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Ultrasonic radiation preparation method for chrysanthemum-like nano-palladium aggregate material

A technology of ultrasonic radiation and nano-palladium, which is applied in the field of ultrasonic radiation preparation of chrysanthemum-shaped nano-palladium aggregate materials, can solve the problems of cumbersome product purification process, environmental pollution of additives, unfavorable large-scale production, etc., and achieve easy control of reaction rate and production The effect of short cycle and low cost

Inactive Publication Date: 2013-01-16
ANHUI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, on the one hand, this synthesis method needs to use organic phases such as o-dichlorobenzene as solvents, which is highly toxic, and at the same time introduces many chemical reagents such as dihydric alcohol reducing agents, oleylamine and other dispersion stabilizers, and the product purification process is cumbersome. The consumption of additives may also cause certain environmental pollution problems. On the other hand, reflux equipment is required, and the reaction temperature is high, which is not conducive to large-scale industrial production.

Method used

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  • Ultrasonic radiation preparation method for chrysanthemum-like nano-palladium aggregate material
  • Ultrasonic radiation preparation method for chrysanthemum-like nano-palladium aggregate material

Examples

Experimental program
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Effect test

Embodiment 1

[0025] 1. Add 50mL of water and 10mL of ethanol to the reactor to obtain a water-ethanol mixed solvent system;

[0026] 2. Put 2.8×10 -5 mol of PdCl 2 , 8.4×10 -6 mol of PVP and 1.96×10 -5 mol of SDS was added to the water-ethanol mixed solvent system, the temperature was controlled at 40-45°C, and N 2 Protection, N 2 The flow rate was 50mL / min, the ultrasonic instrument was turned on, the ultrasonic output power was controlled at 400W, the ultrasonic reaction was 60min, and the ultrasonic was stopped to obtain a black suspension.

[0027] 3. The black precipitate obtained in the reaction solution was separated by centrifugation, washed with ethanol and acetone by centrifugation, and vacuum-dried at 40° C. for 16 hours to obtain a chrysanthemum-shaped nano-palladium aggregate material.

[0028] The microscopic morphology of the chrysanthemum-shaped nano-palladium aggregate material prepared in this example is shown in the attached figure 1 As shown, the aggregates look l...

Embodiment 2

[0030] 1. Add 40mL of water and 8mL of ethanol to the reactor to obtain a water-ethanol mixed solvent system;

[0031] 2. Set 2.24×10 -5 mol of PdCl 2 , 6.72×10 -6 mol of PVP and 1.57×10 -5 mol of SDS was added to the water-ethanol mixed solvent system, the temperature was controlled at 43±2°C, and N 2 Protection, N 2 The flow rate was 80mL / min, the ultrasonic instrument was turned on, the ultrasonic output power was controlled at 200W, the ultrasonic reaction was performed for 90min, and the ultrasonic was stopped to obtain a black suspension.

[0032] 3. The black precipitate obtained in the reaction solution was separated by centrifugation, washed with ethanol and acetone, and vacuum-dried at 40° C. for 12 hours to obtain a chrysanthemum-shaped palladium nano-aggregate material with an average aggregate size of about 60 nm.

Embodiment 3

[0034] 1. Add 60mL of water and 12mL of ethanol to the reactor to obtain a water-ethanol mixed solvent system;

[0035] 2. Set 3.36×10 -5 mol of PdCl 2 , 1.01×10 -5 mol of PVP and 2.35×10 -5 mol of SDS was added to the water-ethanol mixed solvent system, the temperature was controlled at 43±2°C, and N 2 Protection, N 2 The flow rate was 40mL / min, the ultrasonic instrument was turned on, the ultrasonic output power was controlled at 600W, the ultrasonic reaction was performed for 45min, and the ultrasonic was stopped to obtain a black suspension.

[0036] 3. The black precipitate obtained in the reaction solution was separated by centrifugation, washed with ethanol and acetone, and vacuum-dried at 40° C. for 24 hours to obtain a chrysanthemum-shaped palladium nano-aggregate material with an average size of about 100 nm.

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Abstract

The invention discloses an ultrasonic radiation preparation method for a chrysanthemum-like nano-palladium aggregate material. The method comprises the following steps of: adding water and ethanol into a reactor; then adding PdCl2 powder and a surfactant-macromolecule combined system soft template; under protection of nitrogen, performing ultrasonic reaction; after the reaction is finished, performing centrifugal separation to collect sediments; and washing by using ethanol and acetone, and drying in vacuum to obtain the nano-palladium aggregate material. Under the reduction action of the ethanol and the action of a cosolvent, and under the condition that a chemical reducing agent such as sodium borohydride and ascorbic acid is not added, the chrysanthemum-like nano-palladium aggregate material is synthesized; the reaction rate is easy to control; the cost is low; and the operation process is simple and feasible. The size of the prepared chrysanthemum-like nano-palladium aggregate material is 60 to 100 nm.

Description

1. Technical field [0001] The invention relates to a method for preparing nanometer materials, in particular to a method for preparing a chrysanthemum-shaped nano-palladium aggregate material by ultrasonic radiation. 2. Background technology [0002] In the upsurge of research on nanomaterials, the unique optical, electrical, and catalytic properties of metal nanomaterials and their applications in new energy research, photoelectric information storage, and biomedicine have attracted extensive attention in related research fields. The properties of nanoparticles largely depend on their shape and size. Great progress has been made in the controllable synthesis of one-dimensional (1D) and two-dimensional (2D) noble metal nanoparticles. Many research groups have synthesized Nanostructures such as noble metal nanorods, nanosheets, and nanowires were studied, and the correlation between their tunable light absorption properties, catalytic activity, and local field enhancement eff...

Claims

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Application Information

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IPC IPC(8): B22F9/20
Inventor 王艳丽谭德新张明旭闵凡飞徐初阳王晓宇方熙
Owner ANHUI UNIV OF SCI & TECH
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