CN109244488A - A kind of carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst and preparation method - Google Patents
A kind of carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst and preparation method Download PDFInfo
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- CN109244488A CN109244488A CN201811028249.8A CN201811028249A CN109244488A CN 109244488 A CN109244488 A CN 109244488A CN 201811028249 A CN201811028249 A CN 201811028249A CN 109244488 A CN109244488 A CN 109244488A
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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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- 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
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
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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
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
- H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
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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
Abstract
The invention discloses a kind of preparation methods of carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst.It uses tetramethylol chloride for reducing agent, restores silver nitrate under alkaline condition.For the size of nano silver between 1~6 nm, average-size is 2.9 nm, is uniformly distributed in multi-wall carbon nano-tube pipe surface.Under lower silver load capacity, carbon multi-wall nano tube loaded nano-silver catalyst also can restore oxygen by four electronic processes, have preferable oxygen reduction catalytic activity and stability, and methanol tolerant toxicity is more than commercial platinum/C catalyst.
Description
Technical field
The present invention relates to a kind of carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst and preparation methods.
Background technique
The chemical energy of fuel molecule is converted electric energy by fuel cell, it is considered to be a kind of effective substitution conventional mineral combustion
The energy storage device of material.Direct methanol fuel cell (DMFCs) is a subclass of proton exchange fuel cell, is fired using methanol
Material, it is produced electricl energy by the oxidation of methanol and the reduction of oxygen.Cathodic oxygen reduction is a master for restricting DMFCs performance
Bottleneck is wanted, slow dynamics promotes the research of high activated catalyst.(Chem.Soc.Rev.2015,44,2168-2201) platinum
(Pt) it is the best catalyst of oxygen reduction reaction (ORR), and has been commercialized, and high cost, natural scarcity, durability and resistance to
Methanol toxicity difference is the major obstacle of the large-scale application in DMFCs.(Chem.Rev.2016,116,3594-3657) is current
Research is dedicated to exploring substitute of abundant, cheap, the stable catalyst as Pt, including low platinum (Pt alloy)
(Appl.Catal.B.2015,162,593-601) and non-Pt material (non-Pt noble metal, base metal and the doped carbon without metal
Material).(ChemElectroChem.2018,5,1073-1079,J.Mater.Chem.A 2014,2,10146–10153,
Chem.Mater.2016,28,1737–1745.)
In various elctro-catalysts, silver-colored (Ag) because of its acceptable ORR catalytic activity, durability, high abundance and low cost,
It can apply on a large scale, be considered being hopeful to replace Pt.(Electrochimica Acta 2015,174,919-924) however,
The catalytic performance of silver is still below Pt, and average electron transfer number (n) of ORR is in 2 (2e, oxygen reduction generate hydrogen peroxide) and 4
Between (4e, oxygen reduction generate water), make the efficiency of ORR far below theoretical value, and the production of hydrogen peroxide is to the length of DMFCs film
Phase stability is harmful.(J.Power Sources 2012,197,107–110.).
Reducing granular size helps to enhance specific surface area and active site, helps to improve ORR catalytic activity.However,
Due to high surface energy, Ag particle is often grown up, and is difficult to obtain finely dispersed small size Ag.(Electrochimica
Acta 2014,135,168-174.) in most of documents, the Ag particle greater than 10 nanometers is generally yielded, some are even up to
Hundreds of nanometers.End-capping reagent is considered as reducing nanoparticle size most efficient method, can be effectively formed scattered small ruler
Very little Ag.Although some researchs think that end-capping reagent prevents mass transfer and electronics transfer on the surface of the catalyst, there are also grind
Study carefully proof, the catalyst with end-capping reagent still can show brilliant catalytic activity.
The present invention is reducing agent using tetrahydroxy phosphorus chloride, restores silver nitrate under alkaline condition.And tetrahydroxy in reacting
The oxidation product trihydroxy phosphorous oxide of phosphorus chloride makes nano silver with the average-size of 2.9nm in multi-wall carbon nano-tube as end-capping reagent
It is uniformly distributed on pipe.Obtained Ag/MWNTs also has high catalytic activity in the lower situation of Ag load capacity, while also having
The methanol tolerant toxicity of high stability and super business Pt/C catalyst.
