CN111545229A - Method for preparing MXene supported noble metal catalyst by ultrasonic-assisted method - Google Patents
Method for preparing MXene supported noble metal catalyst by ultrasonic-assisted method Download PDFInfo
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- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 92
- 239000003054 catalyst Substances 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002243 precursor Substances 0.000 claims abstract description 29
- 238000000227 grinding Methods 0.000 claims abstract description 24
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 146
- 239000006185 dispersion Substances 0.000 claims description 67
- 239000002904 solvent Substances 0.000 claims description 66
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 44
- 238000009210 therapy by ultrasound Methods 0.000 claims description 41
- 239000007788 liquid Substances 0.000 claims description 29
- 239000002253 acid Substances 0.000 claims description 28
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 24
- 229910052708 sodium Inorganic materials 0.000 claims description 24
- 239000011734 sodium Substances 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 239000007787 solid Substances 0.000 claims description 22
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 21
- 239000007769 metal material Substances 0.000 abstract description 4
- 229910052723 transition metal Inorganic materials 0.000 abstract description 4
- 150000003624 transition metals Chemical class 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 238000001035 drying Methods 0.000 description 20
- 238000003760 magnetic stirring Methods 0.000 description 20
- 238000001816 cooling Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 12
- 239000003446 ligand Substances 0.000 description 6
- 239000002082 metal nanoparticle Substances 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000851 scanning transmission electron micrograph Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
- C25B11/093—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds at least one noble metal or noble metal oxide and at least one non-noble metal oxide
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Abstract
The invention relates to a method for preparing MXene supported noble metal catalyst by an ultrasonic-assisted method, belonging to the field of material science, engineering technology and chemistry. The catalyst prepared by the method takes a two-dimensional transition metal material MXene as a carrier to load cluster or atomically dispersed noble metal Pt/Ir/Au/Rh/Ru/Pd. Firstly, preparing a carrier solution A with a certain concentration, adding a noble metal precursor solution B after uniform ultrasonic dispersion, adding the solution B into the solution A, stirring, and grinding and recovering a sample C in a mortar. Part of the supported catalyst can be annealed to obtain catalyst D in which the noble metal state is monatomic. The invention has the advantages of simple preparation process, high efficiency, good performance, low cost and the like.
Description
(2) Field of the invention
The invention relates to a method for preparing MXene supported noble metal catalyst by an ultrasonic-assisted method, belonging to the field of material science, engineering technology and chemistry.
(3) Background of the invention
Due to their high surface area, metal nanoparticles have become an important class of heterogeneous catalysts for a wide range of chemical transformations. Many parameters, including composition, size, shape and surface structure, have been shown to be important factors in influencing the catalytic performance of metal nanoparticles. To date, ligands on metal nanoparticles have been thought to hinder their catalytic action in most cases, and more recent studies have emphasized that surface ligands modulate the morphological synthesis and properties of metal nanoparticles as a challenge in the field of nanomaterials. Surface ligands lack an effective means for characterizing nanoparticle surface ligand coordination in modulating metal nanoparticle catalysis. The nanoclusters are expected to become an ideal system for solving the influence of surface ligands on the catalytic action of the metal nanoparticles. In order to clearly determine the role of surface ligands in catalysis, it is highly desirable to prepare ideal nanoclusters. Keeping all its structures intact. Recently, several metal nanoclusters having a well-defined composition or structure have been prepared.
The strength is not easy to control by simple stirring, the strength is too high, the liquid is uniformly distributed, but the precipitated particles are easy to break; the stirring intensity is too low, and the liquid cannot be uniformly mixed. We have found that ultrasound assistance not only aids in the rapid nucleation of the metal atoms generated by the in situ reaction, resulting in metal clusters of smaller size, but also promotes their uniform loading on the surface of the support. Based on an ultrasonic method, water is often used as a medium, so that reaction conditions are simplified, cost is reduced, and pollution is reduced.
(4) Summary of the invention
1. Objects of the invention
The invention aims to provide a method for preparing a noble metal loaded two-dimensional transition metal material Ti by an ultrasonic-assisted method2CTxThe method of the catalyst is characterized in that a noble metal precursor solution is reduced into a nano-scale cluster by an ultrasonic method, the advantages of firm carrier loading and multiple active sites are utilized, so that the metal precursor is uniformly and firmly dispersed on the carrier, and monatomic degradation performance is formed by annealing. The method can obtain the catalyst with good performance, high efficiency and low cost.
