CN101007273A - In-situ synthesis of Pt-supported fullerene catalyst - Google Patents
In-situ synthesis of Pt-supported fullerene catalyst Download PDFInfo
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- CN101007273A CN101007273A CNA2007100614696A CN200710061469A CN101007273A CN 101007273 A CN101007273 A CN 101007273A CN A2007100614696 A CNA2007100614696 A CN A2007100614696A CN 200710061469 A CN200710061469 A CN 200710061469A CN 101007273 A CN101007273 A CN 101007273A
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Abstract
The invention discloses an original position synthesis method of fullerene Pt catalyst. The method uses the chloroplatinic acid and deionized water to produce chloroplatinic acid solution, places it in containers and then immerses the negative pole and anode under liquid surface to energizing and striking of arc, the electric arc discharges to make the anode evaporate and provide carbon resource for the growth of fullerene structure, while the metal positive ion in brine solution is deacidized to generating Pt metal particles and load is under the surface of fullerene; then stops discharge, collect product after cooling and gains the fullerene Pt catalyst after drying. The innovation of the invention lies on: fullerene is prepared while Pt is loaded on the surface of carbon material, it achieves the original position synthesis of fullerene Pt catalyst; it is tested that the fullerenes Pt catalyst has excellent catalytic activity to carbinol oxidation, and the process is simple and easy to control, the application prospects are charming.
Description
Technical field
The invention belongs to a kind of synthetic method of Pt-supported fullerene catalyst, relate generally to the in-situ synthetic method that a kind of CNT shape fullerene and onion-like fullerene carry the Pt catalyst.
Background technology
The eelctro-catalyst that DMFC is commonly used mainly is carbon (as carbon black, CNT, Graphite Nano Fiber) load platinum (Pt) nano particle of high-specific surface area, makes Pt reach better dispersion, to reduce the consumption of Pt, reduces the cost of catalyst.Fullerene-based material (CNT and onion-like fullerene) has high conductivity, chemistry and advantages such as electrochemical stability, high-specific surface area, has shown wide application prospect gradually as the support applications aspect.The method that the inventor formerly prepares Pt-supported fullerene catalyst is at first to prepare carbon carrier, utilizes technologies such as immersion reduction method, vacuum vapour deposition or electrochemical deposition method that Pt or platinum group metal are stated from the carbon carrier then.The preparation process complexity, influence factor is many, easily introduces impurity, and catalyst performance is had considerable influence.To this, the inventor has done further to grind and test, and has drawn a kind of in-situ synthesis of Pt-supported fullerene catalyst.Effectively avoided carbon in the technology formerly to carry some shortcomings in the Pt catalyst preparation process.
Summary of the invention
The problem to be solved in the present invention be the foregoing invention people formerly carbon carry some shortcomings in the Pt catalyst preparation process, and a kind of in-situ synthesis of new Pt-supported fullerene catalyst is proposed.
The present invention is based on the problems referred to above and purpose, the concrete processing step of in-situ synthesis that has proposed Pt-supported fullerene catalyst is as follows:
1. the in-situ synthesis of a Pt-supported fullerene catalyst is characterized in that the concrete processing step of this method is as follows:
(1) chloroplatinic acid is dissolved in the deionized water, is made into the platinum acid chloride solution that concentration is 0.000965～0.00386mol/L, join in the heatproof container;
(2) graphite for spectroanalysis is immersed under the liquid level, arranges along horizontal linear, two gaps between electrodes are 0.8～1mm, and electric arc ignites;
(4) arc discharge makes the anode evaporation that the carbon source of fullerene structure growth is provided, and the metal cation reduction generates the Pt metallic particles in the salting liquid simultaneously, loads on the surface of fullerene structure;
(5) after discharge finishes, the product of collection container bottom, drying obtains Pt-supported fullerene catalyst.
Wherein, fullerene structure is CNT and onion-like fullerene.
