CN110961131A - Pt/C-N composite electro-catalytic material with efficient hydrogen evolution performance and preparation method thereof - Google Patents
Pt/C-N composite electro-catalytic material with efficient hydrogen evolution performance and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 38
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000001257 hydrogen Substances 0.000 title claims abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 19
- 239000002082 metal nanoparticle Substances 0.000 claims abstract description 15
- 239000002028 Biomass Substances 0.000 claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 claims abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 238000011068 loading method Methods 0.000 claims abstract description 5
- 238000004873 anchoring Methods 0.000 claims abstract description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 4
- 241000220259 Raphanus Species 0.000 claims description 25
- 235000006140 Raphanus sativus var sativus Nutrition 0.000 claims description 25
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- 230000008014 freezing Effects 0.000 claims description 13
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- 239000007789 gas Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 150000004687 hexahydrates Chemical class 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 4
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 150000005837 radical ions Chemical class 0.000 claims description 4
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- 230000000694 effects Effects 0.000 abstract description 2
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 35
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- 239000002243 precursor Substances 0.000 description 11
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- 229910052697 platinum Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 229910000510 noble metal Inorganic materials 0.000 description 2
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/33—Electric or magnetic properties
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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Abstract
The invention relates to a Pt/C-N composite electro-catalytic material with high-efficiency hydrogen evolution performance and a preparation method thereof, belonging to the technical field of energy catalytic conversion. The catalyst is formed by anchoring Pt metal nanoparticles on the surface of a nitrogen-doped biomass carbon material in situ, wherein the particle size of the Pt metal nanoparticles in the Pt/C-N composite electro-catalytic material is about 1nm-10nm, the exposed crystal face is a {111} active crystal face, and the loading capacity is 3-25 wt%. The N atoms are doped in situ in the biomass carbon material in the Pt/C-N composite electro-catalytic material provided by the invention, the Pt metal nanoparticles are uniformly loaded on the biomass carbon material, the loading capacity is controllable, the grain size is adjustable, and the electro-catalytic hydrogen evolution activity is excellent.
Description
Technical Field
The invention relates to a Pt/C-N composite electro-catalytic material with high-efficiency hydrogen evolution performance and a preparation method thereof, belonging to the technical field of energy catalytic conversion.
Background
Since the 21 st century, people are very urgent for the development of new clean energy, improvement of energy utilization efficiency, environmental pollution treatment and other sustainable development technologies for solving the problems of energy, environment and the like. Chemical reaction control is the core science and technology of energy conversion, petrochemical industry, environmental problem solving and the like, a catalysis technology is one of representative technologies for reducing chemical reaction activity, accelerating chemical reaction rate, improving production efficiency and energy utilization rate, is a 'basic stone' in the fields of energy, chemical industry, even environmental protection and the like, and the innovative research of a high-efficiency composite catalyst has very important influence on the alleviation of energy and environmental problems.
Platinum (Pt) is a noble metal micromolecule with unique activation performance, and because the d electron orbit is not filled, reactants are easily adsorbed on the surface, the strength is moderate, an intermediate active compound is favorably formed, and the catalytic activity is higher. Moreover, the catalyst has strong catalytic selectivity, convenient preparation and small usage amount. In the catalytic reaction, platinum is considered as the most advanced catalytic material and has wide application prospect in catalysis because the platinum is in the best state of hydrogen adsorption Gibbs free energy (delta GH), and only a negligible overpotential is needed to realize high current. At this stage, the development of nanocatalysts mainly focuses on two directions: firstly, the important research is to further reduce the size of the nano catalyst, increase the effective surface area of the metal catalyst, improve the utilization rate of the noble metal of the catalyst and reduce the production cost; secondly, the technical problem of stable performance control of the nano-catalyst is solved, and the nano-catalyst which has good structural stability, high dispersion degree of catalytic active sites, high catalytic efficiency and can be recycled is developed.
