CN113699550B - Molybdenum sulfide/fluoride host-guest catalytic material, preparation method and application - Google Patents
Molybdenum sulfide/fluoride host-guest catalytic material, preparation method and application Download PDFInfo
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Abstract
The invention discloses a molybdenum sulfide/fluoride host-guest catalytic material, a preparation method and application thereof, wherein the molybdenum sulfide/fluoride host-guest catalytic material comprises a molybdenum sulfide host compound and an interlayer intercalator guest compound, the interlayer intercalator is inserted between (002) crystal faces of a molybdenum sulfide matrix, and the interlayer intercalator is a fluorine compound. The catalytic material of the invention adopts the technical scheme of widening the ion channel to increase the ion transmission rate in the electrochemical hydrogen evolution process, thereby effectively improving the electrocatalytic hydrogen evolution activity of the catalytic material.
Description
Technical Field
The invention relates to new energy, in particular to a molybdenum sulfide/fluoride host-guest catalytic material, a preparation method and application.
Background
The hydrogen is produced by electrolyzing water by utilizing renewable energy sources (light, wind and hydroelectric power generation), and the carbon peak reaching and carbon neutralization can be realized. The noble metal platinum electrode is considered to be an ideal hydrogen evolution material for electrolysis water because of low hydrogen evolution overpotential and low tafel slope. However, the noble metal is limited in resource and expensive, so that it is difficult to industrially popularize and apply the noble metal on a large scale. For this reason, non-noble metal hydrogen evolution electrocatalysts have been developed. Molybdenum sulfide (MoS)2) This is of particular interest because the sulfur edge in its structure adsorbs hydrogen similarly to Pt metal. It has three structures, 1T-MoS2, 2H-MoS2And 3R-MoS2。1T-MoS2The octahedron coordination of the structure has metallicity and belongs to a metastable state structure; 2H-MoS2The crystal form contains two Mo-S units and belongs to a stable state structure; 3R-MoS2Crystal form ratio of 2H-MoS2The crystal form has one more Mo-S unit, namely contains three Mo-S units and also belongs to a metastable state structure. 1T-MoS2And 3R-MoS2The stability is not high, and the catalyst is not an ideal hydrogen evolution electrocatalyst; 2H-MoS2The molybdenum sulfide is relatively stable, but the conductivity is poor, so that molybdenum sulfide is doped with metal elements such as nickel and cobalt, and the hydrogen evolution performance of the molybdenum sulfide is improved. The above method is based on increasing the number of active sites, thereby improving the hydrogen evolution performance. However, doping cannot change the size of the ion channel, and the hydrogen evolution capacity, stability and the like of the ion channel are to be improved.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide a molybdenum sulfide/fluoride host-guest catalytic material, a preparation method and application, which can expand an ion channel of molybdenum sulfide, improve the microstructure of a catalyst, improve the proton transfer rate, enhance the mobility of ions in the electrochemical reaction process, reduce the flow resistance of the ions and improve the hydrogen evolution electrocatalytic activity.
In order to achieve the above object, an embodiment of the present invention provides a molybdenum sulfide/fluoride host-guest catalytic material, including a molybdenum sulfide matrix and an interlayer insertion agent, where the interlayer insertion agent is inserted between (002) crystal faces of the molybdenum sulfide matrix, and the interlayer insertion agent is a fluorine compound.
In one or more embodiments of the present invention, the interplanar spacing between the (002) crystal planes of the molybdenum sulfide matrix after interlayer intercalator insertion is not less than 9.0 a.
In one or more embodiments of the invention, the interlayer intercalant comprises 0.2 to 7.5 mole percent of the catalytic material. The content ratio of the interlayer intercalator in the catalytic material in the present invention is mainly related to the concentration of the interlayer intercalator at the time of reaction. The influence of other possible factors such as reaction time, solvent, temperature, pressure etc. is of course not absolutely excluded.
In one or more embodiments of the present invention, the interlayer intercalating agent is potassium fluoride or sodium fluoride.
In one or more embodiments of the present invention, a method for preparing a molybdenum sulfide/fluoride host-guest catalytic material includes the steps of, a, preparing MoS2A base material; B. MoS2The matrix material is added into a solution containing an interlayer insertion agent, and the insertion agent is inserted between (002) crystal faces of the molybdenum sulfide matrix under the reduced reaction condition.