The Pt-supported fullerene catalyst in-situ synthetic method that the present invention realizes according to above-mentioned processing step, its innovation part is when fullerene structure generates Pt to be supported on the carbon material surface, its advantage and good effect are: (1) processing step is simple and easy to control, and preparation time is short; (2) avoid the use of reagent such as strong acid, highly basic, avoided the introducing of the impurity in the preparation process simultaneously; (3) fullerene and Pt particle are pretended usefulness in the synthetic Pt/ fulvene compounding material of original position, help the realization of catalytic process; (4) under the effect of shape fullerene carrier, the decentralization of Pt greatly improves, and has reduced the Pt gathering simultaneously; (5) use the solution of low concentration to make year high catalyst material of Pt amount, greatly reduced cost.
The above-mentioned processing step of the present invention makes Pt-supported fullerene catalyst, after the product collected ground with mortar, get a little ultrasonic dispersion in ethanol, with hanging drop on little grid copper mesh, use JSM-6700F ESEM (SEM) and JEM-2010 type high-resolution-ration transmission electric-lens (HRTEM after dry, accelerating potential is 200kY, and point resolution is 0.19nm) it is observed sign, find that the uniform Pt particle deposition of size is on fullerene structure.Through detecting, this Pt-supported fullerene catalyst has excellent catalytic activity to methanol oxidation, and application prospect is very tempting.
Processing step of the present invention is simple and easy to control, when fullerene generates with the Pt particulate load on the fullerene surface, realized that the original position of Pt-supported fullerene catalyst is synthetic.Fullerene carrier diameter is the 10-50 nanometer, and Pt catalyst granules diameter is the 3-5 nanometer, has realized that the original position of Pt-supported fullerene catalyst is synthetic.
Description of drawings
Fig. 1 is the SEM figure that the present invention makes Pt-supported fullerene catalyst
Fig. 2 is the HRTEM figure that the present invention makes Pt-supported fullerene catalyst
The specific embodiment
Embodiment 1
1 gram chloroplatinic acid is dissolved in and is made into the platinum acid chloride solution that concentration is 0.00193mol/L in the 1L deionized water, join in the heatproof container.Adopt the spectroscopically pure graphite rod to make electrode, wherein the negative electrode diameter is 12mm, and anode diameter is 6mm, and two electrodes are arranged along horizontal linear, are immersed in 40mm place under the liquid level.Electric current and voltage are controlled at 30A and 28V respectively, and must make two gaps between electrodes after the starting the arc is 0.8mm.Arc discharge makes the anode evaporation that the carbon source of fullerene structure growth is provided, and the metal cation reduction generates the Pt metallic particles in the salting liquid simultaneously, loads on the surface of fullerene structure.Stop discharge after 10 minutes, treat the product of collection container bottom after the water cooling, evaporating water just obtains Pt-supported fullerene catalyst.Wherein, described fullerene structure is CNT and onion-like fullerene.
Embodiment 2
1 gram chloroplatinic acid is dissolved in and is made into the platinum acid chloride solution that concentration is 0.000965mol/L in the 2L deionized water, join in the heatproof container.Adopt the spectroscopically pure graphite rod to make electrode, wherein the negative electrode diameter is 12mm, and anode diameter is 6mm, and two electrodes are arranged along horizontal linear, are immersed in 40mm place under the liquid level.Electric current and voltage are controlled at 30A and 28V respectively, and must make two gaps between electrodes after the starting the arc is 1mm.Arc discharge makes the anode evaporation that the carbon source of fullerene structure growth is provided, and the metal cation reduction generates the Pt metallic particles in the salting liquid simultaneously, loads on the surface of fullerene structure.Stop discharge after 10 minutes, treat the product of collection container bottom after the water cooling, evaporating water just obtains Pt-supported fullerene catalyst.Wherein, described fullerene structure is CNT and onion-like fullerene.
