CN112194136A - Preparation method of three-dimensional bouquet structure alpha-molybdenum carbide @ carbon with efficient photo-thermal conversion characteristic - Google Patents
Preparation method of three-dimensional bouquet structure alpha-molybdenum carbide @ carbon with efficient photo-thermal conversion characteristic Download PDFInfo
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Abstract
A preparation method of alpha-molybdenum carbide @ carbon with a three-dimensional bouquet structure and high-efficiency photothermal conversion characteristics relates to alpha-MoC with high-efficiency photothermal conversion characteristics1‑xA process for the preparation of @ C. The invention aims to solve the technical problems that the existing preparation method of molybdenum carbide has harsh preparation conditions, easy agglomeration, easy spontaneous combustion and small specific surface area, and greatly influences the application effect of the existing preparation method in the field of solar seawater desalination. alpha-MoC with three-dimensional bouquet structure prepared by the invention1‑xThe specific surface area of @ C is 300-600 m2g‑1The pore volume is 2-5 cm3·g‑1And has super-hydrophobicity; the three-dimensional bouquet structure alpha‑MoC1‑x@ C at low loading of 0.01-1 mgcm‑2When the absorption rate is 92% in the range of 200-2500 nm, the light absorption rate is 92% in the simulated sun illumination (1 kW.m)‑2) The lower water evaporation rate is 1.77kgm‑2h‑1。
Description
Technical Field
The invention relates to an alpha-MoC with efficient photo-thermal conversion characteristic1-xA process for the preparation of @ C.
Background
Seawater desalination is an effective method for solving the water resource crisis. The conventional seawater desalination technology such as multi-effect distillation, multi-stage flash evaporation and the like can realize the desalination and desalination of seawater, but the problem of high energy consumption and high cost exists, so that the wide application of the seawater is limited. Solar seawater desalination is a seawater desalination technology driven by solar energy, and is an important direction for development of a low-energy-consumption, green and economic seawater desalination technology. Although the inorganic semiconductor photo-thermal conversion material shows a certain photo-evaporation capacity due to the advantages of low cost, easy shape control, high absorbance and the like, the problems of poor repeatability, small specific surface area, low photo-evaporation rate and the like exist at present, so that the large-scale application of the inorganic semiconductor photo-thermal conversion material is limited. The development of novel high-efficiency photothermal conversion materials has very important research significance.
Molybdenum carbide is an interstitial compound formed by inserting carbon atoms into a metal lattice, and chemical bonds consist of metallic bonds, ionic bonds and covalent bonds. The incorporation of carbon atoms modifies the d-band nature of the metal, resulting in its noble metal-like properties, and the presence of its ionic and covalent bonds also imparts ionic and covalent crystalline properties to the material. However, the existing various molybdenum carbide preparation methods have the defects of harsh preparation conditions, easy agglomeration, easy spontaneous combustion, small specific surface area and the like, and greatly influence the application research of the molybdenum carbide in the field of solar seawater desalination.
Disclosure of Invention
The invention provides a preparation method of alpha-molybdenum carbide @ carbon with a three-dimensional bouquet structure and high-efficiency photothermal conversion characteristics, aiming at solving the technical problems that the existing preparation method of molybdenum carbide has the defects of harsh preparation conditions, easy agglomeration, easy spontaneous combustion, small specific surface area and the like, and the application effect of the existing preparation method of molybdenum carbide in the field of solar seawater desalination is greatly influenced.
