare the bismuth carbonate nano material, has simple preparation process and easy operation, and is suitable for industrial application.
In the invention, the bismuth source is preferably bismuth nitrate pentahydrate;
the concentration of the sodium acetate trihydrate solution is 13-14 mol/L, and preferably 13.6 mol/L;
the concentration of the bismuth source ethylene glycol solution is 19-20mol/L, preferably 19.4 mol/L;
the mass ratio of the sodium acetate trihydrate or urea to the bismuth source is 1: 3.5;
the mixing is preferably carried out under ultrasonic conditions;
the power of the ultrasonic wave is 190-210W, preferably 200W, and the time is 0.5-1.5 h, preferably 1 h;
the reaction temperature is 170-190 ℃, preferably 180 ℃, and the reaction time is 11-13 h, preferably 12 h.
The invention also provides the application of the bismuth carbonate nano material or the bismuth carbonate nano material prepared by the preparation method in electrocatalytic reduction of carbon dioxide.
The invention also provides a preparation method of formic acid, which comprises the following steps:
and (2) preparing the bismuth carbonate nano material and carbon black into ink, dropwise adding the ink on carbon cloth to serve as a working electrode, constructing a three-electrode system, and introducing carbon dioxide into electrolyte to perform electrocatalytic reaction to obtain formic acid.
In the invention, the mass ratio of the bismuth carbonate nano material to the carbon black is 1: 1-3, preferably 1: 2; the concentration of the ink is 1 mg/ml; the carbon black is obtained by calcining a carbon nano tube at high temperature; the electrolyte is preferably sodium bicarbonate; the concentration of the electrolyte is preferably 0.5M; the size of the carbon cloth is 1 x 0.5cm2(ii) a The potential range of the test of the electrocatalytic reaction is-0.7 to-1.2V relative to a standard hydrogen electrode; the time for testing at each potential is preferably 2 h.
According to the technical scheme, the invention has the following advantages:
the invention provides aThe bismuth carbonate nano material is formed by piling uniformly distributed bismuth carbonate nano particles, has large specific surface area, greatly improves the catalytic reduction capability, and catalyzes CO in an electric way2In the process of preparing formic acid by reduction, the catalyst shows higher catalytic activity and selectivity under room temperature and mild conditions. In addition, the bismuth carbonate nano material also has larger current density (>100mA cm-2)。
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the description of the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without inventive labor.
Fig. 1 is a Scanning Electron Microscope (SEM) image of a bismuth carbonate nanomaterial composed of uniformly distributed nanoparticles provided in example 1 of the present invention;
FIG. 2 is a Transmission Electron Microscope (TEM) image of a bismuth carbonate nanomaterial composed of uniformly distributed nanoparticles provided in example 1 of the present invention;
fig. 3 is an X-ray diffraction (XRD) pattern of the bismuth carbonate nanomaterial composed of uniformly distributed nanoparticles provided in example 1 of the present invention;
FIG. 4 is an X-ray electron spectroscopy (XPS) chart of a bismuth carbonate nano-material composed of uniformly distributed nano-particles provided in example 1 of the present invention;
FIG. 5 shows CO of bismuth carbonate nano-material composed of uniformly distributed nano-particles provided in example 1 of the present invention2Performance map of reduction.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be apparent that the embodiments described below are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This example is a preparation of bismuth carbonate, which comprises the following specific steps:
0.272g of sodium acetate trihydrate was dissolved in 20ml of deionized water by sonication, designated solution 1, and then Bi (NO) was added3)3.5H2Mixing O (0.972g) and glycol (50ml) for 20min, named as solution 2, mixing the solution 1 and the solution 2, performing ultrasonic treatment for 1 hour, then transferring the solution into a high-pressure reaction kettle, setting the reaction temperature to be 180 ℃ and the reaction time to be 12 hours, cooling the solution, and then mixing ethanol and water according to a volume ratio of 1: 1, then setting the rotating speed to 8000, carrying out centrifugal washing for 6 times, and finally drying in a 60-degree oven for 12 hours to obtain the bismuth carbonate nano material.
Referring to fig. 1, which corresponds to an SEM image of the bismuth carbonate nanosheets composed of uniformly distributed nanoparticles of the present invention, it can be clearly seen from the figure that the bismuth carbonate nanosheets synthesized by the hydrothermal method constitute a flower-ball-shaped bismuth carbonate nanomaterial, the width of the bismuth carbonate nanosheets is 10um to 20um, the thickness of the bismuth carbonate nanosheets is 0.04 um to 0.06um, the length of the bismuth carbonate nanosheets is 20um to 30um, and the particle size of the bismuth carbonate nanoparticles is 10nm to 20 nm.
Referring to fig. 2, it is a TEM image of the bismuth carbonate nanomaterial composed of uniformly distributed nanoparticles of the present invention, and it can be seen from fig. 2 that the nanomaterial is composed of uniformly distributed nanoparticles, which illustrates that the bismuth carbonate nanomaterial catalyst prepared by the preparation method of the present invention has many nanoparticles with smaller particle size and sheets with larger specific surface area, which is beneficial to improving the electrocatalytic performance.