Aiming at the problems, the invention directly realizes that the N-doped C material and the metal Pt nano particles are uniformly and stably loaded on the carbon material in one step by taking white radish as a carrier and Pt as an active component through the processes of ion exchange, chemical bond anchoring, in-situ carbonization-co-reduction treatment and the like, obtains the Pt/C-N composite electro-catalytic material with high-efficiency hydrogen evolution performance, and lays a theoretical foundation for promoting the wide application of the metal nano catalyst in the fields of energy, chemical industry, environmental protection and the like.
Disclosure of Invention
The invention aims to provide a Pt/C-N composite electro-catalytic material with high-efficiency hydrogen evolution performance and a preparation method thereof, which are used for solving the problems of low catalytic activity, high preparation cost and difficulty in realizing large-scale utilization of the existing catalyst.
In order to realize the purpose, the invention designs a Pt/C-N composite electro-catalytic material with high-efficiency hydrogen evolution performance and a preparation method thereof, and the technical scheme adopted by the invention is as follows:
a Pt/C-N composite electro-catalytic material with high hydrogen evolution performance comprises a white radish biochar carrier and Pt metal nanoparticles dispersed in the carrier. The Pt metal nanoparticles are formed by anchoring on the surface of a biomass carbon material in situ, N atoms are doped in the biomass carbon material in the Pt/C-N composite electro-catalytic material in situ, and the loading capacity of the Pt metal nanoparticles is 3-25 wt%.
In the scheme, the size of the Pt metal nano particles is adjustable within the range of 1nm-10nm, and the exposed crystal face is a {111} active crystal face.
The preparation method of the Pt/C-N composite electro-catalytic material with high-efficiency hydrogen evolution performance comprises the steps of taking white radish as a biological carbon carrier and taking chloroplatinic acid hexahydrate as a precursor solution, soaking the white radish and distilled water, and then putting the white radish into the chloroplatinic acid solution for soaking, so that chloroplatinic acid radical ions are fully diffused and form bonds with cellulose, phospholipid bilayers, membrane proteins, saccharides and glycolipids in cell walls and membranes. And then freeze-drying the radish blocks in a freeze dryer to obtain dried radish blocks stably combined with chloroplatinic acid radical ions, then placing the dried radish blocks in a tubular furnace, carrying out heat treatment in a set environment, and taking out the radish blocks after cooling to obtain the Pt/C-N composite electro-catalytic material.
According to the scheme, the white radish is cut into blocks with the side length of 1-2 cm and the thickness of 1-3 mm, and is soaked in distilled water for 1-5 hours.
According to the scheme, the concentration of the chloroplatinic acid solution is within the range of 1mmol/L-0.2mol/L, and the immersion time is 0.5-8 hours.
According to the scheme, the temperature of a cold trap of the freeze dryer is-40 ℃ to-60 ℃, the freezing time is 0.5 to 1 day, the vacuum degree is 1 to 100Pa, and the drying time is 2 to 3 days.
According to the scheme, the heat treatment setting environment is any one atmosphere of nitrogen, argon, nitrogen/hydrogen mixed gas or argon/hydrogen mixed gas, the heat treatment temperature is 400-1000 ℃, and the reaction time is 2-5 hours.
The invention has the following advantages:
the invention provides a Pt/C-N composite electro-catalytic material with high-efficiency hydrogen evolution performance and a preparation method thereof, and the Pt/C-N composite electro-catalytic material has the advantages that:
(1) according to the electrocatalytic material, N atoms are doped in the biomass carbon material in situ, and Pt metal nanoparticles can be anchored on the surface of the nitrogen-doped biomass carbon material in situ;
(2) the Pt metal nanoparticles can be uniformly loaded on the biomass carbon material, the loading capacity is controllable, and the grain size is adjustable;
(3) the biomass carbon material and the Pt metal nanoparticles in the prepared composite electro-catalytic material are tightly combined, so that the stability of the electro-catalytic material in a catalytic reaction is greatly improved;
(4) the preparation method is simple to operate, low in cost and strong in universality.
Drawings
Fig. 1 is a transmission electron microscope image provided in embodiment 1 of the present invention.
Figure 2 is an XRD pattern provided by example 1 of the present invention.
