CN112553641B - MXene and transition metal sulfide composite nano catalyst based on fiber framework and preparation method thereof - Google Patents
MXene and transition metal sulfide composite nano catalyst based on fiber framework and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a composite nano catalyst of MXene and transition metal sulfide based on a fiber framework and a preparation method thereof, belonging to the field of nano materials and catalysis. The method comprises the following steps: the preparation method comprises the steps of treating fibers, metal salts and transition metal carbide MXene prepared by electrostatic spinning by a low-temperature-low-oxygen impregnation method, freeze-drying to obtain MXene of a fiber framework, and then calcining at high temperature under a protective atmosphere to obtain the supported electrolytic water catalyst with a controllable structure and components and a nano structure. The invention takes the fiber as the MXene framework to overcome the defect that the layered structure of the transition metal carbide is easy to stack, so that the MXene has larger effective load specific surface area, the combination effect between the substrate and the load compound is improved, the catalyst shows more excellent effect and stability, and meanwhile, the preparation process is simple, efficient, green and environment-friendly, and has wide application prospect in the industrial process of hydrogen energy.
Description
Technical Field
The invention belongs to the field of nano materials, energy and catalysis, and particularly relates to an MXene and transition metal sulfide composite nano catalyst based on a fiber framework and a preparation method thereof.
Background
Fossil fuels including coal, petroleum, natural gas and the like belong to non-renewable resources and are exhausted in the future based on the current consumption rate. Meanwhile, the use of fossil fuels in large quantities brings about the harm of difficult reversion to the global environment, and serious environmental problems such as global warming and serious reduction of air quality caused by the emission of harmful gases such as dust particles, waste water, noise, sulfur oxides, nitrogen oxides and the like and carbon dioxide in large quantities cause wide social importance. The hydrogen energy is considered as the clean energy with the development prospect in the 21 st century due to the advantages of abundant resources, high combustion heat value, cleanness, environmental protection, no secondary pollution and the like. There are many industrial hydrogen production methods, wherein hydrogen products obtained by water electrolysis hydrogen production are clean and high in purity, and meanwhile, electric energy from solar energy, wind energy and the like can be stored as chemical energy to be utilized. At present, the widely used electrolyzed water catalyst is a precious metal with limited reserves and high price, and the development of the catalyst with low cost, stability and high efficiency is the key for realizing the industrial application of the electrolyzed water.
Since the first report in 2011, the two-dimensional layered MXenes nano material-transition metal carbide/nitride attracts extensive attention of researchers due to the graphene-like two-dimensional structure and excellent performance thereof. MXenes can be obtained by selective etching of the common MAX phase, which has the formula Mn+1XnTx(M is transition metal element, X is carbon or nitrogen element, T is surface group), has the advantages of unique multilayer structure, conductivity, high specific surface area, excellent chemical stability, hydrophilicity, good biocompatibility, abundant surface functional groups and the like. The characteristic of the special structure and the surface rich in functional groups provides excellent conditions for constructing the nano catalyst with stable structure and high performance. The Lan Huang et al prepared the MXene composite catalyst loaded with molybdenum disulfide, and the good electrocatalytic activity is shown, but the MXene lamella has the defect of easy stacking, so that the loading area of the molybdenum disulfide nanosheet is reduced, and the electrocatalytic performance of the MXene composite catalyst is influenced.
The unique physical and chemical properties of the nano-material make it popular with researchers. The nano material with unique structure and surface characteristic has very wide prospect when being applied to the field of electrocatalysis. The transition metal compound with the nano structure shows excellent electrochemical performance, so that the realization of precise regulation of the microstructure or the construction of a stable composite structure to improve the catalytic performance becomes one of the hot points of research.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a MXene and transition metal sulfide composite nano catalyst based on a fiber framework and a preparation method thereof.