2. The invention of the technology
The key points of the invention are as follows:
(1) preparing a carrier dispersion liquid A with the mass-volume concentration of 3.0mg/mL by using a solvent, wherein the precursor is a metal monoatomic compound, the metal monoatomic compound is Pt, and the solvent is ethanol;
(2) the noble metal precursor solution B is 0.1mol/L of aqueous solution of chloroplatinic acid, chloroiridic acid, chloroauric acid, sodium chlororhodate, sodium chlororuthenate and sodium chloropalladate;
(3) carrying out ultrasonic treatment on the carrier dispersion liquid A prepared in the step (1) at room temperature to uniformly disperse the carrier dispersion liquid A, adding the noble metal precursor solution B in the step (2) into the ultrasonically treated dispersion liquid A, and stirring for 1h by using a magnetic stirrer;
(4) pouring the solution with uniform components after ultrasonic treatment into an agate mortar, and forcibly grinding for about 2 hours until the solution is completely volatilized and the color of the residual solid matter is uniform, so as to obtain a sample C;
(5) annealing the part of the sample C in inert gas to obtain the catalyst D with the noble metal state as a single atom. The invention relates to a method for preparing a noble metal loaded two-dimensional transition metal material Ti by an ultrasonic method2CTxThe method for preparing the catalyst is characterized in that the experimental steps are simple, the product performance is good, the cost is low, the nano-scale noble metal cluster is obtained by grinding and stably dispersed in the carrier, the uniformly dispersed noble metal monoatomic catalyst can be obtained by simple treatment, and the chemical performance is obviously improved.
(5) Attached drawings of the invention
FIG. 1 shows that the noble metal Pt prepared by the method of the invention is loaded with a two-dimensional transition metal material Ti2CTxScanning transmission electron microscopy images of the catalyst after annealing. a.20nm and b.10nm
FIG. 2 shows a Pt supported two-dimensional substrate Ti prepared by the method of the present invention2CTxHydrogen Evolution (HER) electrocatalytic activity and stability test performance diagram of the catalyst. a, b are 0.5M H in sequence2SO4Polarization curves in electrolyte, Tafel kinetics curves.
(6) Examples of the invention
The following describes embodiments of the method of the invention:
example 1
MXene(Ti2CTx) Preparation of Supported Pt noble Metal catalyst (Pt @ Ti)2CTx)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L chloroplatinic acid solution, wherein the solvent is water; of a carrierThe dispersion liquid is subjected to ultrasonic treatment to uniformly disperse the carrier in the solvent. 51uL of a 0.1mol/L chloroplatinic acid solution was added to Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. And pouring the solution with uniform components after ultrasonic treatment into an agate mortar, forcibly grinding for about 2 hours until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain the MXene supported Pt noble metal catalyst.
Example 2
MXene(Ti2CTx) Preparation of Supported Ir noble Metal catalyst (Ir @ Ti)2CTx)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L chloroiridic acid solution, wherein the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L chloroiridic acid solution was added to Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, forcibly grinding for about 2 hours until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Ir noble metal catalyst.
Example 3
MXene(Ti2CTx) Preparation of Supported Au noble Metal catalyst (Au @ Ti)2CTx)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L chloroauric acid solution, and the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L chloroauric acid solution is added to Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, grinding for about 2 hours by force until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Au noble metal catalyst.
Example 4
MXene(Ti2CTx) Preparation of Supported Rh noble Metal catalyst (Rh @ Ti)2CTx)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L of sodium chlororhodate solution, wherein the solvent is water; the carrier is uniformly dispersed in the solvent when the dispersion liquid of the carrier is subjected to ultrasonic treatment. 51uL of 0.1mol/L sodium chlororhodate solution is added into Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, grinding for about 2 hours by force until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Rh noble metal catalyst.
Example 5
MXene(Ti2CTx) Preparation of supported Ru noble metal catalyst (Ru @ Ti)2CTx)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L of chlorine ruthenate sodium solution, and the solvent is water; the carrier is uniformly dispersed in the solvent when the dispersion liquid of the carrier is subjected to ultrasonic treatment. 51uL of 0.1mol/L sodium chlororuthenate solution was added to Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, grinding for about 2 hours by force until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Ru noble metal catalyst.
Example 6
MXene(Ti2CTx) Preparation of Supported Pd noble Metal catalyst (Pd @ Ti)2CTx)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L sodium chloropalladate solution, and water as a solvent; sonicating the dispersion of the carrierThe carrier is uniformly dispersed in the solvent during the treatment. 51uL of 0.1mol/L sodium chloropalladate solution is added into Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, grinding for about 2 hours by force until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Pd noble metal catalyst.
Example 7
600 ℃ annealed MXene (Ti)2CTx) Preparation of Supported Pt noble Metal catalyst (Pt @ Ti)2CTx-600℃)。
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L chloroplatinic acid solution, wherein the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of a 0.1mol/L chloroplatinic acid solution was added to Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, grinding for about 2 hours by force until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Pt noble metal catalyst. Then putting the prepared catalyst into a tubular furnace, heating to 600 ℃, preserving heat for 1h, and cooling to obtain MXene (Ti) annealed at 600 DEG C2CTx) A supported Pt noble metal catalyst.
