CN101880038A - Preparation method of carbon nano-tube supported palladium nano-composite material - Google Patents
Preparation method of carbon nano-tube supported palladium nano-composite material Download PDFInfo
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- CN101880038A CN101880038A CN2009101382587A CN200910138258A CN101880038A CN 101880038 A CN101880038 A CN 101880038A CN 2009101382587 A CN2009101382587 A CN 2009101382587A CN 200910138258 A CN200910138258 A CN 200910138258A CN 101880038 A CN101880038 A CN 101880038A
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Abstract
The invention discloses a method for preparing a carbon nano-tube supported palladium nano-composite material by utilizing phase transfer and self-assembly technology. The method of the invention comprises the following steps: dissolving dodecyl sulfide and palladium acetate in absolute ethyl alcohol, and heating and stirring to obtain a Pd nano-particle ethanol solution; adding the prepared Pd nano-particle ethanol solution into an organic solvent containing benzyl mercaptan, extracting the ethanol through distilled water, and transferring Pd nano-particles into the organic solvent through phase transfer; and adding the organic solvent containing the Pd nano-particles into CNTs in the corresponding suspension of the organic solvent, and carrying out conventional treatment to obtain a Pd/CNTs nano-composite material. The analysis result shows that the Pd nano-particles of the material synthesized by the method are uniformly distributed on the surfaces of the CNTs.
Description
Technical field
The present invention relates to a kind of method of utilizing phase transition and self-assembling technique to prepare carbon nano-tube supported palladium nano-composite material.
Background technology
As a class brand-new material, carbon nanotube-based (CNTs) matrix material causes that with its unique physics and chemical property people study interest greatly.Decoration has the CNTs matrix material (being abbreviated as Pd/CNTs) of Pd nanoparticle to estimate at nano electron device, gas sensing, and fuel cell and heterogeneous catalysis field have the potential using value.At present, the preparation method of Pd/CNTs nano composite material comprises: supercritical CO
2Fluid technique, microemulsion, electrochemical deposition and tensio-active agent autoreduction etc.Though these methods successfully support the CNTs surface with the Pd nanoparticle, they otherwise be subjected to the harsh reaction conditions or the restriction of equipment, or be subjected to loaded down with trivial details tediously long experimentation puzzlement (J.Phys.Chem.C, 2008,112:8172-8176).Therefore, invent a kind of simple, gentleness, effective means prepares the Pd/CNTs nano composite material and remains the target that many investigators pursue.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing carbon nano-tube supported palladium nano-composite material.
The objective of the invention is to be achieved through the following technical solutions:
Based on the former study basis, we utilize phase transition and self-assembling technique, successfully with pre-synthetic particle diameter and distribute the Pd nanoparticle controlled and support the CNTs surface.
The present invention is dissolved in dodecyl thioether and palladium in the dehydrated alcohol, and heated and stirred obtains the Pd nano-particle ethanol solution.The Pd nano-particle ethanol solution of preparation is joined in the organic solvent that contains benzyl mercaptan, extract ethanol, make the phase transition of Pd nanoparticle to organic solvent by distilled water.The organic solvent that will contain the Pd nanoparticle joins CNTs in the suspension of corresponding organic solvent, obtains the Pd/CNTs nano composite material through conventional processing.
A kind of preparation method of carbon nano-tube supported palladium nano-composite material is characterized in that this method may further comprise the steps:
A. palladium and dodecyl thioether are dissolved in the dehydrated alcohol, under 40-100 ℃ of heated and stirred, obtain black Pd nano-particle ethanol solution;
B. the Pd nano-particle ethanol solution with preparation joins in the organic solvent of the benzene,toluene,xylene, hexanaphthene or the octane that contain benzyl mercaptan, stir, extract ethanol by distilled water, the Pd nanoparticle is transferred in the organic solvent of benzene,toluene,xylene, hexanaphthene or octane;
The organic solvent that C. will contain benzene,toluene,xylene, hexanaphthene or the octane of Pd nanoparticle joins CNTs at benzene, toluene, dimethylbenzene, in the suspension of hexanaphthene or octane, supersound process, filter, wash respectively with dehydrated alcohol and distilled water, drying obtains the Pd/CNTs nano composite material.
In preparation process of the present invention, the mol ratio of palladium and dodecyl thioether is 1: 2-1: 20.
In preparation process of the present invention, the mol ratio of palladium and benzyl mercaptan is 1: 5-1: 100.
In preparation process of the present invention, Pd and CNTs mass ratio are 0.01-1.
The Pd/CNTs nano composite material of the present invention's preparation shows that by the transmission electron microscope photo Pd nanoparticle is evenly distributed on the CNTs surface.
