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Preparation method of nano palladium oxide hollow spheres

A technology of palladium oxide and hollow spheres, which is applied in the field of preparation of palladium oxide hollow spheres, can solve problems such as difficult removal by chemical methods, and achieve the effects of good sedimentation stability, increased surface area, and improved catalytic performance

Inactive Publication Date: 2014-09-24
NANJING JIANTE ENVIRONMENTAL PROTECTION TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Another method is to use palladium chloric acid as the palladium source, and PVP as a stabilizer to prepare nano-scale palladium oxide under microwave irradiation. The palladium oxide prepared by this method is easy to combine with PVP in the reaction solution, and due to the chemical properties of PVP Stable, it is difficult to remove it by chemical methods, so it is generally separated repeatedly by high-speed centrifugation, which limits its wide application to a certain extent

Method used

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  • Preparation method of nano palladium oxide hollow spheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Iron particles with a diameter of about 150 nm were obtained by reducing ferrous sulfate with sodium borohydride in water. 10 g of the prepared iron nanoparticles were added to 400 mL of palladium nitrate aqueous solution with a concentration of 0.2 mol / L and a temperature of 40° C., and mechanically stirred for 10 minutes. Prepare 400mL of palladium nitrate and glycine mixed aqueous solution, wherein the concentration of palladium nitrate is 0.3mol / L, the molar ratio of glycine to palladium nitrate is 1:1, and a certain amount of sodium hydroxide aqueous solution is added to adjust the pH value of the mixed solution to 9. Add the iron particles that have been surface-activated by palladium salt into the mixed aqueous solution of palladium nitrate, glycine and sodium hydroxide, heat the mixed solution to 95°C and keep it warm for 1 hour. 300 mL of hydrogen peroxide with a concentration of 50% was added dropwise to prepare spherical palladium oxide / iron core particles ha...

Embodiment 2

[0034] Iron particles with a diameter of about 20 nm were obtained by reducing ferrous sulfate with sodium borohydride in water. 10 g of the prepared iron nanoparticles were added to 400 mL of palladium nitrate aqueous solution with a concentration of 0.2 mol / L and a temperature of 40° C., and mechanically stirred for 10 minutes. Prepare 400mL of palladium nitrate and glycine mixed aqueous solution, wherein the concentration of palladium nitrate is 0.3mol / L, the molar ratio of glycine to palladium nitrate is 1:1, and a certain amount of sodium hydroxide aqueous solution is added to adjust the pH value of the mixed solution to 9. Add the iron particles that have been surface-activated by palladium salt into the mixed aqueous solution of palladium nitrate, glycine and sodium hydroxide, heat the mixed solution to 85°C for 1 hour, and at the same time add the mixed solution to the mixed solution at a rate of 4mL / min under mechanical stirring. 300 mL of hydrogen peroxide with a con...

Embodiment 3

[0036] Iron particles with a diameter of about 50 nm were obtained by reducing ferrous sulfate with sodium borohydride in water. 10 g of the prepared iron nanoparticles were added to 400 mL of palladium nitrate aqueous solution with a concentration of 0.2 mol / L and a temperature of 40° C., and mechanically stirred for 10 minutes. Prepare 400mL of palladium nitrate and glycine mixed aqueous solution, wherein the concentration of palladium nitrate is 0.3mol / L, the molar ratio of glycine to palladium nitrate is 1:1, and a certain amount of sodium hydroxide aqueous solution is added to adjust the pH value of the mixed solution to 9. Add the iron particles treated with palladium salt surface activation to the mixed aqueous solution of palladium nitrate, glycine and sodium hydroxide, heat the mixed solution to 90°C for 1 hour, and at the same time add the mixed solution to the mixed solution at a rate of 4mL / min under mechanical stirring. 300 mL of hydrogen peroxide with a concentra...

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Abstract

The invention provides a preparation method of nano palladium oxide hollow spheres. The preparation method comprises the following steps: preparing a palladium nitrate-glycine mixed aqueous solution; adding a certain amount of a sodium hydroxide aqueous solution into the palladium nitrate-glycine mixed aqueous solution so as to adjust the pH value of the mixed solution to be alkaline; adding iron particles subjected to palladium chloride surface activation treatment into the mixed aqueous solution of palladium nitrate, glycine and sodium hydroxide; heating the mixed aqueous solution to 85-95 DEG C, and carrying out heat preservation on the mixed aqueous solution; dropwise adding a certain amount of an oxidant solution into the mixed aqueous solution at a certain speed under the condition of mechanical stirring so as to prepare spherical particles with an iron core-palladium oxide shell structure; and after the spherical particles with the iron core-palladium oxide shell structure are taken out and cleaned, adding the spherical particles into an acid solution so as to remove iron cores by dissolving, and carrying out mechanical stirring to obtain the nano palladium oxide hollow spheres. According to the preparation method provided by the invention, through preparing the nano palladium oxide hollow spheres, the surface area of palladium oxide is increased, and then the distribution rate and service efficiency of palladium are improved, thus the purpose of fully using and improving the catalytic activity of palladium oxides is achieved.

Description

technical field [0001] The invention belongs to the field of nanomaterial preparation, in particular to a preparation method of palladium oxide hollow spheres. Background technique [0002] The way to generate catalytic palladium oxide particles in traditional three-way catalysts for automobiles is to add a certain amount of palladium salt to the slurry prepared by mixing catalyst coating powder and weak acid aqueous solution and coat it on the surface of the catalyst carrier. The catalyst-coated carrier is heated to above 500°C for sintering. During the sintering process, the palladium salt in the slurry is oxidized and transformed into palladium oxide particles attached to the surface of the catalyst carrier and having a catalytic effect. This palladium oxide particle is formed under the high temperature in the sintering process, and the diameter of the palladium oxide particle in the catalyst support coating prepared by this method is relatively large, about hundreds of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G55/00B01J23/44B01J35/08
Inventor 姚小刚刘颖温术来
Owner NANJING JIANTE ENVIRONMENTAL PROTECTION TECH