CN109994747A - The preparation method of high carrying capacity noble metal carbon nanocatalyst - Google Patents
The preparation method of high carrying capacity noble metal carbon nanocatalyst Download PDFInfo
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- CN109994747A CN109994747A CN201711471803.5A CN201711471803A CN109994747A CN 109994747 A CN109994747 A CN 109994747A CN 201711471803 A CN201711471803 A CN 201711471803A CN 109994747 A CN109994747 A CN 109994747A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The present invention relates to a kind of methods that can largely prepare high carrying capacity noble metal carbon nanocatalyst, include the following steps: for precious metal salt to be prepared into metal carbonyl clusters solvent；Surfactant is added in activated carbon and ultrasonic disperse is uniform；The metal carbonyl clusters solvent is mixed with the active carbon solution that is uniformly dispersed；The mixed liquor is stirred, air is filled with, oxidation obtains metal noble metal；Finally high carrying capacity carbon supported noble metal nanocatalyst will be obtained after solution filtering, cleaning, drying.Surfactant and Carbonyl Clusters method are used in conjunction in preparation method of the invention, are made catalyst loading height of preparation, good dispersion, uniform, can largely be prepared.
Description
Technical field
The present invention relates to field of new energy technologies more particularly to a kind of preparation sides of high carrying capacity noble metal carbon nanocatalyst
Method.
Background technique
Proton Exchange Membrane Fuel Cells is the device that a kind of chemical energy by hydrogen and oxygen is directly translated into electric energy, is had
The advantages that no pollution, high energy conversion efficiency, it is considered to be one of following best energy.In recent years in relation to pem fuel
The research of cell catalyst is concentrated mainly on low noble metal dosage (alloy, core-shell structure, hetero-junctions, hollow sphere etc.) and your non-gold
In terms of metal catalyst (carbon-based, transition metal oxide, Metallomacrocycle race), although the use of this kind of catalyst can substantially reduce
The cost of fuel cell, but its catalytic efficiency and service life are not met by the demand of current fuel cell, and noble metal base is urged
Agent (Pt/C, Pd/C) is current main fuel cell nano catalyst, how to improve the preparation side of Pt/C, Pd/C catalyst
Method can largely be prepared with realistic meaning.
The research paper delivered at present largely focuses on the research of the catalyst of noble metal carrying capacity low (< 40wt%), so
And in practical applications, to reduce the internal resistance of cell, inside battery mass transfer is promoted, this just needs the catalyst of high metal carrying capacity.Cause
This, the carbon supported noble metal catalyst of preparation high metal carrying capacity, the high activity that metal dispersion is good, metal partial size is small and stability is more
Has meaning.But when preparing high carrying capacity catalyst, metal material is easy to reunite, is led to nanoparticle due to the nano-meter characteristic of itself
Son is non-uniformly distributed in carbon support；Carbon carrier can also settle in prolonged reaction process, also lead to noble metal
Nanoparticle is not easy to disperse on its surface.
Therefore it is current that preparation high metal carrying capacity, which has both metal nanoparticle to have fine dispersion degree in carbon support,
A major challenge.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of preparation sides of high carrying capacity noble metal carbon nanocatalyst
Method prepares the noble metal carbon nanocatalyst with the high carrying capacity of good dispersion.
To solve the above-mentioned problems, the present invention provides a kind of preparation method of high carrying capacity noble metal carbon nanocatalyst,
Include the following steps:
Step 1: weighing precious metal chemical complex, it is 5g/L~10g/L that solvent, which is added, and is diluted to platinum concentration, is added under stiring
Inorganic base adjusts pH to 8~12, is passed through CO gas, and stirring 12h~72h forms metal carbonyl clusters；
Step 2: being 250m by specific surface area2/ g~1600m2/ g, activated carbon of the average grain diameter in 20nm~100nm are added
Into deionized water, so that the concentration of carbon is 1g/L~15g/L, surfactant, activated carbon and surfactant is then added
Mass ratio be 1:(0.01~2)；
Step 3: two kinds of solution that mixing step 1 and step 2 obtain, so that in mixed solution, the quality of noble metal and carbon
Than for 1:(0.6~9) it is filled with oxygen-containing gas and is aoxidized, for 24 hours~96h is stirred under the conditions of 20 DEG C~50 DEG C, uses deionized water
Cleaning filtering, obtains high carrying capacity noble metal carbon nanocatalyst after dry.