The preparation method of the three-dimensional bouquet structure alpha-molybdenum carbide @ carbon with efficient photothermal conversion characteristics is carried out according to the following steps:
firstly, sequentially adding molybdenum powder and 30 mass percent aqueous hydrogen peroxide solution into liquid alcohol, stirring for 24-48 h, adding melamine, continuously stirring for 0.5-48 h, centrifuging for 5-10 min at the rotating speed of 3000-5000 rpm, and finally drying to obtain a molybdenum precursor;
the ratio of the mass of the molybdenum powder to the volume of the aqueous hydrogen peroxide solution with the mass fraction of 30% is 1g (0.5 mL-50 mL);
the mass ratio of the molybdenum powder to the liquid alcohol is 1g (10 mL-500 mL);
the mass ratio of the molybdenum powder to the melamine is 1 (1-50);
secondly, mechanically mixing the molybdenum precursor obtained in the step one with urea, then putting the mixture into a crucible, calcining the mixture in a tubular furnace under inert atmosphere, wherein the calcining temperature is 450-950 ℃, and the heating rate is 5 ℃ for min-1～10℃min-1The heat preservation time is 2-8 h, and the alpha-MoC with the three-dimensional bouquet structure is obtained1-x@ C; and in the second step, the mass ratio of the molybdenum precursor to the urea is 1 (3-900).
The preparation method has good repeatability and high yield, and the prepared alpha-MoC with the three-dimensional bouquet structure1-xThe specific surface area of @ C is 300-600 m2 g-1The pore volume is 2-5 cm3·g-1(ii) a The three-dimensional bouquet structure is alpha-MoC1-x@ C has super-hydrophobicity, and can prevent the salt from depositing in the material to influence the absorption of sunlight; the three-dimensional bouquet structure is alpha-MoC1-x@ C at low loading of 0.01-1 mg cm-2When the water is evaporated, the absorbance is 92% in the range of 200-2500 nm, and the water evaporation rate is 1.77kg m-2h-1。
alpha-MoC with three-dimensional bouquet structure prepared by the invention1-x@ C can be applied to photo-thermal seawater desalinationThe material consumption can be obviously reduced, and the material cost is reduced.
Drawings
FIG. 1 shows the alpha-MoC of the three-dimensional bouquet structure prepared in experiment one1-xA transmission electron microscopy image of @ C;
FIG. 2 shows the alpha-MoC of the three-dimensional bouquet structure prepared in experiment one1-xAn atomic force microscopy image of @ C;
FIG. 3 shows the alpha-MoC of the three-dimensional bouquet structure prepared in experiment two1-xA nitrogen desorption curve of @ C;
FIG. 4 shows the alpha-MoC of the three-dimensional bouquet structure prepared in experiment two1-xThe BJH method differential integral pore area and pore diameter distribution curve chart of @ C;
FIG. 5 shows the alpha-MoC of the three-dimensional bouquet structure prepared in experiment two1-xContact angle test chart of @ C;
FIG. 6 shows the α -MoC of the three-dimensional bouquet structure prepared in experiment two1-xScanning electron microscopy images of @ C;
FIG. 7 is a graph of the photo-evaporation rate at different loadings for run four;
FIG. 8 is a graph of the alpha-MoC of the three-dimensional bouquet structure prepared in experiment three1-xUV-vis-IR diffuse reflectance spectral curve @ C.
Detailed Description
The first embodiment is as follows: the embodiment is a preparation method of alpha-molybdenum carbide @ carbon with a three-dimensional bouquet structure and efficient photothermal conversion characteristics, and the preparation method is specifically carried out according to the following steps:
firstly, sequentially adding molybdenum powder and 30 mass percent aqueous hydrogen peroxide solution into liquid alcohol, stirring for 24-48 h, adding melamine, continuously stirring for 0.5-48 h, centrifuging for 5-10 min at the rotating speed of 3000-5000 rpm, and finally drying to obtain a molybdenum precursor;
the volume ratio of the molybdenum powder to the aqueous hydrogen peroxide solution with the mass fraction of 30% is 1g (0.5 mL-50 mL);
the mass ratio of the molybdenum powder to the liquid alcohol is 1g (10 mL-500 mL);
the mass ratio of the molybdenum powder to the melamine is 1 (1-50);
secondly, mechanically mixing the molybdenum precursor obtained in the step one with urea, then putting the mixture into a crucible, calcining the mixture in a tubular furnace under inert atmosphere, wherein the calcining temperature is 450-950 ℃, and the heating rate is 5 ℃ for min-1～10℃min-1The heat preservation time is 2-8 h, and the alpha-MoC with the three-dimensional bouquet structure is obtained1-x@ C; and in the second step, the mass ratio of the molybdenum precursor to the urea is 1 (3-900).