Summary of the invention
The purpose of the present invention is preferable to seek a kind of catalytic activity and stability, methanol tolerant toxicity ability is stronger, cost
Lower oxygen reduction catalyst replaces commercial platinum catalyst, provides a kind of carbon multi-wall nano tube loaded nano silver hydrogen reduction and urges
Agent and preparation method.
Carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst of the present invention, nano silver having a size of 1~6nm,
Average-size is 2.9nm；Nano silver is uniformly distributed on the carbon nanotubes, the load capacity of nano silver be mass percent 10~
40%；In carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst preparation, reducing agent is tetramethylol chloride；End-capping reagent is
The oxidation product trihydroxy phosphorous oxide of tetramethylol chloride.
The specific steps of carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst preparation are as follows:
(1) 1000mg multi-walled carbon nanotube is placed in Suction filtration device and carries out surface oxidation treatment, filtered at 0.01MPa
Negative pressure is formed after ten minutes, and the H that 100mL mass percentage concentration is 30%~35% is added2O2Stirring is stood overnight again after 2 hours,
It is 5 hours dry at 80 DEG C after centrifuge washing.
(2) 35~75mg step (1) resultant multi-wall carbon nanotube is molten for the silver nitrate of 1~3mmol/L with 100mL concentration
Liquid is uniformly mixed by ultrasound and magnetic agitation.
(3) using concentration for the pH of mixture obtained by the potassium hydroxide regulating step (2) of 1.0mol/L is 11~13.
(4) in the alkaline mixed solution obtained by step (3), the tetra methylol chlorination that 5mL concentration is 30~60mmol/L is added
Phosphorus solution restores silver nitrate, after being stirred to react 2 hours, the reduzate trihydroxy oxidation of tetramethylol chloride in reaction process
Phosphorus becomes the end-capping reagent of nano silver, stands overnight.
(5) using reaction product obtained by centrifugation deionized water cleaning step (4), until supernatant is in neutrality, it will
It is 5 hours dry at 80 DEG C after solid resultant product collection, obtain multi-walled carbon nanotube loading nano silvery oxygen reduction catalyst.
Preparation method of the present invention is simple, at low cost, can apply in direct methanol fuel cell in Cathodic oxygen reduction；
There is the carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst of preparation nano silver to be uniformly distributed on multi-walled carbon nanotubes,
And the lesser feature of nano silver size, the oxygen reduction catalytic activity of nano silver can be improved；And nanometer silver surface have end-capping reagent into
Row protection, can improve the stability in long-time catalytic process of nano silver.Carbon multi-wall nano tube loaded nanometer of the invention
Silver catalyst has preferable oxygen reduction catalytic activity, stability and methanol tolerant toxicity.
Detailed description of the invention
Fig. 1 is the TEM photo of the carbon nanotube loaded nano silver oxygen reduction catalyst of embodiment according to the present invention 1.
Fig. 2 is the size of the nano silver of according to embodiments of the present invention 1 carbon nanotube loaded nano silver oxygen reduction catalyst
Distribution.
Fig. 3 is the XRD diagram of the carbon nanotube loaded nano silver oxygen reduction catalyst of embodiment according to the present invention 1.
Fig. 4 is the XPS figure of the carbon nanotube loaded nano silver oxygen reduction catalyst of the embodiment of the present invention 1.
Fig. 5 is the TG figure of the carbon nanotube loaded nano silver oxygen reduction catalyst of the embodiment of the present invention 1.
Fig. 6 is the rotating disk electrode (r.d.e) polarization of the carbon nanotube loaded nano silver oxygen reduction catalyst of the embodiment of the present invention 1
Curve.
Fig. 7 is the electronics of the oxygen reduction reaction of the carbon nanotube loaded nano silver oxygen reduction catalyst of the embodiment of the present invention 2
Transmit number and hydrogen peroxide yield.
Fig. 8 is the cyclical stability figure of the carbon nanotube loaded nano silver oxygen reduction catalyst of the embodiment of the present invention 3.