Optionally, the noble metal is platinum or palladium.
Optionally, the precious metal chemical complex is chlorine noble metal acid sodium, nitric acid noble metal, sulfuric acid noble metal and noble metal ammonia
At least one of complex.
Optionally, the solvent is ethyl alcohol, propyl alcohol, tetrahydrofuran, N, in N- dimethyl pyrazole network alkanone and toluene at least
It is a kind of.
Optionally, the inorganic base is NaOH, KOH, CH3COONa、NaCO3At least one of with ammonium hydroxide.
Optionally, the surfactant is lauryl sodium sulfate, neopelex, cetyl sulfonic acid
Sodium, cetyl benzenesulfonic acid sodium, polyvinylpyrrolidone, polyvinyl alcohol, 1-Methyl-2-Pyrrolidone, citrate and second two
At least one of amine tetraacethyl sodium.
Optionally, the activated carbon is VXC-72, VXC-72R, BP2000, EC-300, EC-600, ordered mesopore carbon, carbon
At least one of nanofiber and carbon nanotube.
Optionally, in the high carrying capacity noble metal carbon nanocatalyst obtained in step 3, the mass ratio of noble metal and carbon
It is 40%~90%.
Optionally, in step 2, it is added after surfactant, carries out ultrasonic disperse 30min~60min.
The preparation method of high carrying capacity noble metal carbon nanocatalyst of the invention passes through metal carbonyl clusters method and right
The surface of activated carbon is modified, suitable for largely preparing high carrying capacity noble metal carbon nanocatalyst, obtains with high metal carrying capacity, particle
Uniformly, the high nanocatalyst of metallic dispersion degree.The catalyst prepared in the present invention has in fuel cell practical process
There are higher electro catalytic activity and stability.
Detailed description of the invention
Fig. 1 is the transmission electron microscope photo of the 40wt.%Pt/C catalyst prepared in the embodiment of the invention；
Fig. 2 is the transmission electron microscope photo of the 70wt.%Pt/C catalyst prepared in the embodiment of the invention；
Fig. 3 is the linear of the 40wt.%Pt/C and commercialization 40wt.%Pt/C prepared in the embodiment of the invention
Scan volt-ampere curve.
Specific embodiment
With reference to the accompanying drawing to the specific reality of the preparation method of high carrying capacity noble metal carbon nanocatalyst provided by the invention
The mode of applying elaborates.
In a specific embodiment of the invention, the preparation method of the high carrying capacity noble metal carbon nanocatalyst includes as follows
Step:
Step 1: weighing precious metal chemical complex, it is 5~10g/L that solvent, which is added, and is diluted to platinum concentration, and nothing is added under stiring
Machine alkali adjusts pH to 8~12, is passed through CO gas, and 12~72h of stirring forms metal carbonyl clusters.
The precious metal chemical complex can match for chlorine noble metal acid sodium, nitric acid noble metal, sulfuric acid noble metal and noble metal ammonia
Close at least one of object；Wherein the noble metal can be the noble metals such as platinum or palladium.The solvent can for ethyl alcohol, propyl alcohol,
Tetrahydrofuran, N, at least one of N- dimethyl pyrazole network alkanone and toluene.The inorganic base can for NaOH, KOH,
CH3COONa、NaCO3At least one of with ammonium hydroxide.CO gas is precursors, whole process is participated in, with precious metal atom
Complexing occurs and forms metal carbonyl clusters.By forming metal carbonyl clusters, enable to metal partial size small, size is equal
It is even, additionally it is possible to increase metal nanoparticle in subsequent loading process, the active force between activity carbon carrier improves catalyst
Activity and stability.
