CN105552390A - Platinum-based/molybdenum-based compound-carbon catalyst and preparation method therefor - Google Patents
Platinum-based/molybdenum-based compound-carbon catalyst and preparation method therefor Download PDFInfo
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- CN105552390A CN105552390A CN201510953271.3A CN201510953271A CN105552390A CN 105552390 A CN105552390 A CN 105552390A CN 201510953271 A CN201510953271 A CN 201510953271A CN 105552390 A CN105552390 A CN 105552390A
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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Abstract
The invention discloses a platinum-based/molybdenum-based compound-carbon catalyst and a preparation method therefor. The platinum-based/molybdenum-based compound-carbon catalyst is prepared from a platinum-and-molybdenum-based compound-carbon carrier; the specific preparation method comprises the following steps of 1, weighing a molybdenum-based compound precursor and a carbon material, mixing with deionized water, and performing ultrasonic dispersion for 1-3h; 2, putting the mixture into a water bath kettle for heating and stirring at a temperature of 70-90 DEG C to obtain a mixture A; 3, drying the mixture A, and putting the dried mixture A into a tubular furnace under inert atmosphere protection for performing heating and annealing treatment to obtain a material B, and namely obtaining the molybdenum-based compound-carbon carrier; and 4, taking the material B as the carrier, preparing the molybdenum-based catalyst by an ethylene glycol reduction method taking microwave as an auxiliary part to obtain the platinum-based/molybdenum-based compound-carbon catalyst. According to the preparation method, the molybdenum-based compound is compounded with the carbon material, so that more oxygen-containing groups are provided, more active sites are provided for platinum particles, and the activity of the catalyst is improved consequently.
Description
Technical field
The invention belongs to field of material technology, relate to a kind of novel platinum based catalyst and preparation method thereof, be specifically related to a kind of platinum base/molybdenum based compound-C catalyst and preparation method thereof.
Background technology
Direct methanol fuel cell (DMFC) due to its there is high-energy-density, be easy to charging, the advantage such as the fast and fail safe of cold-starting speed is good, attracted increasing researcher to pay close attention to, focus is researched and developed in the application becoming Portable power source.Wherein, carrier material, as the core material of anode catalyst, has important impact for the activity and stability improving anode catalyst.
Catalyst carrier, except adopting new carbon (carbon nano-tube, carbon nano-fiber etc.) improvement, also can adopt some as carbide (TiC, WC), inorganic, metal oxide (VO
x, SnO
2) and conducting polymer (polystyrolsulfon acid, poly-3,4-Ethylenedioxy Thiophene) etc. improve.Above novel carriers material can strengthen metal-support interaction, improve the corrosion resistance etc. of catalyst, thus improves activity and the stability of catalyst.
Carrier material is indispensable key component in catalyst composition, and it affects the performance of catalyst and even whole battery, life-span and validity to a great extent.Therefore, the research for novel carriers material has very important effect.
Summary of the invention
The object of this invention is to provide a kind of novel platinum base/molybdenum based compound-C catalyst and preparation method thereof, by by molybdenum based compound and material with carbon element compound, provide more oxy radical, for platinum particles provides more active sites, thus improve the activity of catalyst.
The object of the invention is to be achieved through the following technical solutions:
A kind of platinum base/molybdenum based compound-C catalyst, be prepared from by platinum and molybdenum based compound-carbon carrier, the mass ratio of platinum and molybdenum based compound-carbon carrier is 1: 0.25 ~ 1: 19, described molybdenum based compound-carbon carrier is prepared from by molybdenum based compound presoma and material with carbon element, and the mass ratio of molybdenum based compound presoma and material with carbon element is 1: 0.5 ~ 1.