FIG. 3 shows the electrocatalytic hydrogen production performance of Pt metal nanoparticles and commercial Pt/C in 0.5M sulfuric acid provided in example 1 of the present invention.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
Raw materials:
the biological carbon material (white radish) is a commercial raw material
The chloroplatinic acid hexahydrate is used as raw material of alatin official net
White radish was cut into 1 × 2cm pieces, and the pieces were immersed in a 0.08mol/L chloroplatinic acid precursor solution for 6 hours.
After the impregnation is finished, the sample is subjected to freeze drying, wherein the freezing temperature is-60 ℃, the vacuum degree is 1Pa, the freezing time is 1 day, and the drying time is 2 days, so that the biochar precursor capable of maintaining the cell structure of the biochar material is obtained.
Carbonizing the biological carbon precursor at the carbonization temperature of 600 ℃, wherein the heating rate is 2 ℃/min, the heat preservation time is 2 hours, and the protective atmosphere is Ar gas, so that the Pt/C-N composite electro-catalytic material is obtained.
The electrochemical hydrogen evolution performance of the biological porous carbon material with the loaded Pt metal nano particles is tested by taking the biological porous carbon material as the catalyst, and the current density is 100mA/cm2The potential of the counter hydrogen electrode was 77mV and the Tafel efficiency was 23 mV/dec.
Example 2
Raw materials:
the biological carbon material (white radish) is a commercial raw material
The chloroplatinic acid hexahydrate is used as raw material of alatin official net
White radish was cut into 1 × 2cm pieces, and the pieces were immersed in 0.04mol/L chloroplatinic acid precursor solution for 6 hours.
After the impregnation is finished, the sample is subjected to freeze drying, wherein the freezing temperature is-60 ℃, the vacuum degree is 1Pa, the freezing time is 1 day, and the drying time is 2 days, so that the biochar precursor capable of maintaining the cell structure of the biochar material is obtained.
Carbonizing the biological carbon precursor at the carbonization temperature of 600 ℃, wherein the heating rate is 2 ℃/min, the heat preservation time is 2 hours, and the protective atmosphere is Ar gas, so that the Pt/C-N composite electro-catalytic material is obtained.
Example 3
Raw materials:
the biological carbon material (white radish) is a commercial raw material
The chloroplatinic acid hexahydrate is used as raw material of alatin official net
White radish was cut into 1 × 2cm pieces, and the pieces were immersed in a 0.12mol/L chloroplatinic acid precursor solution for 6 hours.
After the impregnation is finished, the sample is subjected to freeze drying, wherein the freezing temperature is-60 ℃, the vacuum degree is 1Pa, the freezing time is 1 day, and the drying time is 2 days, so that the biochar precursor capable of maintaining the cell structure of the biochar material is obtained.
Carbonizing the biological carbon precursor at the carbonization temperature of 600 ℃, wherein the heating rate is 2 ℃/min, the heat preservation time is 2 hours, and the protective atmosphere is Ar gas, so that the Pt/C-N composite electro-catalytic material is obtained.
Example 4
Raw materials:
the biological carbon material (white radish) is a commercial raw material
The chloroplatinic acid hexahydrate is used as raw material of alatin official net
White radish was cut into 1 × 2cm pieces, and the pieces were immersed in a 0.08mol/L chloroplatinic acid precursor solution for 6 hours.
After the impregnation is finished, the sample is subjected to freeze drying, wherein the freezing temperature is-60 ℃, the vacuum degree is 1Pa, the freezing time is 1 day, and the drying time is 2 days, so that the biochar precursor capable of maintaining the cell structure of the biochar material is obtained.
Carbonizing the biological carbon precursor at the carbonization temperature of 400 ℃, wherein the heating rate is 2 ℃/min, the heat preservation time is 2 hours, and the protective atmosphere is Ar gas, so that the Pt/C-N composite electro-catalytic material is obtained.
Example 5
Raw materials:
the biological carbon material (white radish) is a commercial raw material
The chloroplatinic acid hexahydrate is used as raw material of alatin official net
The white radish was cut into 1 × 2cm pieces, and immersed in a 0.08mol/L chloroplatinic acid-leaching precursor solution for 6 hours.