In one or more embodiments of the invention, step a is to prepare a molybdenum source solution and a sulfur source solution, dropwise add the sulfur source solution into the molybdenum source solution and sufficiently mix the solution, heat the mixed solution in a high-pressure hydrothermal reaction kettle to react until the reaction is finished, separate, remove impurities, and dry the mixed solution to obtain MoS2A base material. Preferably, the molybdenum source is a molybdate, particularly sodium molybdate, potassium molybdate, or the like. The sulfur source is preferably thiourea, sodium thiosulfate, or the like.
In one or more embodiments of the invention, the heating reaction in the high-pressure hydrothermal reaction kettle in the step A is at 220 ℃ for 20-24 h.
In one or more embodiments of the invention, step B is preparing an interlayer intercalant solution and adding an appropriate amount of MoS2Adding the interlaminar intercalator solution into the matrix material, heating and reacting in a high-pressure hydrothermal reaction kettle until the reaction is finished, separating, removing impurities, and drying to obtain the molybdenum sulfide/fluoride host-guest catalytic material.
In one or more embodiments of the invention, the heating reaction in the high-pressure hydrothermal reaction kettle in the step B is carried out at 140 ℃ and 200 ℃ for 7-10 h.
In one or more embodiments of the invention, the use of molybdenum sulfide/fluoride host-guest catalytic materials in the catalytic production of hydrogen.
Compared with the prior art, the catalytic material provided by the invention has the advantages that the fluoride is inserted into the 2H-MoS2The surface spacing between (002) crystal surfaces of the material is increased from 6.5A to 9.0A, so that the ion mobility in the electrochemical reaction process is enhanced, the flow resistance of ions is reduced, and the hydrogen evolution electrocatalytic activity is improved, thereby greatly widening the ion flux of the electrochemical reactionTherefore, the capability of preparing hydrogen by electrocatalysis is obviously improved. The hydrogen prepared by the method is high-purity hydrogen, does not contain carbon monoxide, hydrogen sulfide and other pollutants which poison fuel cell electrode materials, and is simple, easy to implement, green and environment-friendly.
Drawings
FIG. 1 is a powder diffraction pattern of various samples according to one embodiment of the present invention, (a) 2H-MoS2；(b) KF0.5-MoS2; (c)KF0.6-MoS2And (d) KF0.75-MoS2；
FIG. 2 is an electrocatalytic hydrogen evolution curve of various samples according to one embodiment of the invention, wherein (a) MoS2; (b)KF0.25-MoS2; (c)KF0.5-MoS2; (d)KF0.6-MoS2; (e) KF0.75-MoS2; (f)Pt/C(10%); (g)KF1-MoS2. The scanning rate is 10 mV S-1The electrolyte is 1.0mol/L KOH;
FIG. 3 is a MoS according to an embodiment of the present invention2-XPS plot of KF host guest compound;
FIG. 4 is a MoS according to an embodiment of the present invention2-XPS plot of molybdenum element in KF host guest compound;
FIG. 5 is a MoS according to an embodiment of the present invention2-XPS plot of elemental sulphur in KF host guest compound;
FIG. 6 is a MoS according to an embodiment of the present invention2-XPS plot of potassium element in KF host guest compound;
FIG. 7 is a MoS according to an embodiment of the present invention2XPS plot of elemental fluorine in KF host-guest compounds.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
In the prior art, for MoS2The crystal material is prepared by adopting molybdenum sources such as sodium molybdate and the like and sulfur sources such as thiourea and the like through hydrothermal reaction at high temperature and high pressure. In the research of the scheme of the invention, the MoS prepared by the first step hydrothermal reaction is discovered2The crystal quality of the host material will greatly affect the feasibility of introducing the interlaminar intercalant between (002) crystal planes in the second hydrothermal reaction. Through comparative research, the MoS obtained by the first step hydrothermal reaction preparation2If the quality of the crystal material is not high, collapse occurs in the second hydrothermal reaction, and then lattice damage and erosion occur.
In the invention, MoS is prepared by strictly adjusting the first step hydrothermal reaction2The reaction conditions of the main material are adopted, so that a high-quality crystal structure is obtained, and the insertion of the fluoride into MoS can be realized only by adopting higher reaction conditions, higher reaction temperature, reaction time and higher fluoride concentration in the second step of hydrothermal reaction2The (002) crystal face of the crystal is between, and a high-quality electrochemical hydrogen production material is obtained.