Step 2: being 250m by specific surface area2/ g~1600m2/ g, activated carbon of the average grain diameter in 20nm~100nm are added
Into deionized water, so that the concentration of carbon is 1g/L~15g/L, surfactant, activated carbon and surfactant is then added
Mass ratio be 1:(0.01~2).
The surfactant can be lauryl sodium sulfate, neopelex, sodium cetanesulfonate, ten
Six sodium alkyl benzene sulfonates, polyvinylpyrrolidone, polyvinyl alcohol, 1-Methyl-2-Pyrrolidone, citrate, ethylenediamine tetrem
At least one of sour sodium.The activated carbon can be VXC-72, VXC-72R, BP2000, EC-300, EC-600, order mesoporous
At least one of carbon, carbon nano-fiber and carbon nanotube.
Due to the Nano-property of carbon carrier itself and the hydrophobicity on surface, carbon carrier is reunited together in the solution,
After surfactant is added, carbon monodisperse as far as possible may make in the solution, carbon carrier sedimentation is placed, so that noble metal nano
Particle can be uniformly dispersed in carbon surface in loading process, and the uniform performance of particle size is controlled, and increasing carbon carrier can bear
The bullion content of load.After the surfactant is added, ultrasonic disperse can also be carried out to solution, further increase carbon
Monodisperse degree；The ultrasonic disperse can continue 30min~60min.
Step 3: two kinds of solution that mixing step 1 and step 2 obtain, so that in mixed solution, the quality of noble metal and carbon
Than for 1:(0.6~9), it is filled with oxygen-containing gas and is aoxidized, 24~96h is stirred under the conditions of 20 DEG C~50 DEG C, uses deionized water
Cleaning filtering, obtains high carrying capacity noble metal carbon nanocatalyst after dry.
Since metal carbonyl clusters, such as carbonyl platinum or carbonylic palladium have reproducibility, it is to allow that oxygen-containing gas, which is added,
The Precious metal oxidation of high-valence state is at zeroth order.In order to control reaction speed, need to control oxygen content, generally with air compared with
It is good, in other specific embodiments, it can also be passed through the gas with certain oxygen content according to the actual situation.Reaction to be oxidized
After the completion, filtering 5~8 times is cleaned with deionized water；Place into vacuum drying oven and dry, for example, at 60 DEG C dry 180~
360min。
The following are the embodiments of several methods for preparing high carrying capacity noble metal carbon nanocatalyst.
Embodiment 1
(1) preparation of metal carbonyl clusters:
Platinic sodium chloride is weighed, it is 5g/L that 4L tetrahydrofuran, which is added, and is diluted to platinum concentration, and sodium acetate is added under stiring, adjusts
PH to 8, is passed through CO gas, and stirring forms metal carbonyl clusters for 24 hours；
(2) dispersion of activity carbon carrier:
BP2000 is added into 10L deionized water, so that the solubility of carbon is 3g/L, lauryl sodium sulfate is added, makes
Obtaining its concentration is 0.3g/L, ultrasonic disperse 30min.
(3) two kinds of solution in mixing step (1) and (2), wherein the mass ratio of platinum and carbon is 2:3, air is filled with, 50
It is stirred for 24 hours under the conditions of DEG C.
(4) to after the reaction was completed, clean filtering 5~8 times with deionized water.
(5) it is put into vacuum drying oven, continues 180~360min at 60 DEG C.
(6) filter cake after taking-up is dry, obtains catalyst sample after breaing up.
As shown in Figure 1 for using the transmission electron microscope of 40wt.%Pt/C catalyst obtained by preparation method in embodiment 1 photograph
Piece, it can be seen that small and uniform using catalyst granules prepared by this method, the dispersion degree of nanoparticle is high, passes through Fig. 3
Linear sweep voltammetry curve nanocatalyst activity obtained by the present invention can be obtained be better than commercialized 40wt.%Pt/C nanometers and urge
Agent activity.