Example 8
600 ℃ annealed MXene (Ti)2CTx) Preparation of Supported Ir noble Metal catalyst (Ir @ Ti)2CTx-600℃)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L chloroiridic acid solution, wherein the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L chloroiridic acid solution was added to Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Will be ultrasonicPouring the solution with uniform components into an agate mortar, forcibly grinding for about 2 hours until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Ir noble metal catalyst. Then putting the prepared catalyst into a tubular furnace, heating to 600 ℃, preserving heat for 1h, and cooling to obtain MXene (Ti) annealed at 600 DEG C2CTx) A supported Ir noble metal catalyst.
Example 9
600 ℃ annealed MXene (Ti)2CTx) Preparation of Supported Au noble Metal catalyst (Au @ Ti)2CTx-600℃)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L chloroauric acid solution, and the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L chloroauric acid solution is added to Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, grinding for about 2 hours by force until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Au noble metal catalyst. Then putting the prepared catalyst into a tubular furnace, heating to 600 ℃, preserving heat for 1h, and cooling to obtain MXene (Ti) annealed at 600 DEG C2CTx) A supported Au noble metal catalyst.
Example 10
600 ℃ annealed MXene (Ti)2CTx) Preparation of Supported Rh noble Metal catalyst (Rh @ Ti)2CTx-600℃)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L of sodium chlororhodate solution, wherein the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L sodium chlororhodate solution is added into Ti2CTxDispersing the carrier in the solution, stirring for 1h by using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, grinding for about 2 hours by force until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Rh noble metal catalyst. Then putting the prepared catalyst into a tubular furnace, heating to 600 ℃, preserving heat for 1h, and cooling to obtain MXene (Ti) annealed at 600 DEG C2CTx) A supported Rh noble metal catalyst.
Example 11
600 ℃ annealed MXene (Ti)2CTx) Preparation of supported Ru noble metal catalyst (Ru @ Ti)2CTx-600℃)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L of chlorine ruthenate sodium solution, and the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L sodium chlororuthenate solution was added to Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, grinding for about 2 hours by force until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Ru noble metal catalyst. Then putting the prepared catalyst into a tubular furnace, heating to 600 ℃, preserving heat for 1h, and cooling to obtain MXene (Ti) annealed at 600 DEG C2CTx) A supported Ru noble metal catalyst.
Example 12
600 ℃ annealed MXene (Ti)2CTx) Preparation of Supported Pd noble Metal catalyst (Pd @ Ti)2CTx-600℃)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L sodium chloropalladate solution, and water as a solvent; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L sodium chloropalladate solution is added into Ti2CTxIn a carrier dispersion solution, usingStirring for 1h under magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, grinding for about 2 hours by force until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Pd noble metal catalyst. Then putting the prepared catalyst into a tubular furnace, heating to 600 ℃, preserving heat for 1h, and cooling to obtain MXene (Ti) annealed at 600 DEG C2CTx) A supported Pd noble metal catalyst.
Example 13
MXene (Ti) annealed at 900 deg.C2CTx) Preparation of Supported Pt noble Metal catalyst (Pt @ Ti)2CTx-900℃)。
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L chloroplatinic acid solution, wherein the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of a 0.1mol/L chloroplatinic acid solution was added to Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, grinding for about 2h until the solvent is completely volatilized and the color of the residual solid substance is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Pt noble metal catalyst. Then putting the prepared catalyst into a tubular furnace, heating to 900 ℃, preserving heat for 1h, and cooling to obtain MXene (Ti) annealed at 900 DEG C2CTx) A supported Pt noble metal catalyst.
Example 14
MXene (Ti) annealed at 900 deg.C2CTx) Preparation of Supported Ir noble Metal catalyst (Ir @ Ti)2CTx-900℃)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L chloroiridic acid solution, wherein the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L chloroiridic acid solution was added to Ti2CTxCarrier dispersion solutionIn (1), stirring is carried out for 1h by using magnetic stirring. Pouring the stirred solution with uniform components into an agate mortar, forcibly grinding for about 2 hours until the solvent is completely volatilized and the color of the residual solid substance is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Ir noble metal catalyst. Then putting the prepared catalyst into a tubular furnace, heating to 900 ℃, preserving heat for 1h, and cooling to obtain MXene (Ti) annealed at 900 DEG C2CTx) A supported Ir noble metal catalyst.
Example 15
MXene (Ti) annealed at 900 deg.C2CTx) Preparation of Supported Au noble Metal catalyst (Au @ Ti)2CTx-900℃)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L chloroauric acid solution, and the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L chloroauric acid solution is added to Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, forcibly grinding for about 2 hours until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Au noble metal catalyst. Then putting the prepared catalyst into a tubular furnace, heating to 900 ℃, preserving heat for 1h, and cooling to obtain MXene (Ti) annealed at 900 DEG C2CTx) A supported Au noble metal catalyst.