In the implementation process of the scheme of the invention, in order to realize the adjustment of the mol percentage content of the interlayer intercalator in the catalytic material, 0.05-0.8mol/L of interlayer intercalator solution and high-quality MoS are selected2The crystal powder reacts, so that the molar percentage of the interlayer insertion agent in the catalytic material is regulated and controlled within the range of 0.2-7.5%. Experimental statistics show that the mole percentage of the interlayer intercalation agent in the catalytic material is directly related to the concentration of the interlayer intercalation agent solution, that is, the mole percentage of the interlayer intercalation agent in the catalytic material is 0.2% when the concentration is 0.05M, without any examples.
Example 1
2.42g (0.01mol) of sodium molybdate (Na) are weighed out2MoO4.2H2O), dissolved in 30mL of deionized water and ultrasonically dispersed for 30 minutes. 3.05g (0.04mol) of thiourea [ (NH) were weighed out2)2CS]Dissolved in 30mL of deionized waterAnd (4) ultrasonically dispersing for 30 minutes. And dropwise adding the thiourea aqueous solution into the sodium molybdate aqueous solution, and carrying out ultrasonic dispersion on the mixed solution for 30 minutes. After the ultrasonic treatment is finished, the mixed aqueous solution is subjected to constant volume to 80mL and transferred into a 100 mL high-pressure hydrothermal reaction kettle with a polytetrafluoroethylene lining, the reaction kettle is sealed, and then the reaction kettle is placed into a thermostat and heated to 200 ℃ for reaction for 24 hours. After the reaction is finished, naturally cooling, carrying out suction filtration, washing with deionized water and ethanol to be neutral, and removing soluble substances. Drying the finally obtained product in a vacuum drying oven for 6 h at the temperature of 60 ℃ to obtain MoS2A host material.
KF (2.788g) was weighed and dissolved in 80.0 mL of deionized water to prepare a solution of KF at a concentration of 0.6 mol/L. Then, 0.4 gMoS was weighed2The powder was added to the prepared KF solution. The mixed solution was transferred to a 80mL stainless steel autoclave lined with Teflon, sealed and held at 140 ℃ for 10 h. Collecting black product, filtering, and drying at 60 deg.C for 6 hr in vacuum chamber to obtain host KF-MoS2A composite material.
KF-MoS obtained in this example2The mole percent of KF in the composite material was about 5.5%, and it should be noted that the data here are approximations obtained by multiple statistical averages, not exact values, which range from about ± 0.5%.
Example 2
2.42g (0.01mol) of sodium molybdate (Na) are weighed out2MoO4.2H2O), dissolved in 30mL of deionized water and ultrasonically dispersed for 30 minutes. 3.05g (0.04mol) of thiourea [ (NH) were weighed out2)2CS]Dissolved in 30mL of deionized water and also ultrasonically dispersed for 30 minutes. And dropwise adding the thiourea aqueous solution into the sodium molybdate aqueous solution, and carrying out ultrasonic dispersion on the mixed solution for 30 minutes. After the ultrasonic treatment is finished, the mixed aqueous solution is subjected to constant volume to 80mL and transferred into a 100 mL high-pressure hydrothermal reaction kettle with a polytetrafluoroethylene lining, the reaction kettle is sealed, and then the reaction kettle is placed into a thermostat and heated to 200 ℃ for reaction for 24 hours. After the reaction is finished, naturally cooling, carrying out suction filtration, washing with deionized water and ethanol to be neutral, and removing soluble substances. Drying the finally obtained product in a vacuum drying oven for 6 h at the temperature of 60 ℃ to obtain MoS2A host material.
NaF (2.015g) was weighed and dissolved in 80.0 mL of deionized water to prepare a NaF solution having a concentration of 0.6 mol/L. Then, 0.4 g of the MoS obtained was weighed2The powder was added to the prepared NaF solution. The mixed solution was transferred to a 80mL stainless steel autoclave lined with Teflon, sealed and maintained at 160 ℃ for 9 h. Collecting black product, filtering, and drying at 60 deg.C for 6 hr in vacuum chamber to obtain NaF-MoS as host and guest2A composite material.
NaF-MoS obtained in this example2The mole percent of NaF in the composite material is about 5.5%, and it should be noted that the data herein are approximations obtained by multiple statistical averages, rather than exact values, which range from about + -0.5%.