A kind of preparation method of above-mentioned platinum base/molybdenum based compound-C catalyst, first molybdenum based compound-carbon composite is prepared by mechanical mixture, annealing method, and in this, as catalyst carrier, by microwave radiation technology reduction of ethylene glycol legal system for platinum based catalyst, finally obtain the higher and stability good platinum base/molybdenum based compound-C catalyst of electro-chemical activity.Concrete steps are as follows:
One, the mixing of a certain amount of molybdenum based compound presoma, material with carbon element and deionized water is taken, ultrasonic disperse 1 ~ 3h;
Two, to put it in water-bath 70 ~ 90 DEG C to carry out adding thermal agitation, obtain mixture A;
Three, mixture A is dry, and be placed with in the tube furnace of inert atmosphere protection and carry out thermal anneal process, controlling annealing temperature is 700 ~ 900 DEG C, and annealing time is 1 ~ 3h, when temperature is down to room temperature, obtains material B, i.e. molybdenum based compound-carbon carrier;
Four, using material B as carrier, by microwave radiation technology reduction of ethylene glycol legal system for platinum based catalyst, obtain platinum base/molybdenum based compound-C catalyst.
In above-mentioned preparation method, the one in the mixture (mass ratio 2: 1) of mixture, ammonium molybdate and the thiocarbamide of described molybdenum based compound presoma ammonium molybdate, ammonium molybdate and diammonium hydrogen phosphate (mass ratio 1: 1).
In above-mentioned preparation method, the mass ratio of described molybdenum based compound presoma, material with carbon element and deionized water is 1: 0.5 ~ 1: 1 ~ 3.
In above-mentioned preparation method, described material with carbon element is carbon dust or carbon nano-tube.
In above-mentioned preparation method, described platinum based catalyst is loaded Pt single-metal reforming catalyst.
In above-mentioned preparation method, described molybdenum based compound-carbon carrier is nano level composite material.
Tool of the present invention has the following advantages:
1, molybdenum based compound is as co-catalyst, for nano platinum particle provides more oxy radical, is of value to platinum particles deposition on this carrier, thus improves the electro catalytic activity of catalyst.
2, molybdenum based compound is as inorganic metal compound, enhances the corrosion resistance of carrier, improves the activity of catalyst.
3, this preparation method simple possible, improves activity and the stability of platinum based catalyst largely, is expected to commercial applications.
Accompanying drawing explanation
Fig. 1 is Pt/MoO
3-C catalyst transmission electron microscope photo;
Fig. 2 is Pt/MoO
3-C and Pt/C two kinds of catalyst are at 0.5mol/LH
2sO
4cyclic voltammetry curve in solution;
Fig. 3 is Pt/MoO
3-C and Pt/C two kinds of catalyst are at 0.5mol/LH
2sO
4and 0.5mol/LCH
3the cyclic voltammetry curve of anodic oxidation of methanol in OH solution;
Fig. 4 is Pt/MoO
3-C and Pt/C two kinds of catalyst are at 0.5mol/LH
2sO
4and 0.5mol/LCH
3electrochemical impedance spectroscopy in OH solution.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but do not limit to so; everyly technical solution of the present invention modified or equivalent to replace, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
Embodiment one: present embodiment prepares platinum/molybdenum trioxide-carbon nano-tube catalyst in accordance with the following steps:
Take the mixing of 40mg ammonium molybdate, 40mg carbon nano-tube and 60mL deionized water, ultrasonic disperse 1h; To put it in water-bath 80 DEG C to carry out adding thermal agitation, obtain mixture; Mixture is dry, and be placed with in the tube furnace of inert atmosphere protection and carry out 750 DEG C of thermal anneal process, annealing time is 1h, when temperature is down to room temperature, obtains molybdenum trioxide-carbon nano tube compound material; Using molybdenum trioxide-carbon nano tube compound material as carrier, by microwave radiation technology reduction of ethylene glycol legal system for platinum based catalyst, obtain platinum/molybdenum trioxide-carbon nano-tube catalyst, wherein: the mass ratio of platinum and molybdenum trioxide-carbon nanotube carrier is 1: 4.
Embodiment two: present embodiment prepares platinum/phosphating sludge-C catalyst in accordance with the following steps:
Take the mixing of 40mg ammonium molybdate, 40mg diammonium hydrogen phosphate, 30mg carbon dust and 50mL deionized water, ultrasonic disperse 2h; To put it in water-bath 60 DEG C to carry out adding thermal agitation, obtain mixture; Mixture is dry, and be placed with in the tube furnace of inert atmosphere protection and carry out 800 DEG C of thermal anneal process, annealing time is 2h, when temperature is down to room temperature, obtains phosphating sludge-carbon composite; Using phosphating sludge-carbon composite as carrier, by microwave radiation technology reduction of ethylene glycol legal system for platinum based catalyst, obtain platinum/phosphating sludge-C catalyst, wherein: the mass ratio of platinum and molybdenum trioxide-carbon nanotube carrier is 1: 0.25.