Fig. 9 is the carbon nanotube loaded nano silver oxygen reduction catalyst of the embodiment of the present invention 4 and the perseverance of commercial platinum catalyst
Voltage curve comparison diagram.
Specific embodiment
The present invention can be realized by many different forms, should not be construed as limited to illustrate here specific
Embodiment.These embodiments is provided it is the shape in order to explain carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst of the invention
Looks, structure and practical application to make others skilled in the art it will be appreciated that various implementation conditions of the invention, and add
Rationally to apply.
Embodiment 1:
(1) 1000mg multi-walled carbon nanotube is placed in Suction filtration device and carries out surface oxidation treatment, filtered at 0.01MPa
Negative pressure is formed after ten minutes, and the H that 100mL mass percentage concentration is 35% is added2O2Stirring is stood overnight again after 2 hours, and centrifugation is washed
It is 5 hours dry at 80 DEG C after washing.
(2) 50mg step (1) resultant multi-wall carbon nanotube is passed through with 100mL concentration for the silver nitrate solution of 2mmol/L
Ultrasound and magnetic agitation uniformly mix.
(3) using concentration for the pH of mixture obtained by the potassium hydroxide regulating step (2) of 1.0mol/L is 12.
(4) in the alkaline mixed solution obtained by step (3), it is molten that the tetramethylol chloride that 5mL concentration is 50mmol/L is added
Liquid restore silver nitrate, after being stirred to react 2 hours, in reaction process the reduzate trihydroxy phosphorous oxide of tetramethylol chloride at
For the end-capping reagent of nano silver, stand overnight.
(5) using reaction product obtained by centrifugation deionized water cleaning step (4), until supernatant is in neutrality, it will
It is 5 hours dry at 80 DEG C after solid resultant product collection, obtain multi-walled carbon nanotube loading nano silvery oxygen reduction catalyst.
Obtained carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst, using tetramethylol chloride as reducing agent,
Silver nitrate is restored under alkaline condition, and oxidation product trihydroxy phosphorous oxide is evenly distributed on nano silver more as end-capping reagent
On wall carbon nano tube, size is between 1nm~6nm, average-size 2.9nm, and nano-silver loaded amount is 10 in mass percent
Between~40%.
Transmission electron microscope is carried out (referred to as to obtained carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst
TEM), x-ray diffractometer (abbreviation XRD), x-ray photoelectron spectroscopy are characterized.Test result difference is as Figure 1-Figure 4.
It will be seen from figure 1 that nano silver is uniformly distributed on multi-walled carbon nanotubes.Figure it is seen that the size of nano silver is mainly divided
Cloth is between 1nm~6nm, average-size 2.9nm.Fig. 3 is the XRD diagram of carbon multi-wall nano tube loaded nano silver, it may be determined that is received
The presence of meter Yin, and based on its (111) crystal face with high oxygen reduction activity.Fig. 4 be catalyst P 2p XPS scheme, wherein P with
Tri- kinds of forms of Ag-P, P=O and P-C exist, and the ratio of three's content is 1:1:3, and trihydroxy phosphorous oxide is bonded with Ag, plays
It prevents nano silver reunion and improves the effect of its stability.
Fig. 5 is the TG figure for the carbon multi-wall nano tube loaded nano-silver catalyst that the present embodiment obtains, oxygen at high temperature
In atmosphere, Ag becomes Ag completely2O accounts for about mass percent 17.9%, and the load capacity for obtaining Ag finally is mass percent
16.6%.Fig. 6 is the rotating disk electrode (r.d.e) polarization curve for the carbon multi-wall nano tube loaded nano-silver catalyst that the present embodiment obtains,
Its half wave potential is -0.26V, negative compared with 20%Pt/C (- 0.12V), but its limiting current density is suitable in 20%Pt/C.
Embodiment 2:
(1) 1000mg multi-walled carbon nanotube is placed in Suction filtration device and carries out surface oxidation treatment, filtered at 0.01MPa
Negative pressure is formed after ten minutes, and the H that 100mL mass percentage concentration is 30% is added2O2Stirring is stood overnight again after 2 hours, and centrifugation is washed
It is 5 hours dry at 80 DEG C after washing.