The invention provides a supported water electrolysis hydrogen production catalyst based on MXene and transition metal sulfide composite nano structure of fiber framework and a preparation method thereof, aiming at a series of problems faced by the current water electrolysis catalyst. The problem that the layered structure of MXene is easy to stack can be solved by using the nano fibers as the framework, so that the structure has a very large effective loading area, and the catalytic activity and the stability of the composite material can be improved. The synthesis method is environment-friendly, low in energy consumption and easy to control, and can be used for large-scale production.
The purpose of the invention is realized by at least one of the following technical solutions.
The supported catalyst for hydrogen production by electrolyzing water, which is based on the MXene and transition metal sulfide composite nano structure of the fiber framework, consists of the fiber framework MXene uniformly supporting transition metal sulfide nano particles; the loading capacity of the nano particles is adjustable; the transition metal sulfide comprises at least one or more of molybdenum sulfide, cobalt sulfide and nickel sulfide.
The invention provides a preparation method of MXene and transition metal sulfide composite nano catalyst based on fiber framework, which comprises the following steps:
(1) dissolving a polymer in a high molecular solvent to obtain a spinning solution after complete dissolution, and preparing a polymer fiber membrane by an electrostatic spinning method;
(2) obtaining two-dimensional carbide powder by adopting a selective etching MAX method, adding the two-dimensional carbide powder into deionized water, and performing ultrasonic dispersion to obtain uniform titanium carbide dispersion liquid; adding metal salt into the titanium carbide dispersion liquid, uniformly dispersing by ultrasonic to obtain a suspension, soaking the polymer fiber membrane obtained in the step (1) in the suspension under a protective atmosphere, taking out, and drying to obtain a dipped membrane; this step can be carried out both at room temperature;
(3) and (3) placing the dipping film and the sulfur powder in the step (2) in a high-temperature furnace under a protective atmosphere (the dipping film is placed in the middle section of the high-temperature furnace, and the sulfur powder is placed at the upstream of the high-temperature furnace), and performing high-temperature calcination treatment (CAD method) to obtain the MXene and transition metal sulfide composite nano catalyst based on the fiber framework.
Further, the polymer fiber in the step (1) is more than one of polyvinyl alcohol (PVA), Polyacrylonitrile (PAN) and polyvinylpyrrolidone (PVP); the polymer fibers have a molecular weight of 104。
Preferably, the polymer fiber of step (1) is Polyacrylonitrile (PAN).
Further, the polymer solvent in the step (1) is one or more of Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO).
Preferably, the polymer solvent in step (1) is Dimethylformamide (DMF).
Further, in the spinning solution in the step (1), the mass fraction of the polymer is 5-20%.
Preferably, the electrostatic spinning method in step (1) uses an electrostatic spinning machine with a voltage of 20-30kv and an acceptance distance of 10-25 cm.
Further preferably, the electrostatic spinning method of step (1) uses an electrostatic spinning machine with a voltage of 28kv and an acceptance distance of 20 cm.
Further, the two-dimensional carbide powder in the step (2) is titanium carbide powder; the concentration of the titanium carbide dispersion liquid is 5-20 mg/mL; the metal salt is more than one of water-soluble chloride, nitrate, acetate and polyacid salts of molybdenum, cobalt and nickel; the mass ratio of the two-dimensional carbide powder (transition metal carbide MXene) to the metal salt is (1.0-10.0): 1.
preferably, the metal salt in step (2) is one or more of ammonium molybdate, ammonium tetrathiomolybdate, cobalt chloride and nickel chloride.
Preferably, the two-dimensional carbide powder in the step (2) is prepared by an etching method, and the etching time is 10-15 h.
Further preferably, the etching time is 12 h.
Further, the protective atmosphere in the step (2) is nitrogen or argon, and the dipping time of the polymer fiber membrane in the suspension is 1-6 h.
Preferably, the ultrasound in the step (2) is ultrasound by using a probe crushing ultrasonic machine; the power of the ultrasonic wave is 50-80W, and the time is 3-5 h.
Further preferably, the power of the ultrasound in the step (2) is 70W.