Advantage of the present invention is: (1) is by the particle diameter of control Pd nanoparticle and the relative content of Pd nanoparticle and CNTs, size and the density that can regulate CNTs surface Pd nanoparticle easily; (2) reaction process is simple to operate; (3) reaction conditions gentleness and raw material are easy to get, and the possibility of scale operation is arranged.
Embodiment
Provide following example for further setting forth spy of the present invention.Obviously embodiments of the present invention are not limited to subordinate embodiment.
Embodiment 1
Take by weighing the 0.021g palladium, 0.17g dodecyl thioether is dissolved in it in 50mL dehydrated alcohol.Above-mentioned solution gets black Pd nano-particle ethanol solution at 60 ℃ of heated and stirred 1h.The Pd nano-particle ethanol solution of preparation is joined (50mL) in the toluene solution that contains 1.1mL benzyl mercaptan, after stirring 0.5h, in system, add a large amount of distilled water, solution generation layering, the upper strata is the toluene phase that contains the Pd nanoparticle, and lower floor is water and alcoholic acid mixed phase.Remove lower floor's water, the organic phase on upper strata obtains containing the toluene solution of Pd nanoparticle with distilled water wash 3 times.
Take by weighing 0.1g CNTs, it is scattered in the 50mL toluene solution, supersound process 4h gets the suspension of CNTs in toluene.The toluene solution of above-mentioned Pd nanoparticle is joined in the CNTs toluene suspension, and supersound process 10h filters, and washes respectively 3 times with dehydrated alcohol and distilled water, and 120 ℃ of dried overnight get the Pd/CNTs nano composite material.The transmission electron microscope photo shows that the Pd nanoparticle is evenly distributed on the CNTs surface.
Embodiment 2-4
According to method and the step of embodiment 1, but the quality of change dodecyl thioether is respectively:
(2)0.068g(3)0.34g(4)0.68g
Embodiment 5-8
According to method and the step of embodiment 1, the amount that changes benzyl mercaptan is respectively:
(5)0.55ml(6)0.22ml(7)0.11ml(8)0.055ml
Embodiment 9-12
According to method and the step of embodiment 1, benzyl mercaptan is dissolved in benzene respectively, dimethylbenzene, hexanaphthene and octane one of them.
Embodiment 13-16
According to method and the step of embodiment 1, the quality that changes CNTs is respectively
(13)1.0g?(14)0.05g?(15)0.02g?(16)0.01g
Claims (4)
1. the preparation method of a carbon nano-tube supported palladium nano-composite material is characterized in that this method may further comprise the steps:
A. palladium and dodecyl thioether are dissolved in the dehydrated alcohol, under 40-100 ℃ of heated and stirred, obtain black Pd nano-particle ethanol solution;
B. the Pd nano-particle ethanol solution with preparation joins in the organic solvent of the benzene,toluene,xylene, hexanaphthene or the octane that contain benzyl mercaptan, stir, extract ethanol by distilled water, the Pd nanoparticle is transferred in the organic solvent of benzene,toluene,xylene, hexanaphthene or octane;
The organic solvent that C. will contain benzene,toluene,xylene, hexanaphthene or the octane of Pd nanoparticle joins CNTs at benzene, toluene, dimethylbenzene, in the suspension of hexanaphthene or octane, supersound process, filter, wash respectively with dehydrated alcohol and distilled water, drying obtains carbon nano-tube supported palladium nano-composite material.
2. the method for claim 1, the mol ratio that it is characterized in that palladium and dodecyl thioether is 1: 2-1: 20.
3. the method for claim 1, the mol ratio that it is characterized in that palladium and benzyl mercaptan is 1: 5-1: 100.
4. the method for claim 1 is characterized in that Pd and CNTs mass ratio are 0.01-1.
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| CN2009101382587A CN101880038A (en) | 2009-05-08 | 2009-05-08 | Preparation method of carbon nano-tube supported palladium nano-composite material |
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| CN2009101382587A CN101880038A (en) | 2009-05-08 | 2009-05-08 | Preparation method of carbon nano-tube supported palladium nano-composite material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105945277A (en) * | 2016-05-17 | 2016-09-21 | 中国工程物理研究院激光聚变研究中心 | Onion-shaped fullerene clad metal palladium core shell structure nano-particle and preparation method thereof |
-
2009
- 2009-05-08 CN CN2009101382587A patent/CN101880038A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105945277A (en) * | 2016-05-17 | 2016-09-21 | 中国工程物理研究院激光聚变研究中心 | Onion-shaped fullerene clad metal palladium core shell structure nano-particle and preparation method thereof |
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Application publication date: 20101110 |