Embodiment three: present embodiment prepares platinum/molybdenum sulfide-C catalyst in accordance with the following steps:
Take the mixing of 40mg ammonium molybdate, 80mg thiocarbamide, 25mg carbon dust and 80mL deionized water, ultrasonic disperse 3h; To put it in water-bath 70 DEG C to carry out adding thermal agitation, obtain mixture; Mixture is dry, and be placed with in the tube furnace of inert atmosphere protection and carry out 850 DEG C of thermal anneal process, annealing time is 2h, when temperature is down to room temperature, obtains molybdenum sulfide-carbon composite; Using molybdenum sulfide-carbon composite as carrier, by microwave radiation technology reduction of ethylene glycol legal system for platinum based catalyst, obtain platinum/molybdenum sulfide-C catalyst, wherein: the mass ratio of platinum and molybdenum trioxide-carbon nanotube carrier is 1: 1.5.
Embodiment four: present embodiment prepares platinum/molybdenum trioxide-C catalyst in accordance with the following steps:
Take the mixing of 40mg ammonium molybdate, 20mg carbon and 50mL deionized water, ultrasonic disperse 1h; To put it in water-bath 80 DEG C to carry out adding thermal agitation, obtain mixture; Mixture is dry, and be placed with in the tube furnace of inert atmosphere protection and carry out 900 DEG C of thermal anneal process, annealing time is 1h, when temperature is down to room temperature, obtains molybdenum trioxide-carbon composite; Using molybdenum trioxide-carbon composite as carrier, by microwave radiation technology reduction of ethylene glycol legal system for platinum based catalyst, obtain platinum/molybdenum trioxide-C catalyst, wherein: the mass ratio of platinum and molybdenum trioxide-carbon nanotube carrier is 1: 4, and performance test results as Figure 1-4.
As seen from Figure 1, platinum particles is deposited on molybdenum trioxide-carbon carrier.
Can be seen by Fig. 2, Pt/MoO
3the electrochemical surface area of the Pt of-C catalyst exceeds about 14Amg than Pt/C catalyst
-1.
Can be seen by Fig. 3, Pt/MoO
3-C is higher than the oxidation peak current density of methyl alcohol on Pt/C catalyst, is about 1.7 times of Pt/CNT catalyst, shows good electrocatalysis characteristic.
Can obviously be found out by Fig. 4, Pt/MoO
3the reaction arc of-C catalyst is less than Pt/C, shows MoO
3existence electrochemical reaction speed can be made to accelerate.
Embodiment five: present embodiment prepares platinum/molybdenum trioxide-carbon nano-tube catalyst in accordance with the following steps:
Take the mixing of 40mg ammonium molybdate, 40mg carbon nano-tube and 60mL deionized water, ultrasonic disperse 1h; To put it in water-bath 80 DEG C to carry out adding thermal agitation, obtain mixture; Mixture is dry, and be placed with in the tube furnace of inert atmosphere protection and carry out 750 DEG C of thermal anneal process, annealing time is 1h, when temperature is down to room temperature, obtains molybdenum trioxide-carbon nano tube compound material; Using molybdenum trioxide-carbon nano tube compound material as carrier, by microwave radiation technology reduction of ethylene glycol legal system for platinum based catalyst, obtain platinum/molybdenum trioxide-carbon nano-tube catalyst, wherein: the mass ratio of platinum and molybdenum trioxide-carbon nanotube carrier is 1: 6.5.
Embodiment six: present embodiment prepares platinum/molybdenum trioxide-carbon nano-tube catalyst in accordance with the following steps:
Take the mixing of 40mg ammonium molybdate, 40mg carbon nano-tube and 60mL deionized water, ultrasonic disperse 1h; To put it in water-bath 80 DEG C to carry out adding thermal agitation, obtain mixture; Mixture is dry, and be placed with in the tube furnace of inert atmosphere protection and carry out 750 DEG C of thermal anneal process, annealing time is 1h, when temperature is down to room temperature, obtains molybdenum trioxide-carbon nano tube compound material; Using molybdenum trioxide-carbon nano tube compound material as carrier, by microwave radiation technology reduction of ethylene glycol legal system for platinum based catalyst, obtain platinum/molybdenum trioxide-carbon nano-tube catalyst, wherein: the mass ratio of platinum and molybdenum trioxide-carbon nanotube carrier is 1: 10.5.
