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Pd/C catalyst and preparation method thereof

A technology of catalyst and reducing agent, which is applied in the field of Pd/C catalyst and its preparation, can solve the problems of serious influence on electrochemical catalysis, unfavorable mass production of Pd catalyst, reduction of catalytic activity and catalytic selectivity of catalyst, and achieve high catalytic activity As well as anti-attenuation performance, excellent electrocatalytic activity, and the effect of realizing mass production

Inactive Publication Date: 2019-04-16
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The addition of these surfactants and polymers does reduce the excessive particle size and agglomeration of Pd nanoparticles to a certain extent, but because these additives are easily adsorbed on the surface of Pd nanoparticles and difficult to remove, the catalytic activity of the catalyst and The catalytic selectivity is significantly reduced, and the conductivity of the catalyst is also reduced, which has a great impact on electrochemical catalysis.
Although it is possible to reduce the influence of additives on the Pd catalyst through post-treatment, the process is cumbersome, consumes energy and time, and wastes resources, which is not conducive to the mass production of Pd catalysts.

Method used

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  • Pd/C catalyst and preparation method thereof
  • Pd/C catalyst and preparation method thereof
  • Pd/C catalyst and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment example 1

[0032] 1. Weigh 0.1185mmol PdCl 2 In the flask, add HCl to make 0.1M H 2 PdCl 4 solution, then add 5ml of water, after stirring evenly, add 400ul ammonia water, stir magnetically until the solution becomes colorless and transparent; the molar volume concentration of Pd in ​​the solution is 1.8×10 -2 mol / L, the molar ratio of Pd to ammonia water is 1:22;

[0033] 2. Add 30ml of ultrapure water to the flask, then add 1.5ml of 1M NaOH solution, and stir magnetically for 20min;

[0034] 3. Add 37.5 mg of carbon black powder to the flask, ultrasonicate at 100W for 30 minutes, then transfer the flask to an oil bath, and stir magnetically for 2 hours under an Ar gas atmosphere;

[0035] 4. Then, under the condition of magnetic stirring, add 1ml formaldehyde solution into the flask, and stir for 10min; the molar ratio of Pd to formaldehyde is 1:115.5;

[0036] 5. Heat the above mixture to 60°C at a heating rate of 2°C / min, and react at this temperature for 2 hours;

[0037] 6. Su...

Embodiment example 2

[0039] 1. Weigh 0.1185mmol Na 2 PdCl 4 In the flask, add ultrapure water to make 0.1M Na 2 PdCl 4 solution, then add 5ml of water, after stirring evenly, add 400ul ammonia water, and magnetically stir until the solution becomes colorless and transparent; the molar volume concentration of Pd in ​​the solution is 1.8×10 -2 mol / L, the molar ratio of Pd to ammonia water is 1:22;

[0040] 2. Add 30ml of ultrapure water to the flask, then add 1.5ml of 1M NaOH solution, and stir magnetically for 20min;

[0041] 3. Add 37.5 mg of carbon black powder to the flask, ultrasonicate at 100W for 30 minutes, then transfer the flask to an oil bath, and stir magnetically for 2 hours under an Ar gas atmosphere;

[0042] 4. Then, under the condition of magnetic stirring, add 1ml formaldehyde solution into the flask, and stir for 10min; the molar ratio of Pd to formaldehyde is 1:115.5;

[0043] 5. Heat the above mixture to 60°C at a heating rate of 2°C / min, and react at this temperature for 2...

Embodiment example 3

[0046] 1. Weigh 0.1185mmol K 2 PdCl 4 In the flask, add ultrapure water to make 0.1M K 2 PdCl 4 solution, then add 5ml of water, after stirring evenly, add 400ul ammonia water, and magnetically stir until the solution becomes colorless and transparent; the molar volume concentration of Pd in ​​the solution is 1.8×10 -2 mol / L, the molar ratio of Pd to ammonia water is 1:22;

[0047] 2. Add 30ml of ultrapure water to the flask, then add 1.5ml of 1M NaOH solution, and stir magnetically for 20min;

[0048] 3. Add 37.5 mg of carbon black powder to the flask, ultrasonicate at 100W for 30 minutes, then transfer the flask to an oil bath, and stir magnetically for 2 hours under an Ar gas atmosphere;

[0049] 4. Then, under the condition of magnetic stirring, add 1ml formaldehyde solution into the flask, and stir for 10min; the molar ratio of Pd to formaldehyde is 1:115.5;

[0050] 5. Heat the above mixture to 60°C at a heating rate of 2°C / min, and react at this temperature for 2 h...

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Abstract

The invention discloses a Pd / C catalyst and a preparation method thereof, the Pd / C catalyst takes carbon black as a carrier, and Pd metal nanoparticles are uniformly dispersed on the carbon black; themass percent of the Pd metal nanoparticles in the catalyst is 1%-70%, and the particle diameter is 2 nm to 8 nm. According to the Pd / C catalyst and the preparation method thereof, a liquid phase reduction method is used, ammonium hydroxide and NaOH are added to a Pd saline solution with certain concentration, a Pd complex ion solution is prepared, excessive reducing agent is added then, and the Pd complex ions are reduced on the dispersed carbon black carrier at certain reaction temperature. The Pd / C catalyst prepared with the method has excellent electrocatalytic activity in an oxygen-saturated 0.1 mol / L of HClO4 solution. The difficulties that the particle diameter of the Pd nanoparticles is large, clustering is difficult and the Pd / C catalyst is difficult to prepare in batches are solved.

Description

technical field [0001] The invention relates to the fields of electrochemical technology and fuel cell catalysts, in particular to a Pd / C catalyst with uniform particle size, good dispersion and large-scale preparation and a preparation method thereof. Background technique [0002] In recent years, with the development of science and technology, catalysts with various properties and functions have been continuously manufactured, among which Pd-based catalysts are the most dazzling ones. Pd nanoparticles are used as catalysts in many organic chemical reactions, such as Suzuki, Heck and Stillecoupling. In addition, due to the urgent demand for green and environmentally friendly energy, the application of Pd nanocatalysts in new energy has attracted more and more attention. Among them, the application of Pd in ​​direct formic acid fuel cell is a best example. Formic acid has the characteristics of non-toxic, non-flammable, high open circuit voltage, and low permeability of Na...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J35/00B01J37/16H01M4/92
CPCH01M4/926B01J23/44B01J37/16B01J35/399B01J35/393B01J35/33Y02E60/50
Inventor 章俊良罗柳轩吴爱明蔡熙阳朱凤鹃
Owner SHANGHAI JIAO TONG UNIV
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