(2) silver nitrate solution that 45mg step (1) resultant multi-wall carbon nanotube and 100mL concentration are 2.5mmol/L is led to
It crosses ultrasound and magnetic agitation uniformly mixes.
(3) using concentration for the pH of mixture obtained by the potassium hydroxide regulating step (2) of 1.0mol/L is 11.
(4) in the alkaline mixed solution obtained by step (3), it is molten that the tetramethylol chloride that 5mL concentration is 40mmol/L is added
Liquid restore silver nitrate, after being stirred to react 2 hours, in reaction process the reduzate trihydroxy phosphorous oxide of tetramethylol chloride at
For the end-capping reagent of nano silver, stand overnight.
(5) using reaction product obtained by centrifugation deionized water cleaning step (4), until supernatant is in neutrality, it will
It is 5 hours dry at 80 DEG C after solid resultant product collection, obtain multi-walled carbon nanotube loading nano silvery oxygen reduction catalyst.
Obtained carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst, using tetramethylol chloride as reducing agent,
Silver nitrate is restored under alkaline condition, and oxidation product trihydroxy phosphorous oxide is evenly distributed on nano silver more as end-capping reagent
On wall carbon nano tube, size is between 1nm~6nm, average-size 2.9nm, and nano-silver loaded amount is 10 in mass percent
Between~40%.
Fig. 7 shows the electronics of the carbon multi-wall nano tube loaded nano silver catalytic oxidation-reduction reaction process obtained with the present embodiment
Number and hydrogen peroxide yield are transmitted, from -0.2V to -0.6V, the hydrogen reduction process of carbon multi-wall nano tube loaded nano silver catalysis is then in
Reveal 4 electronic processes, hydrogen peroxide yield is close to 0.
Embodiment 3:
(1) 1000mg multi-walled carbon nanotube is placed in Suction filtration device and carries out surface oxidation treatment, filtered at 0.01MPa
Negative pressure is formed after ten minutes, and the H that 100mL mass percentage concentration is 30% is added2O2Stirring is stood overnight again after 2 hours, and centrifugation is washed
It is 5 hours dry at 80 DEG C after washing.
(2) 55mg step (1) resultant multi-wall carbon nanotube is passed through with 100mL concentration for the silver nitrate solution of 2mmol/L
Ultrasound and magnetic agitation uniformly mix.
(3) using concentration for the pH of mixture obtained by the potassium hydroxide regulating step (2) of 1.0mol/L is 13.
(4) in the alkaline mixed solution obtained by step (3), it is molten that the tetramethylol chloride that 5mL concentration is 50mmol/L is added
Liquid restore silver nitrate, after being stirred to react 2 hours, in reaction process the reduzate trihydroxy phosphorous oxide of tetramethylol chloride at
For the end-capping reagent of nano silver, stand overnight.
(5) using reaction product obtained by centrifugation deionized water cleaning step (4), until supernatant is in neutrality, it will
It is 5 hours dry at 80 DEG C after solid resultant product collection, obtain multi-walled carbon nanotube loading nano silvery oxygen reduction catalyst.
Obtained carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst, using tetramethylol chloride as reducing agent,
Silver nitrate is restored under alkaline condition, and oxidation product trihydroxy phosphorous oxide is evenly distributed on nano silver more as end-capping reagent
On wall carbon nano tube, size is between 1nm~6nm, average-size 2.9nm, and nano-silver loaded amount is 10 in mass percent
Between~40%.
Fig. 8 shows carbon multi-wall nano tube loaded nano silver manufactured in the present embodiment oxygen reduction catalytic activity in multiple circulation
Variation.After circulation 3000 times, the half wave potential of rotating disk electrode (r.d.e) polarization curve shuffles 3mV, and carrying current is slightly decreased,
It can be seen that carbon multi-wall nano tube loaded nano-silver catalyst has preferable stability.