Embodiment seven: present embodiment prepares platinum/molybdenum trioxide-carbon nano-tube catalyst in accordance with the following steps:
Take the mixing of 40mg ammonium molybdate, 40mg carbon nano-tube and 60mL deionized water, ultrasonic disperse 1h; To put it in water-bath 80 DEG C to carry out adding thermal agitation, obtain mixture; Mixture is dry, and be placed with in the tube furnace of inert atmosphere protection and carry out 750 DEG C of thermal anneal process, annealing time is 1h, when temperature is down to room temperature, obtains molybdenum trioxide-carbon nano tube compound material; Using molybdenum trioxide-carbon nano tube compound material as carrier, by microwave radiation technology reduction of ethylene glycol legal system for platinum based catalyst, obtain platinum/molybdenum trioxide-carbon nano-tube catalyst, wherein: the mass ratio of platinum and molybdenum trioxide-carbon nanotube carrier is 1: 13.5.
Claims (8)
1. platinum base/molybdenum based compound-C catalyst, is characterized in that described catalyst is prepared from by platinum and molybdenum based compound-carbon carrier, wherein: the mass ratio of platinum and molybdenum based compound-carbon carrier is 1: 0.25 ~ 1: 19.
2. platinum base according to claim 1/molybdenum based compound-C catalyst, it is characterized in that described molybdenum based compound-carbon carrier is prepared from by molybdenum based compound presoma and material with carbon element, wherein: the mass ratio of molybdenum based compound presoma and material with carbon element is 1: 0.5 ~ 1.
3. platinum base according to claim 2/molybdenum based compound-C catalyst, is characterized in that the one in the mixture of the mixture of described molybdenum based compound presoma ammonium molybdate, ammonium molybdate and diammonium hydrogen phosphate, ammonium molybdate and thiocarbamide.
4. platinum base according to claim 3/molybdenum based compound-C catalyst, is characterized in that the mass ratio of described ammonium molybdate and diammonium hydrogen phosphate is 1: 1, and the mass ratio of ammonium molybdate and thiocarbamide is 2: 1.
5. platinum base according to claim 2/molybdenum based compound-C catalyst, is characterized in that described material with carbon element is carbon dust or carbon nano-tube.
6. a preparation method for platinum base described in the arbitrary claim of claim 1-5/molybdenum based compound-C catalyst, is characterized in that described method step is as follows:
One, the mixing of molybdenum based compound presoma, material with carbon element and deionized water is taken, ultrasonic disperse 1 ~ 3h;
Two, to put it in water-bath 70 ~ 90 DEG C to carry out adding thermal agitation, obtain mixture A;
Three, mixture A is dry, and be placed with in the tube furnace of inert atmosphere protection and carry out thermal anneal process, controlling annealing temperature is 700 ~ 900 DEG C, and annealing time is 1 ~ 3h, when temperature is down to room temperature, obtains material B, i.e. molybdenum based compound-carbon carrier;
Four, using material B as carrier, by microwave radiation technology reduction of ethylene glycol legal system for platinum based catalyst, obtain platinum base/molybdenum based compound-C catalyst.
7. the preparation method of platinum base according to claim 6/molybdenum based compound-C catalyst, is characterized in that the mass ratio of described molybdenum based compound presoma, material with carbon element and deionized water is 1: 0.5 ~ 1: 1 ~ 3.
8. the preparation method of platinum base according to claim 6/molybdenum based compound-C catalyst, is characterized in that described molybdenum based compound-carbon carrier is nano level composite material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109821564A (en) * | 2019-01-23 | 2019-05-31 | 湘潭大学 | A kind of preparation method and catalyst of coated catalyst |
| CN110961101A (en) * | 2019-12-24 | 2020-04-07 | 西南大学 | Platinum-based catalyst, preparation method and application thereof |
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| CN110961101B (en) * | 2019-12-24 | 2022-12-06 | 西南大学 | Platinum-based catalyst, preparation method and application thereof |
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