CN108569678B - Transition metal chalcogenide and preparation method and application thereof - Google Patents
Transition metal chalcogenide and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a transition metal chalcogenide compound and a preparation method and application thereof, and the compound provided by the invention is used as a working electrode material to be applied to electrocatalysis reaction for generating synthesis gas by electrocatalysis reduction of carbon dioxide by controlling the proportion of transition metal and sulfur and the appearance of crystals, the volume ratio of carbon monoxide to hydrogen in the obtained synthesis gas can be approximate to 1, and the synthesis gas has high efficiency, good stability, environmental friendliness and sustainability. The transition metal chalcogenide with the single-layer structure obtained by the preparation method provided by the invention has stable morphology, and has good preparation effect when being used for binary or ternary transition metal chalcogenide.
Description
Technical Field
The invention relates to the field of metal chalcogenide compounds, in particular to a transition metal chalcogenide compound and a preparation method and application thereof.
Background
Syngas is an important industrial feedstock that can be converted to short chain olefins (mainly ethylene, propylene and butylene) or directly synthesized into liquid fuels by fischer-tropsch reaction. The main components of syngas are carbon monoxide (CO) and hydrogen (H)2) The traditional method for preparing the synthesis gas is mainly to gasify solid fuels such as coal, coke or biomass, but CO (10-57%) and H in the synthesis gas obtained from different raw materials2(32-67%) and the coal, coke or biomass and other solid fuels are non-renewable in a short period of time, so that the invention of a sustainable and environment-friendly method for preparing the synthesis gas has important significance.
Electrochemical reduction of carbon dioxide (CO)2) And water (H)2O) is an efficient and environment-friendly way, which not only can reduce the dependence on fossil raw materials, but also can reduce C in the atmosphereO2Is an effective way to cope with the imminent collection of carbon taxes for solving global warming. To date, a number of electrocatalysts have been applied to the conversion of CO2The obtained synthesis gas, but the high-efficiency electrocatalyst is still mainly concentrated in noble metals (such as gold and silver); however, their further commercialization is limited by the low content of noble metals and the high price. Therefore, the search for high-efficiency non-noble metal electrocatalyst with abundant reserves and environmental friendliness has attracted people's attention.
Transition metal chalcogenides (TMDs) are a class of materials that are abundant, environmentally friendly, and have excellent electrocatalytic properties. In an acidic medium, the equilibrium potential for electrochemically reducing water to give hydrogen is 0V (relative to the reversible hydrogen electrode), and the equilibrium potential for reducing carbon dioxide to give carbon monoxide is-0.11V (relative to the reversible hydrogen electrode). TMDs materials are promising electrocatalytic materials that can simultaneously reduce water and carbon dioxide to obtain syngas due to the close reduction potential. TMDs such as molybdenum disulfide and tungsten diselenide have been shown to convert CO to2And H2O is converted into synthesis gas; however, the currently disclosed methods for preparing TMDs are all to mix and react raw materials directly to obtain blocky TMDs, and then to obtain powdery TMDs by grinding; the material has the problems of low conductivity, few active sites, weak intrinsic activity and the like when being applied to the preparation of synthesis gas; and the obtained synthesis gas has a great difference between carbon monoxide and hydrogen, so that the TMDs capable of efficiently catalyzing and synthesizing the synthesis gas are provided.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a transition metal chalcogenide, and a preparation method and an application thereof, in which the compound provided by the present invention is applied to catalysis of syngas as a catalyst, the volume ratio of carbon monoxide to hydrogen in the obtained syngas is approximately 1, and the shape of the compound prepared by the preparation method of the compound provided by the present invention is controllable.
The invention provides a transition metal chalcogenide compound, which has a general formula shown in a formula (I):
MoSexS(2-x)formula (I);
wherein x is more than or equal to 0 and less than or equal to 2;
the compound is of a single-layer structure, and the thickness of the single-layer structure is 0.71-0.76 nm.
The present invention also provides a method for preparing the transition metal chalcogenide according to the present invention, comprising:
1) mixing a molybdenum source, sulfur powder, selenium powder and a solvent to obtain a mixed solution,
the solvent is oleylamine and water,
the molar ratio of the molybdenum source to the sulfur powder to the selenium powder is 1: 1-2.5;
2) heating the mixed solution obtained in the step 1) for reaction and separation to obtain the transition metal chalcogenide shown in the formula (I),
MoSexS(2-x)formula (I);
wherein x is more than or equal to 0 and less than or equal to 2.
Preferably, the volume ratio of the oleylamine to the water is (15-30) to (3-6).
Preferably, the volume ratio of the oleylamine to the water is (5-10) to 1.