Example 3
2.42g (0.01mol) of sodium molybdate (Na) are weighed out2MoO4.2H2O), dissolved in 30mL of deionized water and ultrasonically dispersed for 30 minutes. 3.05g (0.04mol) of thiourea [ (NH) were weighed out2)2CS]Dissolved in 30mL of deionized water and also ultrasonically dispersed for 30 minutes. And dropwise adding the thiourea aqueous solution into the sodium molybdate aqueous solution, and carrying out ultrasonic dispersion on the mixed solution for 30 minutes. After the ultrasonic treatment is finished, the mixed aqueous solution is metered to 80mL and transferred into a 100 mL high-pressure hydrothermal reaction kettle with a polytetrafluoroethylene lining, the reaction kettle is sealed, and then the reaction kettle is placed into a thermostat and heated to 210 ℃ for reaction for 22 h. After the reaction is finished, naturally cooling, carrying out suction filtration, washing with deionized water and ethanol to be neutral, and removing soluble substances. Drying the finally obtained product in a vacuum drying oven for 6 h at the temperature of 60 ℃ to obtain MoS2A host material.
NaF (2.700g) was weighed and dissolved in 80.0 mL of deionized water to prepare a solution of NaF at a concentration of 0.8 mol/L. Then, 0.4 g of the MoS obtained was weighed2The powder was added to the prepared NaF solution. The mixed solution was transferred to a 80mL stainless steel autoclave lined with Teflon, sealed and maintained at 160 ℃ for 8 h. Collecting black product, filtering, and drying at 60 deg.C for 6 hr in vacuum chamber to obtain NaF-MoS as host and guest2A composite material.
NaF-MoS obtained in this example2The mole percent NaF in the composite was about 7.5%, noting that the data is repeated several timesThe range of variation was about + -0.5% for the submultiples obtained by statistical averaging, not for the exact values.
Example 4: 0.01mol of potassium molybdate (K) is weighed2MoO4.2H2O), dissolved in 30mL of deionized water and ultrasonically dispersed for 30 minutes. 3.05g (0.04mol) of thiourea [ (NH) were weighed out2)2CS]Dissolved in 30mL of deionized water and also ultrasonically dispersed for 30 minutes. And dropwise adding the thiourea aqueous solution into the sodium molybdate aqueous solution, and carrying out ultrasonic dispersion on the mixed solution for 30 minutes. After the ultrasonic treatment is finished, the mixed aqueous solution is subjected to constant volume to 80mL and transferred into a 100 mL high-pressure hydrothermal reaction kettle with a polytetrafluoroethylene lining, the reaction kettle is sealed, and then the reaction kettle is placed into a thermostat and heated to 220 ℃ for reaction for 20 hours. After the reaction is finished, naturally cooling, carrying out suction filtration, washing with deionized water and ethanol to be neutral, and removing soluble substances. Drying the finally obtained product in a vacuum drying oven for 6 h at the temperature of 60 ℃ to obtain MoS2A host material.
NaF (2.358g) was weighed and dissolved in 80.0 mL of deionized water to prepare a solution of NaF at a concentration of 0.7 mol/L. Then, 0.4 g of the MoS obtained was weighed2The powder was added to the prepared NaF solution. The mixed solution was transferred to a 80mL stainless steel autoclave lined with Teflon, sealed and maintained at 200 ℃ for 8 h. Collecting black product, filtering, and drying at 60 deg.C for 6 hr in vacuum chamber to obtain NaF-MoS as host and guest2A composite material.
NaF-MoS obtained in this example2The mole percent of NaF in the composite material was about 6.5%, and it should be noted that the data herein are approximations obtained by multiple statistical averages, rather than exact values, which range from about + -0.5%.
TABLE 1 diffraction parameters of potassium fluoride-molybdenum sulfide composites
*KF0.5-MoS2、KF0.6-MoS2And KF0.75-MoS2Respectively represent potassium fluoride-molybdenum sulfide compounds prepared in 0.5, 0.6 and 0.75mol/L KF solution, and the restThe same is true.
As shown in FIG. 1 and FIGS. 2-7, the X-ray diffraction patterns of the samples obtained by the scheme of the invention show that after the reaction, the potassium fluoride-molybdenum sulfide compound still has a complete crystal structure and reacts with MoS which is not subjected to the second reaction2Compared with the crystal, the spacing between crystal faces of (002) in the crystal is increased to be more than 9.0A, which shows that the scheme realizes the effective introduction of sodium fluoride or potassium fluoride between crystal faces on the premise of fully ensuring the integrity of the crystal lattice.
