CN111744471B - Method for preparing self-supporting titanium dioxide supported noble metal catalyst - Google Patents
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention relates to a method for preparing a self-supporting titanium dioxide supported noble metal catalyst, belonging to the field of novel material preparation. The method takes a titanium sheet as a substrate, and obtains a titanium dioxide nanotube array through electrochemical anodic oxidation; by utilizing a constant current electrodeposition technology, noble metal nano particles are loaded on the titanium dioxide nanotube array, and the self-supporting titanium dioxide loaded low-noble metal catalyst can be obtained. The method adopted by the invention is mild and efficient, the preparation process is simple, the operability is strong, the method is suitable for mass production, and the prepared self-supporting titanium dioxide loaded low-noble metal catalyst has better application prospect in the fields of electro-catalysis and photoelectrocatalysis.
Description
Technical Field
The technical scheme of the invention relates to the technical field of novel material preparation, in particular to a method for preparing a self-supporting titanium dioxide supported noble metal catalyst by using an electroplating technology.
Background
To ensure efficient and sustainable use of clean Energy, the storage of Energy in the form of chemical Energy in Energy carriers has become an urgent need for sustainable development in today's society (World Energy Outlook, international Energy Agency, 2019, https:// www. Hydrogen (H) 2 ) As a zero-emission carbon-free fuel, the energy density of the fuel is 33.3 kW h kg -1 Approximately 2.5 times as much as traditional fossil fuels (e.g., methane, gasoline, and diesel), are considered the most promising carriers for clean Energy (renew. Sustatin. Energy rev., 2010, 14, 1293-1302). Therefore, it is necessary to develop a feasible and sustainable efficient hydrogen production strategy. Electrocatalytic or photoelectrocatalytic water splitting reaction (H) 2 O → H 2 + 1/2O 2 ) A clean, efficient and promising sustainable hydrogen production technology (adv. Sci., 2018, 5, 1700464; energy environ. Sci., 2016, 9, 709-728), but its large-scale commercial application remains limited in terms of cost and catalytic performance of hydrogen evolution catalysts: (1) The platinum group noble metal catalyst is expensive and has limited reserves, and large-scale application is difficult to realize; (2) The catalyst has poor stability, and the service life of maintaining high-efficiency electrolytic water to produce hydrogen is short.
In view of these limitations, in recent years, research on hydrogen evolution catalysts has been mainly conducted around low-noble metal materials (nat. Commu., 2015, 6, 6430 acs Appl. Mater. Interfaces, 2019, 11, 4047-4056), and some progress has been made to improve the hydrogen evolution performance of the catalysts while reducing the amount of noble metals used. However, most of the low noble metal catalysts are powders having zero-dimensional or one-dimensional nanostructures, and carbon materials are generally used as carriers for improving dispersibility. As the interaction between the noble metal active component and the carrier is weaker, binders such as Nafion and the like are required to be added, so that the activity of the catalyst is influenced, the active component is more prone to agglomeration and even falling off in the electrolytic process, and the activity is reduced due to the instability of the catalyst structure. And, H generated on the surface of the low noble metal catalyst 2 The molecules accumulate to a certain amount to form bubbles that can be desorbed and diffuse into the electrolyte solution. With the generation and gradual enrichment of hydrogen gas, adsorption of water molecules by the electrode surface is hindered, resulting in a decrease in catalyst activity and hydrogen production efficiency. Therefore, it is necessary to prepare a low noble metal catalyst with a self-supporting porous structure as an electrode material for hydrogen production by electrocatalysis or photoelectrocatalysis water decomposition so as to improve the hydrogen evolution energy efficiency and economic benefit.
Disclosure of Invention
Aiming at the problems of the existing hydrogen evolution catalyst, the invention provides a method for preparing a self-supporting titanium dioxide supported noble metal catalyst by using an electroplating technology, and the preparation method is mild and efficient, has a simple process and strong operability, and can be used for large-scale production.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for preparing a self-supporting titanium dioxide supported low-noble metal catalyst by utilizing an electroplating technology comprises the following steps:
a method for preparing a self-supporting titanium dioxide supported low-noble metal catalyst comprises the following steps:
(1) Placing the titanium sheet into a container containing glycerol, ammonium fluoride, water and concentrated H at normal temperature 2 SO 4 In the mixed solution, titanium dioxide nanotube arrays with different sizes can be obtained by an anodic oxidation method;
(2) And placing the obtained titanium dioxide nanotube array in a mixed aqueous solution in which sodium hypophosphite and noble metal are dissolved, and depositing at constant current at room temperature to obtain the self-supporting titanium dioxide supported noble metal catalyst.
Further, in the mixed solution in the step (1), glycerol, water and concentrated H 2 SO 4 The volume ratio of (A) to (B) is 400.
Further, in the step (1), the anode potential is controlled by using an anodic oxidation method, the voltage is 30-60V, and the oxidation time is 4-12h.