Embodiment 4:
(1) 1000mg multi-walled carbon nanotube is placed in Suction filtration device and carries out surface oxidation treatment, filtered at 0.01MPa
Negative pressure is formed after ten minutes, and the H that 100mL mass percentage concentration is 35% is added2O2Stirring is stood overnight again after 2 hours, and centrifugation is washed
It is 5 hours dry at 80 DEG C after washing.
(2) 35mg step (1) resultant multi-wall carbon nanotube is passed through with 100mL concentration for the silver nitrate solution of 1mmol/L
Ultrasound and magnetic agitation uniformly mix.
(3) using concentration for the pH of mixture obtained by the potassium hydroxide regulating step (2) of 1.0mol/L is 12.
(4) in the alkaline mixed solution obtained by step (3), it is molten that the tetramethylol chloride that 5mL concentration is 60mmol/L is added
Liquid restore silver nitrate, after being stirred to react 2 hours, in reaction process the reduzate trihydroxy phosphorous oxide of tetramethylol chloride at
For the end-capping reagent of nano silver, stand overnight.
(5) using reaction product obtained by centrifugation deionized water cleaning step (4), until supernatant is in neutrality, it will
It is 5 hours dry at 80 DEG C after solid resultant product collection, obtain multi-walled carbon nanotube loading nano silvery oxygen reduction catalyst.
Obtained carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst, using tetramethylol chloride as reducing agent,
Silver nitrate is restored under alkaline condition, and oxidation product trihydroxy phosphorous oxide is evenly distributed on nano silver more as end-capping reagent
On wall carbon nano tube, size is between 1nm~6nm, average-size 2.9nm, and nano-silver loaded amount is 10 in mass percent
Between~40%.
Fig. 9 is the methanol tolerant toxicity energy of carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst manufactured in the present embodiment
Power.After methanol is added, the hydrogen reduction electric current of carbon multi-wall nano tube loaded nano silver is basically unchanged, and the electric current of commercial platinum catalyst
Sharply decline.It can be seen that the more commercial platinum catalyst of methanol tolerant toxicity ability of carbon multi-wall nano tube loaded nano silver is strong.
Claims (2)
1. a kind of carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst, it is characterised in that carbon multi-wall nano tube loaded nano silver
Oxygen reduction catalyst, for nano silver having a size of 1~6 nm, average-size is 2.9 nm；Nano silver is evenly distributed on carbon nanotube
On, the load capacity of nano silver is mass percent 10~40%.
2. the preparation method of carbon multi-wall nano tube loaded nano silver oxygen reduction catalyst according to claim 1, special
Sign is specific steps are as follows:
(1) 1000 mg multi-walled carbon nanotubes are placed in Suction filtration device and carry out surface oxidation treatment, filter 10 at 0.01 MPa
Negative pressure is formed after minute, and the H that 100 mL mass percentage concentrations are 30%~35% is added2O2Stirring is stood overnight again after 2 hours, from
It is 5 hours dry at 80 DEG C after heart washing；
(2) 35~75 mg step (1) resultant multi-wall carbon nanotubes are molten for the silver nitrate of 1~3 mmol/L with 100 mL concentration
Liquid is uniformly mixed by ultrasound and magnetic agitation；
(3) using concentration for the pH of mixture obtained by the potassium hydroxide regulating step (2) of 1.0 mol/L is 11~13；
(4) in the alkaline mixed solution obtained by step (3), it is molten that the tetramethylol chloride that 5mL concentration is 30~60 mmol/L is added
Liquid restores silver nitrate, after being stirred to react 2 hours, the reduzate trihydroxy phosphorous oxide of tetramethylol chloride in reaction process
As the end-capping reagent of nano silver, stand overnight；
(5) using reaction product obtained by centrifugation deionized water cleaning step (4), until supernatant is in neutrality, by solid
It is 5 hours dry at 80 DEG C after collection of products, obtain multi-walled carbon nanotube loading nano silvery oxygen reduction catalyst.
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| CN111408369A (en) * | 2020-04-16 | 2020-07-14 | 桂林理工大学 | Nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst and preparation method thereof |
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| CN111408369A (en) * | 2020-04-16 | 2020-07-14 | 桂林理工大学 | Nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst and preparation method thereof |
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Application publication date: 20190118 |