Further, the protective atmosphere in the step (3) is nitrogen or argon, and the mass ratio of the sulfur powder to the metal salt in the step (2) is (1.0-3.0): 1.
preferably, the protective atmosphere in step (3) is argon.
Further, the temperature of the calcination treatment in the step (3) is 500-.
The invention provides a composite nano catalyst of MXene and transition metal sulfide based on a fiber framework, which is prepared by the preparation method.
The invention prepares the nanometer composite catalyst of evenly loaded transition metal sulfide by preparing MXene of a fiber framework as a substrate and calcining at high temperature.
The invention takes the fiber as the MXene framework to overcome the defect that the layered structure of the transition metal carbide is easy to stack, so that the MXene has larger effective load specific surface area, the combination effect between the substrate and the load compound is improved, the catalyst shows more excellent effect and stability, and meanwhile, the preparation process is simple, efficient, green and environment-friendly, and has wide application prospect in the industrial process of hydrogen energy.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) compared with the conventional MXene-based catalyst, the MXene and transition metal sulfide composite nano-catalyst based on the fiber framework overcomes the problem that an MXene layered structure is easy to stack, and the effective load surface area is increased, so that the catalytic activity of the nano-composite catalyst is improved;
(2) the excellent performance of MXene adopted by the invention provides a very important basis for the catalyst, the excellent electrical property of the composite catalyst is endowed by the excellent electrical conductivity of the MXene, the electrochemical catalysis is facilitated, and meanwhile, the chemical coupling effect between the abundant chemical functional groups (including-O, -OH, -F) on the surface of the MXene and the nano structure of the transition metal sulfide provides higher chemical stability for the structure of the composite catalyst;
(3) the preparation method provided by the invention can realize the precise regulation and control of the microcosmic composition and the morphological structure of the MXene and transition metal sulfide composite nano catalyst based on the fiber framework, and provides a foundation for the diversity of the water electrolysis catalyst;
(4) the preparation method provided by the invention has the advantages of simple process, green and environment-friendly process, easiness for large-scale production and wide application prospect in the field of energy utilization.
Drawings
FIG. 1 is a scanning electron micrograph of titanium carbide used in an embodiment of the present invention;
FIG. 2 is a scanning electron microscope image of MXene and transition metal sulfide composite nano-catalyst based on fiber framework prepared in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of MXene and transition metal sulfide composite nano-catalyst based on fiber framework prepared in example 2 of the present invention;
FIG. 4a is a scanning electron microscope image of MXene and transition metal sulfide composite nano-catalyst based on fiber framework prepared in example 4 of the present invention;
FIG. 4b is a transmission electron microscope image of MXene and transition metal sulfide composite nano-catalyst based on fiber framework prepared in example 4 of the present invention;
FIG. 5 is a graph of the stability of MXene and transition metal sulfide composite nanocatalyst based on fiber framework prepared in example 4 of the present invention;
fig. 6 is a graph of the comparative results of MXene and transition metal sulfide composite nano-catalyst based on fiber framework and commercial Pt/C catalytic activities, prepared in the example of the present invention.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
A preparation method of MXene and transition metal sulfide composite nano-catalyst based on fiber framework comprises the following steps:
(1) 1g of polyacrylonitrile (PAN, molecular weight 10) was weighed4) Dissolving in 20g of N, N-Dimethylformamide (DMF), taking 5mL of the solution after complete dissolution, placing the solution in a needle cylinder, performing electrostatic spinning at a voltage of 28kv, and taking down the spinning fiber membrane after 5 h;
(2) 0.6g of titanium carbide powder (Ti after etching and drying) was weighed out3C2) Adding the obtained product into 30mL of deionized water, carrying out ultrasonic dissolution to obtain a titanium carbide dispersion liquid, then adding 0.06g of ammonium tetrathiomolybdate for dissolution, soaking the spinning fiber membrane obtained in the step (1) in the solution for 1h at room temperature under a nitrogen atmosphere, taking out the obtained product, and drying the obtained product to obtain a soaked membrane;
(3) and (3) under the protection of argon, placing the impregnated film obtained in the step (2) in a high-temperature furnace, placing 0.06g of sulfur powder at the upstream, wherein the calcining temperature is 500 ℃, the calcining time is 5h, and the product is a titanium carbide sheet layer taking fibers as a framework, and is loaded with uniformly distributed molybdenum disulfide nanosheets (MXene and transition metal sulfide composite nano-catalyst based on the fiber framework), and the average size is about 100-300 nm.