Preferably, the molybdenum source is ammonium molybdate.
Preferably, the using amount ratio of the molybdenum source to the solvent is 1mol to (25-35) mL.
Preferably, the reaction temperature is 180-220 ℃.
Preferably, the reaction time is 36 to 50 hours.
The invention also provides a preparation method of the synthesis gas, which comprises the following steps:
preparing the carbon dioxide gas into synthesis gas through electrocatalytic reaction;
wherein the electrocatalytic reaction is performed in a three-electrode system, and a working electrode in the three-electrode system is a glassy carbon electrode spin-coated with the transition metal chalcogenide according to claim 1.
Preferably, the electrolyte in the three-electrode system is EmimBF4And H2And (4) mixing the components.
Compared with the prior art, the transition metal chalcogenide compound with the structure shown in the formula (I) provided by the invention is applied to electrocatalysis reaction for generating synthesis gas by electrocatalysis reduction of carbon dioxide by taking the compound as a working electrode material through controlling the proportion of transition metal and sulfur and the appearance of crystal, the volume ratio of carbon monoxide to hydrogen in the obtained synthesis gas can be approximate to 1, and the synthesis gas has high efficiency and good stability, and is environment-friendly and sustainable.
The present invention also provides a method for preparing the transition metal chalcogenide according to the present invention, comprising: firstly, mixing a molybdenum source, sulfur powder, selenium powder and a solvent to obtain a mixed solution, then heating the mixed solution obtained in the step 1) for reaction, and separating to obtain a compound with a general formula shown in a formula (I), wherein the solvent is selected from oleylamine and water, and the molar ratio of the molybdenum source to the sulfur powder to the selenium powder is controlled to be 1: 1-2.5; and the obtained transition metal chalcogenide is of a single-layer structure, and the method provided by the invention has good preparation effect when being used for preparing binary or ternary transition metal chalcogenide.
Drawings
FIG. 1 MoS prepared in the example2Single layer structure (a), MoSeS alloy single layer structure (b), and MoSe2An XRD diffraction pattern of the monolayer structure (c);
FIG. 2 shows MoS prepared in example2Single layer structure (a), MoSeS alloy single layer structure (b), and MoSe2Raman spectrum of monolayer structure (c);
the MoSeS alloy single-layer structure (A, D) and MoS provided by the embodiment of FIG. 32Single layer structure (B, E) and MoSe2Transmission Electron Micrographs (TEM) and High Resolution Transmission Electron Micrographs (HRTEM) of the monolayer structure (C, F);
FIG. 4 shows the MoSeS alloy single-layer structure (A, D) and MoS provided in the examples2Single layer structure (B, E) and MoSe2An Atomic Force Microscopy (AFM) of the monolayer structure (C, F) and a corresponding height map, wherein 1, 2 in the height map correspond to 1, 2 in the atomic force microscopy;
FIG. 5 shows an embodimentProvides a MoSeS alloy single-layer structure (a) and MoS2Single layer structure (b) and MoSe2Monolayer structure (c) in EmimBF4Linear scanning voltammogram in aqueous solution;
FIG. 6 shows the MoSeS alloy single-layer structure and MoS provided in the examples2Single layer structure and MoSe2EmimBF of working electrode prepared in single-layer structure4Graph of hydrogen (open) and carbon monoxide (solid) yields produced in aqueous solution at a reaction potential of-1.15V (vs. reversible hydrogen electrode).
Detailed Description
The invention provides a transition metal chalcogenide compound, which has a general formula shown in a formula (I):
MoSexS(2-x)formula (I);
wherein x is more than or equal to 0 and less than or equal to 2;
the compound is of a single-layer structure, and the thickness of the single-layer structure is 0.71-0.76 nm.
According to the invention, x is preferably 0.5. ltoreq. x.ltoreq.1.5, more preferably 1. ltoreq. x.ltoreq.1.2.
The transition metal chalcogenide compound with the structure of the formula (I) provided by the invention is applied to electrocatalysis reaction for generating synthesis gas by electrocatalysis reduction of carbon dioxide by taking the compound as a working electrode material by controlling the proportion of transition metal and sulfur and the appearance of crystal, the volume ratio of carbon monoxide to hydrogen in the obtained synthesis gas can be approximate to 1, and the synthesis efficiency is high, the stability is good, and the environment is friendly and sustainable.