Referring to fig. 3 and 4, the XRD and XPS patterns of the bismuth carbonate nano material composed of uniformly distributed nano particles according to the present invention are shown, and the XRD spectrum of the prepared nano material is analyzed from the patterns and compared with the standard card, so that the product phase is Bi of pure phase2O2CO3And XPS further verified the resulting product.
Test examples
1. 0.5mg of the bismuth carbonate nano material prepared in example 1 and 1mg of carbon black are weighed respectively to prepare 1mg/ml of ink (the solvent is ethanol, water and naphthol in a volume ratio of 1: 1: 6) which is dropped on 1 x 0.5cm2The test was performed on the carbon cloth.
2. The electrolytic solution used in the test was 0.5M KHCO3And (3) solution.
3. The reference electrode used in the test process is Ag/AgCl, the working electrode is the carbon cloth prepared in the step 1, the counter electrode is foil wire, and the tested potential range is-0.7 to-1.2V relative to the standard hydrogen electrode.
4. Test at each potential for 2 hours.
5. Carbon dioxide is continuously introduced in the electrolysis process.
Referring to fig. 5, which is a corresponding performance diagram of the bismuth carbonate nano-material composed of uniformly distributed nano-particles of the present invention, it can be seen that the nano-material of example 1 of the present invention has a higher selectivity to formic acid and a larger current density.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The bismuth carbonate nano material is characterized by consisting of bismuth carbonate nano sheets, wherein the bismuth carbonate nano sheets are formed by stacking bismuth carbonate nano particles.
2. The bismuth carbonate nanomaterial of claim 1, wherein the bismuth carbonate nanomaterial is in the shape of a flower sphere;
the width of the bismuth carbonate nano-sheet is 10-20 um, the thickness is 0.04-0.06um, and the length is 20-30 um.
3. The bismuth carbonate nanomaterial according to claim 1, wherein the particle size of the bismuth carbonate nanoparticles is 10nm to 20 nm.
4. The preparation method of the bismuth carbonate nano material is characterized by comprising the following steps of: mixing the alkaline solution with a bismuth source ethylene glycol solution for reaction to obtain a bismuth carbonate nano material;
the alkaline solution is sodium acetate trihydrate solution or urea.
5. The preparation method according to claim 4, wherein the concentration of the sodium acetate trihydrate solution is 13-14 mol/L.
6. The method according to claim 4, wherein the bismuth source is bismuth nitrate pentahydrate;
the concentration of the glycol solution of the bismuth source is 19-20 mol/L.
7. The preparation method according to claim 4, wherein the reaction temperature is 170-190 ℃ and the reaction time is 11-13 h.
8. The production method according to claim 4, wherein the mass ratio of the sodium acetate trihydrate or urea to the bismuth source is 1: 3.5.
9. Use of the bismuth carbonate nanomaterial of claims 1 to 3 or the bismuth carbonate nanomaterial prepared by the preparation method of any one of claims 4 to 8 in electrocatalytic reduction of carbon dioxide.
10. A preparation method of formic acid is characterized by comprising the following steps:
the bismuth carbonate nano material of claims 1 to 3 or the bismuth carbonate nano material prepared by the preparation method of any one of claims 4 to 8 and carbon black are prepared into ink which is dripped on carbon cloth to be used as a working electrode, a three-electrode system is constructed, and carbon dioxide is introduced into electrolyte to carry out electrocatalytic reaction, so that formic acid is obtained.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150210560A1 (en) * | 2014-01-30 | 2015-07-30 | Sandia Corporation | Hydrothermal Synthesis of Bismuth Germanium Oxide |
| CN109482213A (en) * | 2018-12-29 | 2019-03-19 | 陕西师范大学 | A kind of Bi/ (BiO)2CO3The preparation method of nanometer flower ball-shaped photochemical catalyst |
| CN109518222A (en) * | 2019-01-28 | 2019-03-26 | 苏州大学 | For electro-catalysis CO2It is restored to the bismuth-based catalysts and its preparation method and application of formic acid |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150210560A1 (en) * | 2014-01-30 | 2015-07-30 | Sandia Corporation | Hydrothermal Synthesis of Bismuth Germanium Oxide |
| CN109482213A (en) * | 2018-12-29 | 2019-03-19 | 陕西师范大学 | A kind of Bi/ (BiO)2CO3The preparation method of nanometer flower ball-shaped photochemical catalyst |
| CN109518222A (en) * | 2019-01-28 | 2019-03-26 | 苏州大学 | For electro-catalysis CO2It is restored to the bismuth-based catalysts and its preparation method and application of formic acid |
Non-Patent Citations (1)
| Title |
|---|
| LIN MA ET AL.: "Facile Template-free Synthesis of Bi2O2CO3 Flower-like Architecturse in Ethylene Glycol Water System" * |
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