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A kind of preparation method of palladium base catalyst

A catalyst and palladium-based technology are applied in the field of preparation of palladium-based catalysts and can solve problems such as reducing catalyst utilization rate and the like

Active Publication Date: 2015-10-07
SHANDONG SAIKESAISI HYDROGEN ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the disadvantage of using citric acid as a stabilizer is that after the synthesis process of the nanocatalyst is finished, means such as high-temperature burning must be used to remove the stabilizer adsorbed on the surface of the nanocatalyst, so as to prevent the adsorption of the stabilizer from covering the active surface area of ​​the catalyst. The high temperature burning process will inevitably lead to the aggregation of nano-catalysts, which reduces the utilization rate of catalysts.

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  • A kind of preparation method of palladium base catalyst
  • A kind of preparation method of palladium base catalyst
  • A kind of preparation method of palladium base catalyst

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[0038] The invention provides a preparation method of a palladium-based catalyst, comprising the following steps: A) mixing a carrier, a palladium source and a Keggin-type heteropolyacid in a solution to obtain a suspension; B) adjusting the suspension with an alkaline solution pH value, and then add a reducing agent to react to obtain a catalyst; C) calcining the catalyst in an oxygen atmosphere to obtain a palladium-based catalyst.

[0039] All raw materials in the present invention have no special limitation on their sources, and they can be commercially available.

[0040]Carrier, palladium source and Keggin type heteropolyacid are mixed in solution, and wherein, described carrier is the carrier well-known to those skilled in the art and gets final product, does not have special limitation, is preferably activated carbon, carbon nanotube, graphite in the present invention ene or titanium dioxide; the palladium source can be a palladium source well-known to those skilled in...

Embodiment 1

[0051] 1.1 Add 18g Vulcan XC-72 carbon powder into 100ml deionized water and ultrasonically stir to disperse, then add 1.77g (0.01mol) PdCl 2 (dissolved in 1mol / L hydrochloric acid) and 0.1mol Keggin type phosphomolybdic acid H 3 Mo 12 o 40 (PMo 12 ), to obtain a suspension, ultrasonically disperse and stir for 12 hours to ensure that Keggin-type phosphomolybdic acid is adsorbed by Vulcan XC-72 carbon powder; then use 50% (V / V) ammonia solution to adjust the pH value of the suspension to 4.0, then add dropwise freshly prepared NaBH containing 0.015mol 4 The aqueous solution was subjected to a reduction reaction for 2 hours, filtered, washed with mild deionized water, and dried overnight at 60°C in a vacuum oven to obtain a catalyst.

[0052] 1.2 Place the catalyst obtained in 1.1 in a tube furnace and calcinate at 100°C for 24 hours in an oxygen atmosphere, wherein the flow rate of oxygen is 80cc / min, and the tube furnace is heated from room temperature to 100°C at a rate ...

Embodiment 2

[0066] 2.1 Add 18g Vulcan XC-72 carbon powder into 100ml deionized water and ultrasonically stir to disperse, then add 1.77g (0.01mol) PdCl 2 (dissolved in 1mol / L hydrochloric acid) and 0.1mol Keggin type phosphomolybdic acid H 3 Mo 12 o 40 (PMo 12 ), to obtain a suspension, ultrasonically disperse and stir for 12 hours to ensure that Keggin-type phosphomolybdic acid is adsorbed by Vulcan XC-72 carbon powder; then use 50% (V / V) ammonia solution to adjust the pH value of the suspension to 4.0, then add dropwise freshly prepared NaBH containing 0.015mol 4 The aqueous solution was subjected to a reduction reaction for 2 hours, filtered, washed with mild deionized water, and dried overnight at 60°C in a vacuum oven to obtain a catalyst.

[0067] 2.2 Place the catalyst obtained in 2.1 in a tube furnace and calcinate at 80°C for 24 hours in an oxygen atmosphere, wherein the flow rate of oxygen is 80cc / min, and the tube furnace is heated from room temperature to 80°C at a rate of...

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Abstract

The invention provides a preparation method of a palladium based catalyst. The preparation method comprises the following steps: mixing a carrier and a palladium source with a Keggin type heteropolyacid in a solution, regulating the pH of the suspension in an alkaline solution, adding a reducing agent to react to obtain a catalyst, calcining the catalyst in an oxygen atmosphere to obtain the palladium based catalyst. Compared with the existing method, the preparation method has the advantages that the Keggin type heteropolyacid is used as a stabilizer in the preparation method to be attached to the surfaces of carbon and metal in the form of an irreversible monomolecular layer so as to functionalize the surfaces, and the oxidation reduction properties of the Keggin type heteropolyacid can promote the oxidation removal of CO toxic intermediate, and meanwhile, the Keggin type heteropolyacid has a hydrogen spillover effect and can improve the proton conduction rate of the palladium based catalyst; secondly, the catalyst is calcined in the oxygen atmosphere to improve the content of oxide in the palladium based catalyst so as to improve the electrochemical activity of the catalyst; and thirdly, the palladium based catalyst can be obtained by reduction reaction and calcination, so that the preparation method is simple.

Description

technical field [0001] The invention belongs to the technical field of fuel cells, and in particular relates to a preparation method of a palladium-based catalyst. Background technique [0002] As an alternative fuel to methanol, direct formic acid fuel cells (DFAFCs) have received a lot of attention in recent years. Like methanol, formic acid only contains one carbon atom and does not contain C-C bonds. It has the advantages of easy oxidation, cheap price, and abundant sources. Not only that, formic acid also has many advantages that methanol cannot match: non-toxic, and is used by the US Food and Drug Administration. It is approved as a food additive by the Supervision Bureau; it is non-flammable, safe and convenient for storage and transportation; it has a high theoretical open circuit voltage, and the theoretical electromotive force of DFAFC is 1.48V at 25°C; as a fuel, the concentration can be very high, even if the concentration is as high as 20mol / L. It has good perf...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44H01M4/92
CPCY02E60/50
Inventor 邢巍严亮刘长鹏姚世魁常进法李晨阳
Owner SHANDONG SAIKESAISI HYDROGEN ENERGY