Embodiment 3
1 gram chloroplatinic acid is dissolved in and is made into the platinum acid chloride solution that concentration is 0.00386mol/L in the 0.5L deionized water, join in the heatproof container.Adopt the spectroscopically pure graphite rod to make electrode, wherein the negative electrode diameter is 12mm, and anode diameter is 6mm, and two electrodes are arranged along horizontal linear, are immersed in 40mm place under the liquid level.Electric current and voltage are controlled at 30A and 28V respectively, and must make two gaps between electrodes after the starting the arc is 1mm.Arc discharge makes the anode evaporation that the carbon source of fullerene structure growth is provided, and the metal cation reduction generates the Pt metallic particles in the salting liquid simultaneously, loads on the surface of fullerene structure.Stop discharge after 10 minutes, treat the product of collection container bottom after the water cooling, evaporating water just obtains Pt-supported fullerene catalyst.Wherein, described fullerene structure is CNT and onion-like fullerene.
Claims (2)
1. the in-situ synthesis of a Pt-supported fullerene catalyst is characterized in that the concrete processing step of this method is as follows:
(1) chloroplatinic acid is dissolved in the deionized water, is made into the platinum acid chloride solution that concentration is 0.000965～0.00386mol/L, join in the heatproof container;
(2) graphite for spectroanalysis is immersed under the liquid level, arranges along horizontal linear, two gaps between electrodes are 0.8～1mm, and electric arc ignites;
(4) arc discharge makes the anode evaporation that the carbon source of fullerene structure growth is provided, and the metal cation reduction generates the Pt metallic particles in the salting liquid simultaneously, loads on the surface of fullerene structure;
(5) after discharge finishes, the product of collection container bottom, drying obtains Pt-supported fullerene catalyst.
2. the in-situ synthesis of the described a kind of Pt-supported fullerene catalyst of claim 1 is characterized in that fullerene structure is CNT and onion-like fullerene.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007100614696A CN101007273A (en) | 2007-01-26 | 2007-01-26 | In-situ synthesis of Pt-supported fullerene catalyst |
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| CNA2007100614696A CN101007273A (en) | 2007-01-26 | 2007-01-26 | In-situ synthesis of Pt-supported fullerene catalyst |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102656730A (en) * | 2009-12-14 | 2012-09-05 | 原子能与替代能源委员会 | Electrochemical reactor and active layer integrated into said reactor |
| CN105576257A (en) * | 2015-12-21 | 2016-05-11 | 太原理工大学 | Method using underwater arc discharge to prepare graphene supported Pt catalyst |
| CN106680355A (en) * | 2017-01-04 | 2017-05-17 | 太原理工大学 | Method for detecting sunset yellow in food by using carbon onion-loaded Pt nano particle composite material |
| CN108409579A (en) * | 2018-02-08 | 2018-08-17 | 太原理工大学 | A kind of method that the carbon onion load monatomic catalyst of Pt is used for aromatic nitro compound catalytic hydrogenation |
-
2007
- 2007-01-26 CN CNA2007100614696A patent/CN101007273A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102656730A (en) * | 2009-12-14 | 2012-09-05 | 原子能与替代能源委员会 | Electrochemical reactor and active layer integrated into said reactor |
| CN102656730B (en) * | 2009-12-14 | 2015-08-05 | 原子能与替代能源委员会 | Electrochemical reactor and the active layer be integrated in described reactor |
| CN105576257A (en) * | 2015-12-21 | 2016-05-11 | 太原理工大学 | Method using underwater arc discharge to prepare graphene supported Pt catalyst |
| CN106680355A (en) * | 2017-01-04 | 2017-05-17 | 太原理工大学 | Method for detecting sunset yellow in food by using carbon onion-loaded Pt nano particle composite material |
| CN106680355B (en) * | 2017-01-04 | 2019-06-28 | 太原理工大学 | Utilize the method for sunset yellow in carbon onion supporting Pt nano particle composite material detection food |
| CN108409579A (en) * | 2018-02-08 | 2018-08-17 | 太原理工大学 | A kind of method that the carbon onion load monatomic catalyst of Pt is used for aromatic nitro compound catalytic hydrogenation |
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