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Titanium dioxide nanotube carried palladium nano catalyst and preparation method of same

A titanium dioxide and palladium nanotechnology, which is applied in the field of titanium dioxide nanotube-supported palladium nanocatalyst and its preparation, can solve the problems of difficult application of catalytic system and industrialization process, small number of particles, etc. efficiency, increasing the output power

Active Publication Date: 2012-10-03
XIAMEN UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

[0004] However, it should be pointed out that the above metal nanocatalysts with open surface structures are all grown on the surface of smooth glassy carbon electrodes, and most of them only form a single layer of metal nanocrystals with a small number of particles, making it difficult to apply to practical catalytic systems and industrial processes.

Method used

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  • Titanium dioxide nanotube carried palladium nano catalyst and preparation method of same
  • Titanium dioxide nanotube carried palladium nano catalyst and preparation method of same
  • Titanium dioxide nanotube carried palladium nano catalyst and preparation method of same

Examples

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Embodiment 1

[0032] Preparation of titania nanotube array electrodes:

[0033] 1. A two-electrode electrochemical cell system is adopted, with a titanium sheet (diameter 1.1 cm, purity 99.9%) as the working electrode and auxiliary electrode, and the distance between the two electrodes is controlled to be 2 cm. In the alcohol electrolyte, the anodic oxidation potential is controlled at 60V, and the treatment time is 1h. Take it out and rinse it to dry naturally;

[0034] 2. Transfer the anodized sample to a muffle furnace for annealing, control the heating rate to 2.5°C / min, and when the temperature rises to 400°C, turn to a constant temperature and stay for 30 minutes. TiO2 nanotube arrays can be obtained;

[0035] 3. Polish the titanium dioxide nanotube array with metallographic sandpaper (2500 mesh), after ultrasonic cleaning, transfer it to an electrolytic cell containing 5% perchloric acid + 95% acetic acid solution, control the anodic oxidation potential to 50V, and process time for ...

Embodiment 2

[0037] Electroless deposition of metallic palladium nanoparticles on titania nanotube array electrodes:

[0038] 1. Preparation of palladium nanoparticle chemical deposition solution: Weigh an appropriate amount of PdCL 2 , HCL and ethylene glycol, dissolved in deionized water and passed through sulfuric acid solution to prepare 6.0g / L PdCl 2 The aqueous solution of +14.0ml / L HCl+20.0mL / L ethylene glycol is designated as solution A;

[0039] 2. Weigh an appropriate amount of NaBH 4 , dissolved in deionized water to prepare 20.0g / L NaBH 4 Solution, denoted as solution B;

[0040] 3. First, take 4 beakers and discharge them in turn, and add appropriate amount of solution A, deionized water, solution B and deionized water to them respectively; secondly, put the titanium dioxide nanotube array electrode according to solution A; deionized water; solution B and The deionized water was sequentially soaked for 10 s, and the treatment was repeated 10 times to prepare metal palladiu...

Embodiment 3

[0042] "Electrochemical post-treatment" process of palladium catalyst nanoparticles:

[0043] 1. Preparation of the "electrochemical post-treatment" solution: Weigh potassium hydroxide, dissolve it in deionized water, and prepare a 2.0M KOH solution, which is recorded as the "electrochemical post-treatment" solution.

[0044] 2. Adopt a three-electrode electrochemical electrolytic cell system, add an appropriate amount of "electrochemical post-treatment" solution to the electrolytic cell, use a titanium dioxide nanotube array-loaded palladium electrode as the working electrode, and a Pd sheet and a saturated calomel electrode (SCE) as the working electrode, respectively. Auxiliary and reference electrodes. Electrochemical program potential step technology is used for processing, the upper limit potential (Eu) is 4.55V, the upper limit time (tu) is 180s; the lower limit potential (Ed) is -1.95V, the lower limit time (td) is 180s; the processing time is 0.3h. Take it out, wash ...

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Abstract

The invention relates to a nano catalyst and a preparation method thereof, in particular to a titanium dioxide nanotube carried palladium nano catalyst and a preparation method. The method comprises the steps as follows: preparing a titanium dioxide nanotube array electrode first, depositing palladium nanoparticle on the titanium dioxide nanotube electrode through chemical deposition, and preparing an electrochemical post-processing solution; adopting a three-electrode electrochemical electrolytic cell system, and adding the electrochemical post-processing solution in an electrolytic cell, wherein the three electrodes include a working electrode, an auxiliary electrode and a reference electrode, the working electrode is a titanium dioxide nanotube array carried palladium electrode, and the auxiliary electrode is a palladium sheet; adopting an electrochemical program potential step processing method, wherein the upper limit of potential is 0.5-5.5 volt, the upper limit of time is 10-300 seconds, the lower limit of potential is (-4.5)-(-0.5) volt, the lower limit of time is 10-300 seconds, and the processing time is 0.1-6 hours; and taking out the working electrode, flushing and then obtaining the product. The titanium dioxide nanotube carried palladium nano catalyst can be used for preparation of fuel cells and electric organic synthesis as an electro-catalyst.

Description

technical field [0001] The invention relates to a nanocatalyst and its preparation method, in particular to a nanotube of titanium dioxide as a carrier, carrying metal palladium on its surface and controlling the generation of Titanium dioxide nanotube-supported metal palladium nanocatalyst with high-density open surface structure and its preparation method, and its application in important fields such as fuel cell and organic electrosynthesis. Background technique [0002] Palladium (Pd) is a catalytic material widely used in important fields such as fuel cells, electrochemical catalysis, and organic electrosynthesis. In alkaline media, Pd nanomaterials have higher electro-oxidation of ethanol than platinum (Pt). Catalytic activity, indicating that Pd catalyst has a good application prospect in direct ethanol fuel cells. The development of Pd catalysts can not only get rid of the dependence on Pt, but also greatly reduce the cost. In-depth exploration to improve the activ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J37/34H01M4/92C25B11/08
CPCY02E60/50
Inventor 陈声培陈燕鑫孙世刚黄蕊
Owner XIAMEN UNIV
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