Example 2
A preparation method of MXene and transition metal sulfide composite nano-catalyst based on fiber framework comprises the following steps:
(1) 5g Polyacrylonitrile (PAN, molecular weight 10) was weighed4) Dissolving in 20g N, N-Dimethylformamide (DMF), placing 5mL into a syringe after completely dissolving, electrospinning at 28kv, and removing the spun fiber membrane after 5 h.
(2) 0.45g of titanium carbide powder (Ti after etching and drying) was weighed out3C2) Adding into 30mL deionized waterUniformly performing ultrasonic dissolution to obtain titanium carbide dispersion liquid, then adding 0.064g of ammonium molybdate to dissolve the titanium carbide dispersion liquid, soaking the spinning fiber membrane obtained in the step (1) in the solution for 5 hours at room temperature in a nitrogen atmosphere, taking out the spinning fiber membrane and drying the spinning fiber membrane to obtain a soaked membrane;
(3) and (3) under the protection of argon, placing the impregnated film obtained in the step (2) in a high-temperature furnace, placing 0.128g of sulfur powder at the upstream, wherein the calcining temperature is 700 ℃, the calcining time is 1h, and the product is a titanium carbide sheet layer taking fibers as a framework, loaded with uniformly distributed molybdenum disulfide nanosheets (MXene and transition metal sulfide composite nano-catalyst based on the fiber framework) and has the average size of about 100-300 nm.
Example 3
A preparation method of MXene and transition metal sulfide composite nano-catalyst based on fiber framework comprises the following steps:
(1) 3.53g polyacrylonitrile (PAN, molecular weight 10) was weighed4) Dissolving in 20g N, N-Dimethylformamide (DMF), placing 5mL into a syringe after completely dissolving, electrospinning at 28kv, and removing the spun fiber membrane after 5 h.
(2) 0.3g of two-dimensional titanium carbide powder (Ti after etching and drying) was weighed3C2) Adding the obtained product into 30mL of deionized water, carrying out ultrasonic dissolution to obtain a titanium carbide dispersion liquid, then adding 0.075g of cobalt chloride to dissolve the titanium carbide dispersion liquid, soaking the spinning fiber membrane obtained in the step (1) in the solution for 3 hours at room temperature under an argon atmosphere, taking out the obtained product, and drying the obtained product to obtain a soaked membrane;
(3) and (3) under the protection of argon, placing the impregnated film in the step (2) in a high-temperature furnace, placing 0.225g of sulfur powder at the upstream, wherein the calcining temperature is 600 ℃, the calcining time is 3h, and the product is a titanium carbide sheet layer taking fibers as a framework, wherein cobalt sulfide (MXene and transition metal sulfide composite nano catalyst based on the fiber framework) is uniformly distributed and loaded on the titanium carbide sheet layer, and the average size is about 100-300 nm.
Example 4
A preparation method of MXene and transition metal sulfide composite nano-catalyst based on fiber framework comprises the following steps:
(1) 2.22g polyacrylonitrile (PAN, molecular weight 10) was weighed4) Dissolving in 20g N, N-Dimethylformamide (DMF)And after the fiber is completely dissolved, 5mL of the fiber is placed in a needle cylinder, electrostatic spinning is carried out at the voltage of 28kv, and the spinning fiber membrane is taken down after 5 h.
