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A kind of preparation method of nano palladium oxide

A palladium oxide and nanotechnology, which is applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve the problems of easy introduction of impurity ions, failure to reach the nanometer level, coarse particle size of palladium oxide, etc.

Active Publication Date: 2017-10-27
上海三爱思试剂有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] According to domestic and foreign literature reports over the years, in the traditional process, the preparation of palladium oxide is to dissolve palladium in aqua regia, prepare dichlorodiammine palladium precipitation, and then burn at high temperature to obtain the finished product. This method is not easy to introduce impurity ions , and the particle size of the obtained palladium oxide is too thick to reach the nanoscale

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  • A kind of preparation method of nano palladium oxide

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Effect test

Embodiment 1

[0022] Take 10g of palladium powder in a 500ml round-bottomed three-neck flask, add 150ml, 55wt% nitric acid solution, heat to 75 degrees in a water bath, and react for 5 hours. The solution was reddish brown, and a small amount of undissolved palladium powder was filtered out. The filtrate was collected in a small rotary evaporating flask, concentrated under reduced pressure until the content of free nitric acid was less than 10 wt%, cooled to 25°C, and added 0.5 g of octylphenol polyoxyethylene ether. Stir evenly and place for 2 hours, dry, and burn at 600-700°C for at least 3 hours to obtain palladium oxide with a yield of 98.2%, a particle size of 20nm, a palladium content of 86±0.5%, a water content of ≤1.0%, and a specific surface area ≥500cm 2 / g, impurity standard: Pt≤0.0010%, Au≤0.0003%, Pb≤0.0010%, Si≤0.0030%, Fe≤0.0010%, Ni≤0.0010%, Al≤0.0010%, Ir≤0.0010%, Cu≤0.0003% , Rh ≤ 0.0010%, Ag ≤ 0.0003%, Sn ≤ 0.0003%, and the hydrogen absorption catalytic effect under the...

Embodiment 2

[0024] Take 10g of palladium powder in a 500ml round-bottomed three-neck flask, add 200ml of nitric acid solution with a concentration of 55wt%, heat it in a water bath to 85 degrees, and react for 5 hours. The solution was reddish brown, and a small amount of undissolved palladium powder was filtered out. The filtrate was collected in a small rotary evaporating flask, concentrated under reduced pressure until the content of free nitric acid was less than 10 wt%, cooled to 25°C, and added 0.5 g nonylphenol polyoxyethylene ether. Stir evenly and place for 2 hours, dry, and burn at 600-700°C for at least 3.5 hours to obtain palladium oxide with a yield of 99%, a particle size of 22nm, a palladium content of 86±0.5%, a water content of ≤1.0%, and a specific surface area of ​​≥ 500cm 2 / g, impurity standard: Pt≤0.0010%, Au≤0.0003%, Pb≤0.0010%, Si≤0.0030%, Fe≤0.0010%, Ni≤0.0010%, Al≤0.0010%, Ir≤0.0010%, Cu≤0.0003% , Rh ≤ 0.0010%, Ag ≤ 0.0003%, Sn ≤ 0.0003%, and the hydrogen absor...

Embodiment 3

[0026] Take 10g of palladium powder in a 500ml round-bottomed three-neck flask, add 200ml of nitric acid solution with a concentration of 55wt%, heat it in a water bath to 85 degrees, and react for 5 hours. The solution was reddish brown, and a small amount of undissolved palladium powder was filtered out. The filtrate was collected in a small rotary evaporating flask, concentrated under reduced pressure until the free nitric acid content was less than 10 wt%, cooled to 25°C, and 1g of octylphenol polyoxyethylene ether was added. Stir evenly and stand for 2 hours, dry, and burn at 600-700°C for at least 4 hours to obtain palladium oxide with a yield of 99.2%, a particle size of 11nm, and a hydrogen absorption catalytic effect of 0.20ml / g under standard conditions.

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Abstract

The invention discloses a method for preparing nano-palladium oxide with high specific surface area, which comprises the following steps: adding palladium powder into a nitric acid solution with a mass fraction of 50-60% while stirring, controlling the temperature at 70-100°C, and the reaction time is 3 After ~6 hours, the reaction solution was cooled, filtered, then added with a self-made surfactant, concentrated, and burned to obtain the target object, nano-palladium oxide with a high specific surface area. The process of the invention has the characteristics of safety, environmental protection, fast reaction speed, high product yield (>98.0%), etc., and the prepared palladium oxide product has high purity, which is convenient for expanding production.

Description

technical field [0001] The present invention relates to the synthesis of palladium oxide, more precisely a method for preparing nano-palladium oxide with high specific surface area, which belongs to the technical field of catalysts. Background technique [0002] Palladium oxide, English name: Palladium oxide, molecular formula: PdO. Black or dark green powder, stable in air. Insoluble in water, dilute hydrochloric acid, dilute nitric acid, slightly soluble in aqua regia. [0003] Nanoparticles belong to the mesoscopic phase, because they have different energy states and properties from macroscopic substances, so they have attracted widespread attention in the academic circles. Palladium oxide is the raw material for the synthesis of palladium compounds, one of the important palladium group metal oxides, the main solid catalyst, and additives for the preparation of hydrogen-absorbing materials. Nano-palladium oxide has high catalytic activity for natural gas combustion and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G55/00B82Y30/00
Inventor 黄胜杨翠
Owner 上海三爱思试剂有限公司