The electrochemical hydrogen evolution activity test in the embodiment of the invention comprises the following steps: and carrying out an electrocatalytic hydrogen evolution experiment on the sample by adopting a three-electrode system. The working electrode was prepared as follows: weighing 0.10 g of sample to be detected and 0.15 g of graphite powder, grinding the sample to be detected and the graphite powder by using an agate mortar to obtain a fully mixed powder sample, dripping 0.1 ml of silicone oil into the fully mixed powder sample, and fully stirring to obtain a paste sample with fine and uniform particles. The sample was filled into a carbon paste electrode and polished. The Pt sheet electrode was used as a counter electrode, the saturated calomel electrode was used as a reference electrode, and the electrolyte solution was KOH at a concentration of 1.0M. The LSV linear scan test was performed at room temperature and pressure, with a scan rate of 10 mV/s. The resulting hydrogen evolution electrocatalytic curve is shown in figure 2.
The electrocatalytic hydrogen evolution curve of the potassium fluoride-molybdenum sulfide composite is shown in fig. 2. In 1.0mol/L KOH solution, when the working electrode is a graphite electrode, no electrocatalytic hydrogen evolution current exists in a potential scanning window. The potassium fluoride-molybdenum sulfide compound synthesized by different concentrations has a current density of 10 mA cm-2Pure MoS2Has an overpotential of 379mV, while complexes prepared in 0.25, 0.5, 0.6, 0.75mol/LKF have overpotentials of 329 mV,315 mV, 208 mV, 233 mV, respectively. The reduction values of the overpotential are respectively 50mV, 64 mV, 171 mV and 146 mV.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (4)
1. The application of the molybdenum sulfide/fluoride host-guest catalytic material in electrocatalytic hydrogen production is characterized in that the molybdenum sulfide/fluoride host-guest catalytic material comprises a molybdenum sulfide host compound and an interlayer intercalator guest compound, wherein the interlayer intercalator guest compound is inserted between (002) crystal faces of a molybdenum sulfide matrix, the interlayer intercalator guest compound is potassium fluoride or sodium fluoride,
the preparation method of the molybdenum sulfide/fluoride host-guest catalytic material comprises the following steps:
A. preparation of MoS2A host material;
B、MoS2adding a main material into a solution containing an interlayer intercalator compound, and intercalating the intercalator between (002) crystal faces of a molybdenum sulfide matrix under reaction conditions, wherein the interlayer intercalator compound is potassium fluoride or sodium fluoride,
step A is to prepare a molybdenum source solution and a sulfur source solution, dropwise add the sulfur source solution into the molybdenum source solution and fully mix the solution, heat the mixed solution in a high-pressure hydrothermal reaction kettle for reaction until the reaction is finished, separate, remove impurities and dry the mixed solution to obtain MoS2The material of the main body is selected from the group consisting of,
step B is to prepare an interlayer inserting agent compound solution and add an appropriate amount of MoS2Adding the host material into the interlaminar intercalant compound solution, heating and reacting in a high-pressure hydrothermal reaction kettle until the reaction is finished, separating, removing impurities, drying to obtain the molybdenum sulfide/fluoride host-guest catalytic material,
wherein the interplanar spacing between (002) crystal planes of the molybdenum sulfide matrix after insertion of the interlayer interposer compound is not less than 9.0A.
2. The use of a molybdenum sulfide/fluoride host-guest catalytic material in electrocatalytic hydrogen production as in claim 1, wherein the interlayer intercalator compound is present in an amount of 0.2 to 7.5 mole percent of the catalytic material.
3. The application of the molybdenum sulfide/fluoride host-guest catalytic material in electrocatalytic hydrogen production as claimed in claim 1, wherein the heating reaction in the high-pressure hydrothermal reaction kettle in the step A is at 220 ℃ at 200 ℃ for 20-24 h.
4. The application of the molybdenum sulfide/fluoride host-guest catalytic material in electrocatalytic hydrogen production as claimed in claim 1, wherein the heating reaction in the high-pressure hydrothermal reaction kettle in the step B is at 140-200 ℃ for 7-10 h.
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