(2) 0.15g of two-dimensional titanium carbide powder (Ti after etching and drying) was weighed3C2) Adding the obtained product into 30mL of deionized water, carrying out ultrasonic dissolution to obtain a titanium carbide dispersion liquid, then adding 0.15g of ammonium molybdate to dissolve the titanium carbide dispersion liquid, soaking the spinning fiber membrane obtained in the step (1) in the solution for 6 hours at room temperature under a nitrogen atmosphere, taking out the obtained product, and drying the obtained product to obtain a soaked membrane;
(3) and (3) under the protection of argon, placing the impregnated film obtained in the step (2) in a high-temperature furnace, placing 0.15g of sulfur powder at the upstream, wherein the calcining temperature is 800 ℃, the calcining time is 2 hours, and the product is a titanium carbide sheet layer taking fibers as a framework, and is loaded with uniformly distributed molybdenum disulfide nanosheets (MXene and transition metal sulfide composite nano-catalyst based on the fiber framework), and the average size is about 100-300 nm.
Fig. 2 is a scanning electron microscope image of the composite catalyst based on MXene and molybdenum disulfide nanosheet of the fiber framework (composite nanocatalyst based on MXene and transition metal sulfide of the fiber framework) prepared by using ammonium tetrathiomolybdate as a metal salt in example 1. From fig. 2, it can be seen that MXene (composite nano catalyst of MXene and transition metal sulfide based on fiber framework) and simple MXene (titanium carbide Ti) of fiber framework3C2) The layered structure is more extended and has a larger surface area than the layered structure. And the titanium carbide layer is loaded with nanoscale molybdenum disulfide. Meanwhile, as can be seen from a scanning chart (fig. 2), the fibers can also be used as a synergistic carrier of molybdenum disulfide, so that more excellent catalytic activity is endowed to the catalyst.
Fig. 3 is a scanning electron microscope image of the composite catalyst based on MXene and molybdenum disulfide nanosheet of the fiber framework (composite nanocatalyst based on MXene and transition metal sulfide of the fiber framework) prepared by using ammonium molybdate as a metal salt in example 2. The comparison in fig. 3 shows that in the composite catalyst obtained in this example, the loading amount of the molybdenum disulfide nanosheets on the MXene sheet layer of the fiber framework is significantly greater than that in fig. 1, and the size of the nanosheets is more uniform.
Example 4 composite catalyst prepared by changing the ratio of titanium carbide and ammonium molybdate (MXene and transition metal sulfide composite nanocatalyst based on fiber framework) to improve the stacking of molybdenum disulfide sheets is shown in scanning electron microscope as shown in FIG. 4a and transmission electron microscope as shown in FIG. 4 b. The nano-sheets on the surface are smaller in size and more uniformly distributed, so that molybdenum disulfide exposes more active sites, the conductivity of the two-dimensional layered material is kept, and the electron transmission efficiency is improved; the fiber can be used as MXene framework and can be used as synergistic carrier to load more molybdenum disulfide, so that the load rate is improved, and the catalytic activity of the composite material is improved.
Fig. 5 is a graph of the catalytic activity characterization of the fiber framework-based MXene and metal sulfide composite catalyst (fiber framework-based MXene and transition metal sulfide composite nano catalyst) prepared in example 4 of the present invention for hydrogen production by electrolyzing water under acidic conditions and the comparison result with the activity of the commercial Pt/C catalyst.
The test method comprises the following steps: using a three-electrode system at 0.5M H2SO4As an electrolyte, a composite catalyst (a composite nano catalyst based on MXene and transition metal sulfide of a fiber framework) based on MXene and molybdenum disulfide nanosheets of the fiber framework is loaded on a working electrode, and a calomel electrode is a reference electrode. The carbon rod is the counter electrode and the electrochemical workstation is CHI 600. As can be seen from FIG. 5, the catalyst prepared by the present invention has a current density of 10mA cm-2When the catalyst is used, the overpotential is 83mV (vs. RHE), which is close to the overpotential of 47mV (vs. RHE) of a commercial Pt/C catalyst under the same current density, and the catalyst shows excellent electrocatalytic activity and has wide application prospect.