The present invention also provides a method for preparing the transition metal chalcogenide according to the present invention, comprising:
1) mixing a molybdenum source, sulfur powder, selenium powder and a solvent to obtain a mixed solution,
the solvent is oleylamine and water,
the molar ratio of the molybdenum source to the sulfur powder to the selenium powder is 1: 1-2.5;
2) heating the mixed solution obtained in the step 1) for reaction and separation to obtain a transition metal chalcogenide compound with a general formula shown in a formula (I),
MoSexS(2-x)formula (I);
according to the invention, a molybdenum source, sulfur powder, selenium powder and a solvent are mixed to obtain a mixed solution; wherein the molybdenum source is preferably ammonium molybdate; the volume ratio of the oleylamine to the water in the solvent is preferably (15-30) to (3-6), more preferably (5-10) to 1, and most preferably (6-8) to 1; the molar ratio of the molybdenum source to the sulfur powder is 1: 1.1-2.3, and more preferably 1: 1.3-2.1; the molar ratio of the molybdenum source to the selenium powder is 1: 1.1-2.3, and more preferably 1: 1.3-2.1; the dosage ratio of the molybdenum source to the solvent is 1mol to (25-35) mL, more preferably 1mol to (27-33) mL, and most preferably 1mol to (28-31) mL; the present invention does not require any particular mixing means, and any conventional mixing means known in the art may be used.
According to the invention, the mixed solution obtained in the step 1) is heated for reaction and separated to obtain the transition metal chalcogenide compound shown in the general formula (I); wherein the reaction temperature is preferably 180-220 ℃, and more preferably 200-210 ℃; the reaction time is preferably 36 to 50 hours, and more preferably 40 to 48 hours; after the reaction is finished, the invention preferably also naturally cools the reaction liquid after the heating reaction to room temperature, and then the transition metal chalcogenide compound with the general formula shown in the formula (I) is obtained by separation; the separation method is not particularly limited in the present invention, and a transition metal chalcogenide compound represented by the general formula (I) is preferably obtained by centrifugal separation; in order to make the product purity higher, the invention preferably also washes and dries the separated product; wherein the washing solvent is ethanol and cyclohexane; the drying temperature is 60-80 ℃ in order.
The present invention also provides a method for preparing a transition metal chalcogenide according to the present invention, comprising: firstly, mixing a molybdenum source, sulfur powder, selenium powder and a solvent to obtain a mixed solution, then heating the mixed solution obtained in the step 1) for reaction, and separating to obtain a compound with a general formula shown in a formula (I), wherein the solvent is selected from oleylamine and water, and the molar ratio of the molybdenum source to the sulfur powder to the selenium powder is controlled to be 1: 1-2.5; thereby making the obtained transition metal chalcogenide a single-layer structure.
The invention also provides a preparation method of the synthesis gas, which comprises the following steps:
preparing the carbon dioxide gas into synthesis gas through electrocatalytic reaction;
the electrocatalytic reaction is carried out in a three-electrode system, and a working electrode in the three-electrode system is a glassy carbon electrode spin-coated with the transition metal chalcogenide.
In the invention, in the three-electrode system, the reference electrode is preferably Ag/AgCl, and the counter electrode is preferably a platinum electrode; the electrolyte is preferably EmimBF4And H2O mixed solution; in the electrocatalytic reaction, the reaction potential of the working electrode is preferably-0.5 to-1.15V, more preferably-0.8 to-1.1V, and most preferably-0.9 to-1V.
According to the preparation method of the synthesis gas, the compound is selected as the working electrode material, and the proper electrolyte and reaction potential are selected, so that the preparation method of the synthesis gas has high synthesis efficiency, and the synthesis gas with the volume ratio of carbon monoxide to hydrogen being 1 can be obtained.
The following will clearly and completely describe the technical solutions of the embodiments of the present invention, and it is obvious that the described embodiments 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
159mg of ammonium molybdate, 30mg of sulfur powder and 74mg of selenium powder are dissolved in a mixed solution of 28.5mL of oleylamine and 1.5mL of water, stirred vigorously for 10min, and then the obtained mixed solution is transferred into a 50mL high-pressure reaction kettle, sealed and reacted at 220 ℃ for 48 h. After the reaction is finished, the mixture is naturally cooled to room temperature, the product obtained is centrifugally separated, and the product is washed for a plurality of times by ethanol and cyclohexane to remove residual organic matters. And finally drying in a vacuum drying oven at 60 ℃ to obtain black powder, namely a MoSeS alloy single-layer structure, and storing the black powder in a dryer for later use.