Example 16
MXene (Ti) annealed at 900 deg.C2CTx) Preparation of Supported Rh noble Metal catalyst (Rh @ Ti)2CTx-900℃)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L of sodium chlororhodate solution, wherein the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L sodium chlororhodate solution is added into Ti2CTxCarrierIn the dispersion solution, stirring was performed for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, forcibly grinding for about 2 hours until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Rh noble metal catalyst. Then putting the prepared catalyst into a tubular furnace, heating to 900 ℃, preserving heat for 1h, and cooling to obtain MXene (Ti) annealed at 900 DEG C2CTx) A supported Rh noble metal catalyst.
Example 17
MXene (Ti) annealed at 900 deg.C2CTx) Preparation of Supported Pd noble Metal catalyst (Pd @ Ti)2CTx-900℃)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L sodium chloropalladate solution, and water as a solvent; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L sodium chloropalladate solution is added into Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, forcibly grinding for about 2 hours until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Pd noble metal catalyst. Then putting the prepared catalyst into a tubular furnace, heating to 900 ℃, preserving heat for 1h, and cooling to obtain MXene (Ti) annealed at 900 DEG C2CTx) A supported Pd noble metal catalyst.
Example 18
MXene (Ti) annealed at 900 deg.C2CTx) Preparation of supported Ru noble metal catalyst (Ru @ Ti)2CTx-900℃)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L of chlorine ruthenate sodium solution, and the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L sodium chlororuthenate solution was added to Ti2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, forcibly grinding for about 2 hours until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Ti)2CTx) A supported Ru noble metal catalyst. Then putting the prepared catalyst into a tubular furnace, heating to 900 ℃, preserving heat for 1h, and cooling to obtain MXene (Ti) annealed at 900 DEG C2CTx) A supported Ru noble metal catalyst.
Example 19
MXene(Nb2CTx) Preparation of Supported Pt noble Metal catalyst (Pt @ Nb)2CTx)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Nb2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L chloroplatinic acid solution, wherein the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L chloroplatinic acid solution was added to Nb2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, grinding for about 2 hours by force until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain MXene (Nb)2CTx) A supported Pt noble metal catalyst.
Example 20
MXene(Ti2CTx) Preparation of supported Ir noble metal catalyst (Ir @ Nb)2CTx)
First, a carrier dispersion solution a was prepared: 20mL of 3mg/mL Ti2CTxThe solvent is ethanol; noble metal precursor solution B: 0.1mol/L chloroiridic acid solution, wherein the solvent is water; and (3) carrying out ultrasonic treatment on the dispersion liquid of the carrier to uniformly disperse the carrier in the solvent. 51uL of 0.1mol/L chloroiridic acid solution is added to Nb2CTxThe carrier dispersion solution was stirred for 1h using magnetic stirring. Pouring the solution with uniform components after ultrasonic treatment into an agate mortar, forcibly grinding for about 2 hours until the solution is completely volatilized and the color of the residual solid matter is uniform, and naturally drying to obtain the MXene(Nb2CTx) A supported Ir noble metal catalyst.
Claims (1)
1. A method for preparing MXene supported noble metal catalyst by ultrasonic-assisted method is characterized by comprising the following steps:
(1) preparing a carrier dispersion liquid A with the mass-volume concentration of 3.0mg/mL by using a solvent, wherein the precursor is a metal monoatomic compound, the metal monoatomic compound is Pt/Ir/Au/Rh/Ru/Pd, and the solvent is ethanol;
(2) the noble metal precursor solution B is 0.1mol/L of aqueous solution of chloroplatinic acid, chloroiridic acid, chloroauric acid, sodium chlororhodate, sodium chlororuthenate and sodium chloropalladate;
(3) carrying out ultrasonic treatment on the carrier dispersion liquid A prepared in the step (1) at room temperature to uniformly disperse the carrier dispersion liquid A, adding the noble metal precursor solution B in the step (2) into the ultrasonically treated dispersion liquid A, and stirring for 1h by using a magnetic stirrer;
(4) pouring the solution with uniform components after ultrasonic treatment into an agate mortar, and forcibly grinding for about 2 hours until the solution is completely volatilized and the color of the residual solid matter is uniform, so as to obtain a sample C;
(5) annealing the part of the sample C in inert gas to obtain the catalyst D with the noble metal state as a single atom.
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| CN116145173A (en) * | 2023-01-10 | 2023-05-23 | 华南理工大学 | Mxene supported Pd-Ag bimetallic composite nanoparticle hydrogen evolution electrocatalyst and preparation method and application thereof |
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