A ligand protects pt 6 Sub-nano cluster and its preparation method as well as a catalyst and its preparation method and application

A sub-nanometer and catalyst technology, applied in the field of electrochemistry, can solve problems affecting catalyst stability and reducing catalyst activity, and achieve high hydrogen oxidation catalytic activity, high mass activity, and good stability

Active Publication Date: 2021-12-24
CHINA UNIV OF PETROLEUM (EAST CHINA) +1
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  • Description
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Problems solved by technology

Theoretically, as the particle size of Pt decreases, the electrochemical surface area can be increased to increase the H 2 Active sites for adsorption and dissociation can improve catalytic activity, but in the actual production and application process, too small particle size (such as single-atom Pt) is prone to agglomeration, which will affect the stability of the catalyst and reduce the activity of the catalyst

Method used

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  • A ligand protects pt <sub>6</sub> Sub-nano cluster and its preparation method as well as a catalyst and its preparation method and application
  • A ligand protects pt <sub>6</sub> Sub-nano cluster and its preparation method as well as a catalyst and its preparation method and application
  • A ligand protects pt <sub>6</sub> Sub-nano cluster and its preparation method as well as a catalyst and its preparation method and application

Examples

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preparation example Construction

[0030] The present invention provides a ligand-protected Pt 6The preparation method of the sub-nano cluster includes the following steps: mixing a ligand solution, chloroplatinic acid, a reducing agent and an alcohol for a reduction reaction to obtain a reduction product solution, wherein the reduction product is a ligand-protected Pt 6 Sub-nano cluster; the ligand is a phosphine compound, the solvent of the ligand solution is a weakly polar solvent, the polarity of the weakly polar solvent is 1-5, and the reducing agent is an amine complex thing.

[0031] In the present invention, the phosphine compound is preferably one or more of triphenylphosphine, tributylphosphine, diphenylphosphine and dimethylphenylphosphine, more preferably triphenylphosphine; The amine complex is preferably one of borane tert-butylamine complex, boron trifluoride-monoethylamine complex, borane-trimethylamine complex and triethylboraneamine complex or Several, more preferably borane tert-butylamine ...

Embodiment 1

[0051] (1) 200 μL of a 20 mmol / L toluene solution of triphenylphosphine, 200 μL of a 20 mmol / L chloroplatinic acid aqueous solution, and 5 mL of ethanol were thoroughly mixed.

[0052] (2) the mixed solution of step (1) gained is vigorously stirred and the ethanolic solution of the borane tert-butylamine complex of 30 μL 50 mmol / L is added, reacted for 30 minutes, to dark brown ligand protection Pt 6 Subnanocluster solutions.

[0053] figure 1 Protection of Pt for the resulting ligand 6 UV absorption spectra (a) and ESI-MS spectra (b) of subnanoclusters; in figure 1 In the UV absorption spectrum in , Pt appears at 385 and 355 nm 6 The characteristic absorption peak of the sub-nanocluster, the peak at m / z=2400Da in the ESI-MS spectrum, the combined UV absorption spectrum and the ESI-MS spectrum, and the calculation based on the molecular weight of the intermediate product, this example successfully synthesized a stable Presence of Pt 6 subnanoclusters.

Embodiment 2

[0055] (1) Take 5 mL of the ligand-protected Pt prepared in Example 1 6 The sub-nanocluster solution was mixed with 10, 20, and 40 mg of carbon black, respectively, and then 45 mL of ethanol was added, and the mixture was uniformly mixed and stirred for 6 hours to obtain carbon-supported Pt with a loading of 8%, 4%, and 2%, respectively. 6 Subnanocluster solutions.

[0056] (2) The solution obtained in step (1) is subjected to suction filtration separation, and then vacuum-dried at room temperature overnight to obtain carbon-supported Pt 6 Subnanocluster catalysts.

[0057] figure 2 Pt on carbon with a loading of 2% 6 Electron microscope images of sub-nanocluster catalysts, in which (a) is a spherical aberration electron microscope image, (b) is a TEM image, (c) and (d) are HAADF-STEM images of different parts; according to figure 2 It can be seen that Pt 6 The sub-nanoclusters are uniformly dispersed on the carbon black surface.

[0058] Hydrogen electrocatalytic oxid...

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Abstract

The invention relates to the field of electrochemical technology and provides a ligand-protected Pt 6 Subnanometer cluster and its preparation method, a catalyst, its preparation method and application. In the present invention, phosphine compounds are used as ligands, weakly polar solvents with a polarity value of 1 to 5 are used as solvents for ligands, and amine complexes are used as reducing agents. The quantity is precisely controlled to realize the Pt 6 Synthesis of subnanometer clusters. Carbon supported Pt provided by the invention 6 Subnanometer cluster catalysts including carbon supports and ligand-protected Pt supported on carbon supports 6 Subnanometer clusters, under ligand protection, Pt 6 Sub-nanometer clusters can exist stably, and are not easy to agglomerate in the catalytic process; the carbon-supported Pt provided by the invention 6 Subnano-cluster catalysts have ultra-high mass activity and good stability for hydrogen oxidation reactions, and their mass activity and durability are higher than commercial Pt / C catalysts, which have broad application prospects.

Description

technical field [0001] The invention relates to the technical field of electrochemistry, in particular to a ligand-protected Pt 6 Sub-nano cluster and its preparation method and a catalyst and its preparation method and application. Background technique [0002] Hydrogen energy is regarded as the clean energy with the most development potential in the 21st century, and the efficient use of hydrogen energy has become the trend of the development of a new clean society in the future. Among them, the hydrogen fuel cell is an efficient power generation device that relies on hydrogen to obtain green electricity. [0003] Commercialized proton exchange membrane fuel cells (PEMFCs) have been able to achieve low loadings of noble metal Pt (≤0.05 mg Pt cm -2 ) to achieve high catalytic activity for the hydrogen oxidation reaction (HOR), but the oxygen reduction reaction (ORR) that occurs at the cathode side requires a high Pt loading (0.2–0.4 mg due to slow kinetics). Pt cm -2...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/88H01M4/92H01M8/22
CPCH01M4/8878H01M4/926H01M8/22Y02E60/50
Inventor 邢伟袁勋王小宁刘勇吴明铂
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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