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the liquid alcohol in the step one is one or a mixture of more of absolute ethyl alcohol, ethylene glycol and isopropanol. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the drying temperature in step one is 40 ℃. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the volume ratio of the molybdenum powder in the first step to the aqueous hydrogen peroxide solution with the mass fraction of 30% is 1g (20 mL-40 mL). The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: the mass ratio of the molybdenum powder to the alcohol solution in the first step is 1g (100 mL-200 mL). The rest is the same as the fourth embodiment.
The sixth specific implementation mode: the fifth embodiment is different from the fifth embodiment in that: the mass ratio of the molybdenum powder to the melamine in the step one is 1 (10-30). The rest is the same as the fifth embodiment.
The seventh embodiment: the sixth embodiment is different from the sixth embodiment in that: and the mechanical mixing in the step two is grinding or stirring. The rest is the same as the sixth embodiment.
The specific implementation mode is eight: the seventh embodiment is different from the seventh embodiment in that: and the inert atmosphere in the second step is nitrogen. The rest is the same as the seventh embodiment.
The specific implementation method nine: the eighth embodiment is different from the eighth embodiment in that: the calcination temperature in the second step is 500-750 ℃. The rest is the same as the embodiment eight.
The detailed implementation mode is ten: the present embodiment differs from the ninth embodiment in that: in the second step, the mass ratio of the molybdenum precursor to the urea in the second step is 1 (300-600). The rest is the same as in the ninth embodiment.
The invention was verified with the following tests:
test one: the test is a preparation method of three-dimensional bouquet structure alpha-molybdenum carbide @ carbon with efficient photothermal conversion characteristics, and the preparation method is specifically carried out according to the following steps:
firstly, sequentially adding molybdenum powder and 30% aqueous hydrogen peroxide solution into absolute ethyl alcohol, stirring for 48 hours, adding melamine, continuing stirring for 0.5 hour, then centrifuging for 5min at the rotating speed of 5000rpm, and finally drying to obtain a molybdenum precursor; the drying temperature is 40 ℃;
the volume ratio of the mass of the molybdenum powder to the volume of the aqueous hydrogen peroxide solution with the mass fraction of 30% is 1g:3 mL;
the volume ratio of the mass of the molybdenum powder to the volume of the ethanol is 1g:80 mL;
the mass ratio of the molybdenum powder to the melamine is 1: 2;
secondly, mechanically mixing the molybdenum precursor obtained in the step one with urea, then putting the mixture into a crucible, and calcining the mixture in a tube furnace under the inert atmosphere, wherein the calcining temperature is 550 ℃, and the heating rate is 10 ℃ for min-1Keeping the temperature for 6h to obtain the alpha-MoC with the three-dimensional bouquet structure1-x@ C; and in the second step, the mass ratio of the molybdenum precursor to the urea is 1: 8.
FIG. 1 shows the alpha-MoC of the three-dimensional bouquet structure prepared in experiment one1-xIn the transmission electron microscope image of @ C, molybdenum carbide nanocrystals are in the circles, the curved stripes around the molybdenum carbide nanocrystals are carbon materials, and alpha-MoC can be seen from the image1-xThe nanocrystals are encapsulated by a carbon layer, alpha-MoC1-xThe size of the nanocrystal is 3nAnd m is about.
FIG. 2 shows the alpha-MoC of the three-dimensional bouquet structure prepared in experiment one1-xAn atomic force microscope picture of @ C, from which alpha-MoC can be seen1-x@ C is about 3nm thick.
And (2) test II: this test differs from the test one in that: sequentially adding molybdenum powder and 30% aqueous hydrogen peroxide solution into absolute ethyl alcohol, stirring for 48 hours, adding melamine, continuing stirring for 1 hour, centrifuging at the rotating speed of 5000rpm for 5min, and finally drying to obtain a molybdenum precursor; the drying temperature is 40 ℃. The rest is the same as test one.