Further, in the step (2), the concentration of the noble metal in the mixed aqueous solution is 1.0-1.5 mM, the concentration of the sodium hypophosphite is 2.0-4.0 mM, the noble metal is platinum, palladium, gold or ruthenium, and the noble metal is dissolved in water in the form of salt or acid, such as chloroplatinic acid, palladium chloride, chloroauric acid or ruthenium chloride.
Further, in the step (2), the pH of the mixed aqueous solution is adjusted to be 4 with sodium bicarbonate.
Further, the current density of the constant current deposition in the step (2) is 0.4-0.6mA cm -1 The deposition time is 20-40min.
Further, the noble metal loading of the supported titania-supported noble metal catalyst prepared in the step (2) is 5-30 wt.%.
The invention has the beneficial effects that: in the synthesis process, the titanium dioxide nanotube array is prepared by adopting anodic oxidation, and nanotube arrays with different sizes can be obtained by regulating and controlling the anode voltage and the oxidation time; the constant current deposition method is adopted to load low noble metal, and noble metal nano particles with more uniform size and distribution can be prepared by regulating and controlling current. In terms of the process, the preparation method is simple and efficient, has good repeatability and low requirement on equipment, and is extremely easy to realize industrial production. The noble metal nano particles loaded by the method are highly dispersed, so that more active sites can be exposed, and the catalytic activity is improved; in addition, the noble metal nano particles loaded on the surface of the titanium dioxide nano tube array are not easy to agglomerate, thereby being beneficial to improving the catalytic stability and prolonging the cycle service life.
Drawings
FIG. 1 is a scanning electron microscope image of the lateral surface of a self-supporting titanium dioxide nanotube array obtained at a potential of 30V;
FIG. 2 is a scanning electron micrograph of the front surface of the self-supporting titanium dioxide nanotube array obtained at a potential of 60V;
FIG. 3 is a scanning electron micrograph of the lateral surface of the self-supporting titanium dioxide nanotube array obtained at a potential of 60V;
FIG. 4 is an XRD pattern of surface titanium dioxide from anodic titanium oxide wafers at a potential of 60V;
FIG. 5 is an EDS mapping plot of a self-supporting titanium dioxide nanotube array loaded with a low platinum catalyst front face;
FIG. 6 is an EDS energy spectrum of the self-supporting titania nanotube array loaded low platinum catalyst side;
FIG. 7 is a diagram of the catalytic performance of the self-supporting titanium dioxide nanotube array loaded with a low platinum catalyst for the electro-catalytic hydrogen evolution reaction.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
The method for preparing the self-supporting titanium dioxide nanotube array supported platinum catalyst comprises the following steps:
（1）at room temperature, 0.295 g of ammonium fluoride was added to 40 mL of glycerol, 1.2 mL of water and 0.1 mL of concentrated H 2 SO 4 The mixed solution of (2) is cooled to room temperature until the ammonium fluoride is completely dissolved, and a clear and transparent mixed solution is obtained.
(2) And (3) placing a titanium sheet of 1.5cm by 2.5cm in the mixed solution to serve as an anode of an electrolytic reaction, oxidizing for 4 hours at the voltage of 60V, taking out the titanium sheet, washing the residual electrolyte on the surface by deionized water, placing at room temperature for drying, and covering a layer of white substance on the surface of the titanium sheet to obtain the titanium dioxide nanotube array by anodic oxidation.
(3) The resulting self-supporting titania nanotube array was placed in a mixed aqueous solution of 1.16 mM chloroplatinic acid, 2.84 mM sodium hypophosphite (adjusted to pH =4 with sodium bicarbonate) at room temperature with 0.5 mA cm -1 Constant current deposition for 20 min to give a free-standing titania supported platinum catalyst (loading 16.5 wt.%).
The scanning electron microscope images of the titanium dioxide nanotube array obtained in this example are shown in fig. 2 and 3, and the titanium dioxide nanotube array with the pore diameter of about 200 nm and the length of about 1.8 μm was successfully prepared. EDS mapping and energy spectrum diagrams of the self-supporting titanium dioxide supported platinum catalyst are shown in figures 4 and 5, and it can be seen from the figures that Pt nano particles are successfully and uniformly supported on the titanium dioxide nano tubes through constant current deposition.
The influence of different catalysts on the performance of electrocatalytic hydrogen evolution was studied in 0.1M KOH electrolyte by Linear Sweep Voltammetry (LSV) (as shown in FIG. 7), respectively on TiO with an oxidation time of 8h 2 Pt/TiO obtained by electroplating on nanotube 2 Nanotube catalyst and TiO with oxidation time of 12h 2 Pt/TiO plated on nanotubes 2 The nanotube catalyst was compared to the Pt-C catalyst as shown. It can be seen that Pt/TiO 2 The nanotube catalyst has higher electrocatalytic hydrogen evolution activity than the Pt-C catalyst. It can be said that Pt supported TiO 2 The nanotube array formed on the nanotubes results in more active edge sites, significantly increasing the Pt/TiO 2 Catalytic hydrogen evolution activity of (1).