To the embodimentsThe structure of the prepared compound is identified, and the results are shown in figures 1-4, and the MoS prepared in the example of figure 12Single layer structure (a), MoSeS alloy single layer structure (b), and MoSe2An XRD diffraction pattern of the monolayer structure (c); FIG. 2 shows MoS prepared in example2Single layer structure (a), MoSeS alloy single layer structure (b), and MoSe2Raman spectrum of monolayer structure (c); the MoSeS alloy single-layer structure (A, D) and MoS provided by the embodiment of FIG. 32Single layer structure (B, E) and MoSe2Transmission Electron Micrographs (TEM) and High Resolution Transmission Electron Micrographs (HRTEM) of the monolayer structure (C, F); FIG. 4 shows the MoSeS alloy single-layer structure (A, D) and MoS provided in the examples2Single layer structure (B, E) and MoSe2Atomic Force Microscopy (AFM) of the monolayer structure (C, F) and corresponding height maps, wherein 1, 2 in the height maps correspond to 1, 2 in the atomic force microscopy.
Example 2
159mg of ammonium molybdate and 60mg of sulfur powder were dissolved in a mixed solution of 28.5mL of oleylamine and 1.5mL of water, and strongly stirred for 10min, and then the resulting mixture was transferred to a 50mL autoclave, sealed, and reacted at 220 ℃ for 48 hours. After the reaction is finished, the mixture is naturally cooled to room temperature, the product obtained is centrifugally separated, and the product is washed for a plurality of times by ethanol and cyclohexane to remove residual organic matters. Finally drying in a vacuum drying oven at 60 ℃ to obtain a product, namely MoS with a single-layer structure2And storing in a dryer for later use.
The compounds prepared in the examples were subjected to structural identification, and the results are shown in FIGS. 1 to 4, and FIG. 1 shows MoS prepared in the example2Single layer structure (a), MoSeS alloy single layer structure (b), and MoSe2An XRD diffraction pattern of the monolayer structure (c); FIG. 2 shows MoS prepared in example2Single layer structure (a), MoSeS alloy single layer structure (b), and MoSe2Raman spectrum of monolayer structure (c); the MoSeS alloy single-layer structure (A, D) and MoS provided by the embodiment of FIG. 32Single layer structure (B, E) and MoSe2Transmission Electron Micrographs (TEM) and High Resolution Transmission Electron Micrographs (HRTEM) of the monolayer structure (C, F): FIG. 4 shows the MoSeS alloy single-layer structure (A, D) and MoS provided in the examples2Single layer structure (B, E) and MoSe2Atomic Force Microscopy (AFM) of Single-layer Structure (C, F)And a corresponding height map, wherein 1, 2 in the height map correspond to 1, 2 in the atomic force microscopy image.
Example 3
159mg of ammonium molybdate and 148mg of selenium powder are dissolved in a mixed solution of 28.5mL of oleylamine and 1.5mL of water, the mixture is stirred vigorously for 10min, and then the obtained mixed solution is transferred into a 50mL high-pressure reaction kettle, sealed and reacted for 48h at 220 ℃. After the reaction is finished, the mixture is naturally cooled to room temperature, the product obtained is centrifugally separated, and the product is washed for a plurality of times by ethanol and cyclohexane to remove residual organic matters. Finally drying in a vacuum drying oven at 60 ℃ to obtain a product, namely MoS with a single-layer structure2And storing in a dryer for later use.
The compounds prepared in the examples were subjected to structural identification, and the results are shown in FIGS. 1 to 4, and FIG. 1 shows MoS prepared in the example2Single layer structure (a), MoSeS alloy single layer structure (b), and MoSe2An XRD diffraction pattern of the monolayer structure (c); FIG. 2 shows MoS prepared in example2Single layer structure (a), MoSeS alloy single layer structure (b), and MoSe2Raman spectrum of monolayer structure (c); the MoSeS alloy single-layer structure (A, D) and MoS provided by the embodiment of FIG. 32Single layer structure (B, E) and MoSe2Transmission Electron Micrographs (TEM) and High Resolution Transmission Electron Micrographs (HRTEM) of the monolayer structure (C, F); FIG. 4 shows the MoSeS alloy single-layer structure (A, D) and MoS provided in the examples2Single layer structure (B, E) and MoSe2Atomic Force Microscopy (AFM) of the monolayer structure (C, F) and corresponding height maps, wherein 1, 2 in the height maps correspond to 1, 2 in the atomic force microscopy.
Comparative example 1
Dissolving 220mg of molybdenum nitrate pentahydrate, 35mg of sulfur powder and 80mg of selenium powder in a mixed solution of 22mL of oleylamine and 3mL of water, stirring strongly for 10min, transferring the obtained mixed solution into a 50mL high-pressure reaction kettle, sealing, and reacting at 220 ℃ for 48 h. After the reaction is finished, the mixture is naturally cooled to room temperature, the product obtained is centrifugally separated, and the product is washed for a plurality of times by ethanol and cyclohexane to remove residual organic matters. And finally drying the product in a vacuum drying oven at 60 ℃, wherein the obtained product is not a MoSeS alloy single-layer structure through detailed characterization.