FIG. 3 shows the alpha-MoC of the three-dimensional bouquet structure prepared in experiment two1-xThe nitrogen adsorption-desorption curve of @ C,. smallcircle represents the adsorption isotherm curve, and □ represents the desorption isotherm curve, it can be seen that the specific surface area of the final product obtained is as high as 300m2 g-1。
FIG. 4 shows the alpha-MoC of the three-dimensional bouquet structure prepared in experiment two1-xThe BJH method differential integral pore area pore diameter distribution curve chart of @ C, □ corresponding to the right ordinate, and O corresponding to the left ordinate, it can be seen that the pore volume of the final product is 3cm3·g-1。
FIG. 5 shows the alpha-MoC of the three-dimensional bouquet structure prepared in experiment two1-xThe contact angle test chart of @ C shows that the material has super-hydrophobicity.
FIG. 6 shows the α -MoC of the three-dimensional bouquet structure prepared in experiment two1-xIn the scanning electron microscopy image of @ C, it can be seen that the material has a rich pore structure.
And (3) test III: this test differs from the test one in that: the calcination temperature in step two was 650 ℃. The rest is the same as test one.
FIG. 8 is a graph of the alpha-MoC of the three-dimensional bouquet structure prepared in experiment three1-xThe UV-vis-IR diffuse reflectance spectrum curve of @ C shows that the absorptivity of the material in the whole solar wave band (200-2500 nm) is 92%.
And (4) testing: respectively weighing three-dimensional bouquet structure alpha-MoC prepared by experiment three1-x0, 0.1mg, 0.2mg, 0.4mg, 0.8mg and 10mg of @ C material, each dispersed in the azomethyl groupIn a pyrrolidone solution, PVDF is used as a binder, the composite material is filtered on a microporous filter membrane (a nylon membrane) by a vacuum filtration method, the composite material is naturally dried, and blank parts on the microporous filter membrane are cut off to obtain a two-dimensional evaporation membrane; adding 50mL of simulated seawater into a 50mL beaker, taking polystyrene foam as a heat insulation layer, taking a two-dimensional evaporation film as a photo-thermal conversion film, and obtaining the simulated sunlight with the light intensity of 1kWm-2And then carrying out a seawater evaporation test, and recording the change of the seawater quality in the beaker along with the evaporation time. FIG. 7 is a graph of the water evaporation rate under different loading in experiment five, wherein the curve 1 is 0, the curve 2 is 0.1mg, the curve 3 is 0.2mg, the curve 4 is 0.4mg, the curve 5 is 0.8mg, and the curve 6 is 10mg, and the results of the water evaporation experiment show that the simulated sun illumination (1 kWm)-2) Under the condition of jetting, the alpha-MoC 1-x @ C film (in a dry state) can reach a temperature close to the equilibrium within 10s, the water evaporation rate of the material can reach an equilibrium state under a very low dosage (0.8mg), and the water evaporation rate can reach 1.77kg m-2h-1The low-loading advantage is significantly better than other inorganic semiconductor materials reported at present.
Claims (10)
1. A preparation method of three-dimensional bouquet structure alpha-molybdenum carbide @ carbon with efficient photothermal conversion characteristics is characterized in that the preparation method of the three-dimensional bouquet structure alpha-molybdenum carbide @ carbon with efficient photothermal conversion characteristics is carried out according to the following steps:
firstly, sequentially adding molybdenum powder and 30 mass percent aqueous hydrogen peroxide solution into liquid alcohol, stirring for 24-48 h, adding melamine, continuously stirring for 0.5-48 h, centrifuging for 5-10 min at the rotating speed of 3000-5000 rpm, and finally drying to obtain a molybdenum precursor;
the volume ratio of the molybdenum powder to the aqueous hydrogen peroxide solution with the mass fraction of 30% is 1g (0.5 mL-50 mL);
the mass ratio of the molybdenum powder to the liquid alcohol is 1g (10 mL-500 mL);
the mass ratio of the molybdenum powder to the melamine is 1 (1-50);
secondly, mechanically mixing the molybdenum precursor obtained in the step one with urea, and thenThen placing the mixture in a crucible, calcining the mixture in a tubular furnace under the inert atmosphere, wherein the calcining temperature is 450-950 ℃, and the heating rate is 5 ℃ for min-1～10℃min-1The heat preservation time is 2-8 h, and the alpha-MoC with the three-dimensional bouquet structure is obtained1-x@ C; the mass ratio of the molybdenum precursor to the urea in the second step is 1 (3-900).