Example 2
The method for preparing the gold-loaded catalyst of the self-supporting titanium dioxide nanotube array comprises the following steps:
(1) At room temperature, 0.295 g of ammonium fluoride was added to 40 mL of glycerol, 2 mL of water and 0.1 mL of concentrated H 2 SO 4 The mixed solution of (2) is cooled to room temperature until the ammonium fluoride is completely dissolved, and a clear and transparent mixed solution is obtained.
(2) And (3) placing a titanium sheet of 1.5cm by 2.5cm in the mixed solution to serve as an anode of an electrolytic reaction, oxidizing for 6 hours at 50V, taking out the titanium sheet, washing the residual electrolyte on the surface by deionized water, placing at room temperature for drying, and covering a layer of white substance on the surface of the titanium sheet to obtain the titanium dioxide nanotube array by anodic oxidation.
(3) The resulting self-supporting titanium dioxide nanotube array was placed in a mixed aqueous solution of 1 mM chloroauric acid, 2 mM sodium hypophosphite (adjusted to pH =4 with sodium bicarbonate) at room temperature with 0.4 mA cm -1 Constant current deposition for 30 min to give a free-standing titania supported platinum catalyst (loading 17.8 wt.%).
Example 3
The method for preparing the self-supporting titanium dioxide nanotube array supported ruthenium catalyst comprises the following steps:
(1) At room temperature, 0.295 g of ammonium fluoride was added to 40 mL of glycerol, 2 mL of water and 0.1 mL of concentrated H 2 SO 4 The mixed solution of (2) is cooled to room temperature until the ammonium fluoride is completely dissolved, and a clear and transparent mixed solution is obtained.
(2) And (3) placing a titanium sheet of 1.5cm by 2.5cm in the mixed solution to serve as an anode of an electrolytic reaction, oxidizing for 10 hours at 40V, taking out the titanium sheet, washing the residual electrolyte on the surface by using deionized water, placing at room temperature for drying, and covering a layer of white substance on the surface of the titanium sheet to obtain the titanium dioxide nanotube array obtained by anodic oxidation.
(3) The resulting self-supporting titania nanotube array was placed in a mixed aqueous solution of 1.3 mM ruthenium chloride and 3mM sodium hypophosphite (adjusted to pH =4 with sodium bicarbonate) at room temperature with 0.4 mA cm -1 Current density, galvanostatic deposition of 35 min, resulting in a free-standing titania supported ruthenium catalyst (loading of 6.8 wt.%).
Example 4
The method for preparing the self-supporting titanium dioxide nanotube array supported palladium catalyst comprises the following steps:
(1) At room temperature, 0.295 g of ammonium fluoride was added to 40 mL of glycerol, 0.5 mL of water, and 0.1 mL of concentrated H 2 SO 4 The mixed solution of (2) is cooled to room temperature until the ammonium fluoride is completely dissolved, and a clear and transparent mixed solution is obtained.
(2) And (3) placing a titanium sheet of 1.5cm by 2.5cm in the mixed solution to serve as an anode of an electrolytic reaction, oxidizing for 12 hours at 30V, taking out the titanium sheet, washing the residual electrolyte on the surface by using deionized water, placing at room temperature for drying, and covering a layer of white substance on the surface of the titanium sheet to obtain the titanium dioxide nanotube array by anodic oxidation.
(3) The resulting self-supporting titania nanotube array was placed in a mixed aqueous solution of 1.5 mM palladium chloride, 4 mM sodium hypophosphite (adjusted to pH =4 with sodium bicarbonate) at room temperature with 0.6mA cm -1 Constant current deposition for 40min to give a self-supporting titania supported palladium catalyst (28.6 wt.%).
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (1)
1. The preparation method of the self-supporting titanium dioxide nanotube array supported platinum catalyst comprises the following steps:
(1) At room temperature, 0.295 g of ammonium fluoride was added to 40 mL of glycerol, 1.2 mL of water, and 0.1 mL of concentrated H 2 SO 4 In the mixed solution of (1), at room temperature until fluorinationCompletely dissolving ammonium to obtain a clear and transparent mixed solution;
(2) Placing a titanium sheet of 1.5cm x 2.5cm in the mixed solution obtained in the step (1) as an anode of an electrolytic reaction, oxidizing for 4 hours at a voltage of 60V, taking out the titanium sheet, washing the residual electrolyte on the surface with deionized water, placing at room temperature for drying, and covering a layer of white substance on the surface of the titanium sheet to obtain a titanium dioxide nanotube array by anodic oxidation;
(3) Placing the obtained self-supporting titanium dioxide nanotube array in a mixed aqueous solution of 1.16 mM chloroplatinic acid and 2.84 mM sodium hypophosphite, adjusting the pH of the mixed aqueous solution to =4 by sodium bicarbonate, and adjusting the pH of the mixed aqueous solution to 0.5 mA cm at room temperature -1 Constant current deposition for 20 min to obtain a self-supported titania supported platinum catalyst with a loading of 16.5 wt.%.
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