Comparative example 2
159mg of ammonium molybdate, 30mg of sulfur powder and 80mg of selenium powder are dissolved in a mixed solution of 18mL of oleylamine and 6mL of water, the mixture is stirred vigorously for 10min, and then the obtained mixed solution is transferred into a 50mL high-pressure reaction kettle, sealed and reacted for 48h at 160 ℃. After the reaction is finished, the mixture is naturally cooled to room temperature, the product obtained is centrifugally separated, and the product is washed for a plurality of times by ethanol and cyclohexane to remove residual organic matters. And finally drying the product in a vacuum drying oven at 60 ℃, wherein the obtained product is not a MoSeS alloy single-layer structure through detailed characterization.
Example 4
MoSeS electrocatalytic reduction CO with single-layer structure2Example Synthesis gas Generation:
the electrocatalytic reaction is carried out in a three-electrode system. Dispersing 4mg MoSeS alloy in a single layer in a mixed solution of 0.3mL of isopropanol and 0.7mL of water, adding 30 mu L of Nafion (5 wt%) solution, and ultrasonically dispersing the mixed solution for 10min to obtain a uniform electrode solution. Coating 4 mu L of electrode liquid on a glassy carbon electrode in a spinning way, and naturally drying to obtain a working electrode; Ag/AgCl is used as a reference electrode, and a platinum electrode is used as a counter electrode; the electrolyte is EmimBF4/H2And (4) mixing the components. Introducing high-purity CO into the electrolyte for 30min before reaction2Controlling the reaction potential of the working electrode to be-1.15V, and reacting for a certain time to obtain a composition of CO and H2Synthesis gas (ratio approximately 1: 1).
MoSeS was replaced by MoSe according to the above method2、MoS2The working electrode is prepared, other reaction conditions are unchanged, and the carbon dioxide is used as a raw material to prepare the synthesis gas.
Wherein, the results of preparing the synthesis gas are shown in fig. 5-6, wherein fig. 5 shows the MoSeS alloy single-layer structure (a) and MoS provided by the embodiment2Single layer structure (b) and MoSe2Monolayer structure (c) in EmimBF4Linear scanning voltammogram in aqueous solution; FIG. 6 shows the MoSeS alloy single-layer structure and MoS provided in the examples2Single layer structure and MoSe2EmimBF of working electrode prepared in single-layer structure4Graph of hydrogen (open) and carbon monoxide (solid) yields produced in aqueous solution at a reaction potential of-1.15V (vs. reversible hydrogen electrode).
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (7)
1. A method for preparing a transition metal chalcogenide having the general formula of formula (I):
MoSexS(2-x)formula (I);
wherein x is more than 0 and less than 2;
the compound is of a single-layer structure, and the thickness of the single-layer structure is 0.71-0.76 nm;
the preparation method of the transition metal chalcogenide compound comprises the following steps:
1) mixing a molybdenum source, sulfur powder, selenium powder and a solvent to obtain a mixed solution,
the solvent is oleylamine and water, and the volume ratio of the oleylamine to the water is (15-30): (3-6);
the mol ratio of the molybdenum source to the sulfur powder to the selenium powder is 1: (1-2.5): (1-2.5);
the dosage ratio of the molybdenum source to the solvent is 1 mol: (25-35) mL;
2) heating the mixed solution obtained in the step 1) for reaction and separation to obtain the transition metal chalcogenide shown in the formula (I),
MoSexS(2-x)formula (I);
wherein x is more than 0 and less than 2.
2. The preparation method according to claim 1, wherein the volume ratio of the oleylamine to the water is (5-10): 1.
3. the method of claim 1, wherein the molybdenum source is ammonium molybdate.
4. The method according to claim 1, wherein the reaction temperature is 180 to 220 ℃.
5. The method according to claim 1, wherein the reaction time is 36 to 50 hours.
6. A method of producing syngas, comprising:
preparing the carbon dioxide gas into synthesis gas through electrocatalytic reaction;
wherein, the electrocatalytic reaction is carried out in a three-electrode system, and a working electrode in the three-electrode system is a glassy carbon electrode of the transition metal chalcogenide prepared by spin coating the preparation method of the transition metal chalcogenide according to claim 1.
7. The method according to claim 6, wherein the electrolyte in the three-electrode system is EmimBF4And H2And (3) a mixed solution of O.
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