2. The method for preparing alpha-molybdenum carbide @ carbon with a three-dimensional bouquet structure and high efficiency photothermal conversion characteristics as claimed in claim 1, wherein the liquid alcohol in the first step is one or a mixture of anhydrous ethanol, ethylene glycol and isopropanol.
3. The method for preparing the alpha-molybdenum carbide @ carbon having the three-dimensional bouquet structure with efficient photothermal conversion characteristics as claimed in claim 1, wherein the drying temperature in the first step is 40 ℃.
4. The method for preparing alpha-molybdenum carbide @ carbon having a three-dimensional bouquet structure with efficient photothermal conversion characteristics as claimed in claim 1, wherein the ratio of the mass of the molybdenum powder to the volume of the aqueous solution of hydrogen peroxide with a mass fraction of 30% in the step one is 1g (20 mL-40 mL).
5. The method for preparing alpha-molybdenum carbide @ carbon with the three-dimensional bouquet structure and the efficient photothermal conversion characteristic as claimed in claim 1, wherein the mass-to-volume ratio of the molybdenum powder to the alcohol solution in the step one is 1g (100 mL-200 mL).
6. The preparation method of the alpha-molybdenum carbide @ carbon with the three-dimensional bouquet structure and the efficient photothermal conversion characteristic as claimed in claim 1, wherein the mass ratio of the molybdenum powder to the melamine in the step one is 1 (10-30).
7. The method for preparing the alpha-molybdenum carbide @ carbon with the three-dimensional bouquet structure and the efficient photothermal conversion characteristic as claimed in claim 1, wherein the mechanical mixing in the second step is grinding or stirring.
8. The method for preparing the alpha-molybdenum carbide @ carbon with the three-dimensional bouquet structure and the efficient photothermal conversion characteristic as claimed in claim 1, wherein the inert atmosphere in the second step is nitrogen.
9. The method for preparing the alpha-molybdenum carbide @ carbon having the three-dimensional bouquet structure with the efficient photothermal conversion characteristics as claimed in claim 1, wherein the calcination temperature in the second step is 500 ℃ to 750 ℃.
10. The preparation method of the alpha-molybdenum carbide @ carbon with the three-dimensional bouquet structure and the efficient photothermal conversion characteristic according to claim 1, wherein the mass ratio of the molybdenum precursor to urea in the second step is 1 (300-600).
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| CN113443695A (en) * | 2021-06-30 | 2021-09-28 | 福州大学 | Molybdenum carbide auxiliary agent, preparation method thereof and application of molybdenum carbide auxiliary agent in degradation of organic pollutants through Fenton reaction |
| US11502322B1 (en) | 2022-05-09 | 2022-11-15 | Rahul S Nana | Reverse electrodialysis cell with heat pump |
| US11502323B1 (en) | 2022-05-09 | 2022-11-15 | Rahul S Nana | Reverse electrodialysis cell and methods of use thereof |
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| US11855324B1 (en) | 2022-11-15 | 2023-12-26 | Rahul S. Nana | Reverse electrodialysis or pressure-retarded osmosis cell with heat pump |
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| CN113443695B (en) * | 2021-06-30 | 2023-08-22 | 福州大学 | Molybdenum carbide auxiliary agent, preparation method thereof and application thereof in Fenton reaction degradation of organic pollutants |
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