Embodiment 2
(1) preparation of metal carbonyl clusters:
Platinic sodium chloride is weighed, it is 5g/L that 4L tetrahydrofuran, which is added, and is diluted to platinum concentration, and sodium acetate is added under stiring, adjusts
PH to 10, is passed through CO gas, and stirring forms metal carbonyl clusters for 24 hours；
(2) dispersion of activity carbon carrier:
BP2000 is added into 2.85L deionized water, so that the solubility of carbon is 3g/L, the dodecyl of 0.3g/L is added
Sodium sulphate, ultrasonic disperse 30min.
(3) two kinds of solution in mixing step (1) and (2), wherein the mass ratio of platinum and carbon is 7:3, air is filled with, 50
It is stirred under the conditions of DEG C for 24 hours,
(4) to after the reaction was completed, clean filtering 5~8 times with deionized water；
(5) it is put into vacuum drying oven, 180~360min at 60 DEG C；
(6) filter cake after taking-up is dry, obtains catalyst sample after breaing up.
It is illustrated in figure 2 the transmission electron microscope using 70wt.%Pt/C catalyst obtained by the preparation method in embodiment 2
Photo, it can be seen that small and uniform using catalyst granules prepared by this method, the dispersion degree of nanoparticle is high.
Embodiment 3
(1) preparation of metal carbonyl clusters:
Palladium nitrate is weighed, it is 5g/L that 4L tetrahydrofuran, which is added, and is diluted to palladium concentration, and sodium acetate is added under stiring, adjusts pH
To 9, it is passed through CO gas, stirring forms metal-carbonyl palladium cluster compound for 24 hours；
(2) dispersion of activity carbon carrier:
VXC-72R is added into 10L deionized water, so that the solubility of carbon is 3g/L, lauryl sodium sulfate is added, makes
Obtaining its concentration is 0.3g/L, ultrasonic disperse 30min.
(3) two kinds of solution in mixing step (1) and (2), wherein the mass ratio of palladium and carbon is 2:3, air is filled with, 50
It is stirred under the conditions of DEG C for 24 hours,
(4) to after the reaction was completed, clean filtering 5~8 times with deionized water；
(5) it is put into vacuum drying oven, 180~360min at 60 DEG C；
(6) filter cake after taking-up is dry, obtains 40wt%Pb/C catalyst sample after breaing up.
Activated carbon through surfactant and ultrasonic treatment, is enhanced the dispersibility of activated carbon by the present invention, it is therefore prevented that activity
The sedimentation of carbon improves nano-metal particle in the dispersion degree on its surface, increases the tenor that carbon carrier can load；Separately
Outside, not only make metal partial size small, uniform in size by metal carbonyl clusters method, also add nanoparticle and activated carbon
Active force between carrier improves the activity and stability of catalyst.Therefore, surfactant in preparation method of the invention
With being used in conjunction with for Carbonyl Clusters method, makes catalyst loading height of preparation, good dispersion, uniform, can largely prepare.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should be regarded as
Protection scope of the present invention.
Claims (9)
1. a kind of preparation method of high carrying capacity noble metal carbon nanocatalyst, which comprises the steps of:
Step 1: weighing precious metal chemical complex, it is 5g/L~10g/L that solvent, which is added, and is diluted to platinum concentration, is added under stiring inorganic
Alkali adjusts pH to 8~12, is passed through CO gas, and stirring 12h~72h forms metal carbonyl clusters；
Step 2: being 250m by specific surface area2/ g~1600m2/ g, average grain diameter are added in the activated carbon of 20nm~100nm to going
In ionized water, so that the concentration of carbon is 1g/L~15g/L, surfactant, the matter of activated carbon and surfactant is then added
Amount is than being 1:(0.01~2)；
Step 3: two kinds of solution that mixing step 1 and step 2 obtain, so that in mixed solution, the mass ratio of noble metal and carbon is
1:(0.6~9) it is filled with oxygen-containing gas and is aoxidized, for 24 hours~96h is stirred under the conditions of 20 DEG C~50 DEG C, is cleaned with deionized water
Filtering obtains high carrying capacity noble metal carbon nanocatalyst after dry.