After the impregnation is finished, the sample is subjected to freeze drying, wherein the freezing temperature is-60 ℃, the vacuum degree is 1Pa, the freezing time is 1 day, and the drying time is 2 days, so that the biochar precursor capable of maintaining the cell structure of the biochar material is obtained.
Carbonizing the biological carbon precursor at the carbonization temperature of 800 ℃, wherein the heating rate is 2 ℃/min, the heat preservation time is 2 hours, and the protective atmosphere is Ar gas, so that the Pt/C-N composite electro-catalytic material is obtained.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (6)
1. A Pt/C-N composite electro-catalytic material with high-efficiency hydrogen evolution performance is characterized in that: the Pt/C-N composite electro-catalytic material is formed by anchoring Pt metal nanoparticles on the surface of a biomass carbon material in situ, N atoms are doped in the biomass carbon material in situ, and the loading capacity of the Pt metal nanoparticles is 3-25 wt%.
2. The Pt/C-N composite electrocatalytic material of claim 1, wherein: the size of the Pt metal nano particles is adjustable within the range of 1nm-10nm, and the exposed crystal face is a {111} active crystal face.
3. The preparation method of the Pt/C-N composite electro-catalytic material with high hydrogen evolution performance according to claim 1, characterized in that: the method comprises the following steps:
(1) completely dissolving chloroplatinic acid hexahydrate in distilled water to form a chloroplatinic acid solution; cutting white radish into blocks with side length of 1-2 cm and thickness of 1-3 mm, soaking in distilled water for 1-5 hr, taking out, soaking in chloroplatinic acid solution to make chloroplatinic acid radical ions fully diffuse and form bonds with cellulose, phospholipid bilayer, membrane protein, saccharide and glycolipid in cell wall and membrane;
(2) and transferring the soaked white radish blocks into a cold trap of a freeze dryer, freezing completely, putting the white radish blocks into a drying chamber for vacuum freeze drying to obtain dried white radish blocks stably combined with chloroplatinic acid radical ions, putting the dried white radish blocks into a tubular furnace, carrying out heat treatment in a set environment, and taking out the blocks after cooling to obtain the Pt/C-N composite electro-catalytic material.
4. The preparation method of the Pt/C-N composite electro-catalytic material with high hydrogen evolution performance according to claim 3, characterized in that: the concentration of the chloroplatinic acid solution used in the step (1) is within the range of 1mmol/L-0.2mol/L, and the immersion time is 0.5-8 hours.
5. The preparation method of the Pt/C-N composite electro-catalytic material with high hydrogen evolution performance according to claim 3, characterized in that: the temperature of the cold trap used in the step (2) is-40 ℃ to-60 ℃, the freezing time is 0.5 to 1 day, the vacuum degree is 1 to 100Pa, and the drying time is 2 to 3 days.
6. The preparation method of the Pt/C-N composite electro-catalytic material with high hydrogen evolution performance according to claim 3, characterized in that: the set environment in the step (2) is any one atmosphere of nitrogen, argon, nitrogen/hydrogen mixed gas or argon/hydrogen mixed gas, the heat treatment temperature is 400-1000 ℃, and the reaction time is 2-5 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112275282A (en) * | 2020-11-03 | 2021-01-29 | 大连海事大学 | Preparation method and application of Pt nanoparticle-loaded biochar catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112275282A (en) * | 2020-11-03 | 2021-01-29 | 大连海事大学 | Preparation method and application of Pt nanoparticle-loaded biochar catalyst |
| CN112275282B (en) * | 2020-11-03 | 2023-07-04 | 大连海事大学 | Preparation method and application of Pt nanoparticle-loaded biochar catalyst |
| CN113388844A (en) * | 2021-05-26 | 2021-09-14 | 广东省科学院资源利用与稀土开发研究所 | Preparation method and application of low-platinum catalyst |
| WO2023071504A1 (en) * | 2021-10-28 | 2023-05-04 | 中国汽车技术研究中心有限公司 | Biomass in-situ reduction noble metal-based fuel cell catalyst |
| CN115078498A (en) * | 2022-06-13 | 2022-09-20 | 山西大学 | Biomass carbon material loaded metal nanoparticle catalyst and preparation method thereof |
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