FIG. 6 is a stability test of composite catalyst based on MXene and molybdenum disulfide nanosheet of fiber framework (composite nano catalyst based on MXene and transition metal sulfide of fiber framework) prepared in example 4 of the invention under acidic condition, and the stability test is 0.5M H2SO4The composite catalyst of MXene and molybdenum disulfide nanosheets based on a fiber framework is loaded on the working electrode as electrolyte, and the calomel electrode is a reference electrode. The carbon rod is the counter electrode and the electrochemical workstation is CHI 600. As can be seen from FIG. 6, the composite nano-catalyst of MXene and transition metal sulfide based on fiber framework prepared in example 4 of the invention is disclosedAnd when the voltage is on the way, the current density loss is 0.3 after 12h, excellent stability is shown, and a foundation is provided for industrial application of the high-voltage transformer.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (6)
1. A preparation method of MXene and transition metal sulfide composite nano catalyst based on fiber framework is characterized by comprising the following steps:
(1) dissolving a polymer in a high molecular solvent to obtain a spinning solution, and preparing a polymer fiber membrane by an electrostatic spinning method;
(2) adding the two-dimensional carbide powder obtained by adopting a selective etching MAX method into deionized water, and performing ultrasonic dispersion to obtain uniform titanium carbide dispersion liquid; adding metal salt into the dispersion liquid, uniformly dispersing by ultrasonic to obtain a suspension, soaking the polymer fiber membrane obtained in the step (1) in the suspension under a protective atmosphere, taking out, and drying to obtain a dipped membrane;
(3) placing the impregnated film and sulfur powder in the step (2) in a high-temperature furnace under a protective atmosphere, and calcining to obtain the MXene and transition metal sulfide composite nano catalyst based on the fiber framework;
the polymer in the step (1) is more than one of polyvinyl alcohol, polyacrylonitrile and polyvinylpyrrolidone;
in the spinning solution in the step (1), the mass fraction of the polymer is 5-20%;
the two-dimensional carbide in the step (2) is titanium carbide powder; the concentration of the titanium carbide dispersion liquid is 5-20 mg/mL; the metal salt is more than one of water-soluble chloride, nitrate, acetate and polyacid salts of molybdenum, cobalt and nickel; the mass ratio of the titanium carbide powder to the metal salt is (1.0-10.0): 1;
the mass ratio of the sulfur powder in the step (3) to the metal salt in the step (2) is (1.0-3.0): 1;
the temperature of the calcination treatment in the step (3) is 500-800 ℃, and the time of the calcination treatment is 1-5 h.
2. The method for preparing the MXene and transition metal sulfide composite nano catalyst based on the fiber framework of claim 1, wherein the polymer solvent in the step (1) is one or more of dimethylformamide and dimethyl sulfoxide.
3. The method for preparing MXene and transition metal sulfide composite nanocatalyst based on fiber framework according to claim 1, wherein the voltage of the electrostatic spinning machine used in the electrostatic spinning method of step (1) is 20-30kv, and the acceptance distance of the electrostatic spinning machine used in the electrostatic spinning method is 10-25 cm.
4. The method for preparing MXene and transition metal sulfide composite nano catalyst based on fiber framework of claim 1, wherein the protective atmosphere in step (2) is nitrogen or argon, and the dipping time of the polymer fiber membrane in the suspension is 1-6 h.
5. The method for preparing MXene and transition metal sulfide composite nano catalyst based on fiber framework of claim 1, wherein the protective atmosphere in step (3) is nitrogen or argon.
6. MXene and transition metal sulfide composite nanocatalyst based on fiber framework prepared by the preparation method of any one of claims 1 to 5.
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| CN111082051A (en) * | 2019-12-27 | 2020-04-28 | 华南理工大学 | Carbon fiber composite material containing single-layer MXene nanosheet and preparation and application thereof |
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