2. the preparation method of high carrying capacity noble metal carbon nanocatalyst according to claim 1, which is characterized in that described expensive
Metallic compound is at least one of chlorine noble metal acid sodium, nitric acid noble metal, sulfuric acid noble metal and noble metal amine complex.
3. the preparation method of high carrying capacity noble metal carbon nanocatalyst according to claim 2, which is characterized in that described expensive
Metal is platinum or palladium.
4. the preparation method of high carrying capacity noble metal carbon nanocatalyst according to claim 1, which is characterized in that described molten
Agent is ethyl alcohol, propyl alcohol, tetrahydrofuran, N, one of N- dimethyl pyrazole network alkanone and toluene.
5. the preparation method of high carrying capacity noble metal carbon nanocatalyst according to claim 1, which is characterized in that the nothing
Machine alkali is NaOH, KOH, CH3COONa、NaCO3At least one of with ammonium hydroxide.
6. the preparation method of high carrying capacity noble metal carbon nanocatalyst according to claim 1, which is characterized in that the table
Face activating agent is lauryl sodium sulfate, neopelex, sodium cetanesulfonate, cetyl benzenesulfonic acid sodium, gathers
At least one of vinylpyrrolidone, polyvinyl alcohol, 1-Methyl-2-Pyrrolidone, citrate and sodium ethylene diamine tetracetate.
7. the preparation method of high carrying capacity noble metal carbon nanocatalyst according to claim 1, which is characterized in that the work
Property carbon be VXC-72, VXC-72R, BP2000, EC-300, EC-600, ordered mesopore carbon, carbon nano-fiber and carbon nanotube in
It is at least one.
8. the preparation method of high carrying capacity noble metal carbon nanocatalyst according to claim 1, which is characterized in that step 3
Obtained in the high carrying capacity noble metal carbon nanocatalyst, the mass ratio of noble metal and carbon is 40%~90%.
9. the preparation method of high carrying capacity noble metal carbon nanocatalyst according to claim 1, which is characterized in that in step
It in 2, is added after surfactant, carries out ultrasonic disperse 30min~60min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110624604A (en) * | 2019-08-30 | 2019-12-31 | 厦门大学 | Modified palladium-carbon catalyst, preparation method and application thereof |
| CN113594483A (en) * | 2021-07-28 | 2021-11-02 | 宁波中科科创新能源科技有限公司 | Preparation method of PtCo intermetallic compound catalyst and fuel cell |
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| CN101318131A (en) * | 2008-02-04 | 2008-12-10 | 中国科学院长春应用化学研究所 | Preparation method for direct methanoic acid fuel cell palladium-on-carbon nano-catalyst |
| US20120308912A1 (en) * | 2011-06-02 | 2012-12-06 | Hong Suk-Gi | Catalyst slurry, electrode prepared by using the catalyst slurry, and fuel cell including the electrode |
| CN104815651A (en) * | 2015-04-21 | 2015-08-05 | 南京邮电大学 | Preparation method of precious metal/titanium dioxide nano composite |
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| CN101007272A (en) * | 2006-12-01 | 2007-08-01 | 中国科学院上海微系统与信息技术研究所 | Preparation method of platinum nanoparticle electrocatalyst based on metal cluster approach |
| CN101318131A (en) * | 2008-02-04 | 2008-12-10 | 中国科学院长春应用化学研究所 | Preparation method for direct methanoic acid fuel cell palladium-on-carbon nano-catalyst |
| US20120308912A1 (en) * | 2011-06-02 | 2012-12-06 | Hong Suk-Gi | Catalyst slurry, electrode prepared by using the catalyst slurry, and fuel cell including the electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110624604A (en) * | 2019-08-30 | 2019-12-31 | 厦门大学 | Modified palladium-carbon catalyst, preparation method and application thereof |
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| CN113594483A (en) * | 2021-07-28 | 2021-11-02 | 宁波中科科创新能源科技有限公司 | Preparation method of PtCo intermetallic compound catalyst and fuel cell |
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