CN109037710A - A kind of preparation method of zinc and air cell catalyst and its application in catalysis ORR, OER and HER reaction - Google Patents
A kind of preparation method of zinc and air cell catalyst and its application in catalysis ORR, OER and HER reaction Download PDFInfo
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- CN109037710A CN109037710A CN201810716792.0A CN201810716792A CN109037710A CN 109037710 A CN109037710 A CN 109037710A CN 201810716792 A CN201810716792 A CN 201810716792A CN 109037710 A CN109037710 A CN 109037710A
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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
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
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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
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/08—Hybrid cells; Manufacture thereof composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
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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
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a kind of preparation method of zinc and air cell catalyst and its applications in catalysis ORR, OER and HER reaction, belong to zinc and air cell catalyst technical field.Technical solution of the present invention main points are as follows: fold fine structure directed agents are introduced on presoma MOF, element sulphur and P elements are introduced while so that its surface is formed fold fine nanometer package assembly, it introduces nickel source dopant and magnesium source doping agent respectively again, synthesizes zinc and air cell catalyst at normal temperature.Zinc and air cell catalyst prepared by the present invention is with the fine package assembly of surface folding and has hollow structure feature, increase specific surface area, therefore the contact area of catalyst and electrolyte is increased, improve its electrocatalysis characteristic, the introducing of element sulphur and P elements increases effective catalytic active center and improves the delocalized of carbon atom charge, therefore improves the catalytic activity of catalyst.
Description
Technical field
The invention belongs to zinc and air cell catalyst technical fields, and in particular to a kind of preparation method of zinc and air cell catalyst
And its application in catalysis ORR, OER and HER reaction.
Background technique
Since current environmental pollution, energy crisis are got worse, the exploitation of new energy is extremely urgent.New energy conversion
Device such as zinc and air cell has many advantages, such as that environmental-friendly, energy conversion efficiency is high, has experimental application in many fields, more next
More get more and more people's extensive concerning.Furthermore zinc and air cell is small in size, charge capacity is big, quality is small, can be in wide temperature range
It is interior to work normally, is corrosion-free and safe and reliable.For the lithium ion battery of closed system, since zinc and air cell is
Semi-open system provides oxygen with the air in environment, increases energy density while reducing air electrode volume.Cause
This, zinc and air cell has extraordinary application prospect.
In zinc and air cell, the key factor for restricting its development is electrode catalyst agent material, and catalyst is zinc and air cell
Core component, and determine the critical material of battery cost and performance.Common catalyst has noble metal catalyst and non-
Noble metal catalyst, but noble metal reserves are few, it is expensive；And individually base metal is difficult to play intrinsic catalysis work
Property.Therefore, develop the catalyst that a kind of price is low, performance is high be have in zinc and air cell catalyst synthesis technology field it is to be solved
One of major issue.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of preparation method of zinc and air cell catalyst, made from this method
Catalyst can be used in ORR, OER and HER reaction for being catalyzed zinc and air cell, effectively increase the chemical property of zinc and air cell.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of preparation side of zinc and air cell catalyst
Method, it is characterised in that detailed process are as follows: introduce fold fine structure directed agents on presoma MOF, its surface is made to form fold
Element sulphur and P elements are introduced while fine nanometer package assembly, then introduce nickel source dopant and magnesium source doping agent respectively,
Zinc and air cell catalyst is synthesized under room temperature, wherein presoma MOF is ZIF-67, and fold fine structure directed agents are thio-alcohol chemical combination
Object and triphenyl phosphorus, the sulfur alcohol compound are 2-mercaptobenzothiazole or 2-mercaptobenzimidazole, and nickel source dopant is nitric acid
Nickel, magnesium source doping agent are magnesium nitrate.
Further preferably, the preparation method of the zinc and air cell catalyst, it is characterised in that specific steps are as follows:
Step S1: 249mg cobalt nitrate and 328mg 2-methylimidazole are added in 50mL methanol and are uniformly mixed, room temperature
For 24 hours, with ethyl alcohol centrifuge washing, vacuum drying obtains presoma MOF to lower standing afterwards for several times；
Step S2: presoma MOF and fold fine structure directed agents that step S1 is obtained are added in ethyl alcohol and pass through water-bath
90 DEG C of 6 ~ 8h of reaction are heated to, repeatedly vacuum drying obtains surface with the fine nanometer assembling knot of fold afterwards with ethyl alcohol centrifuge washing
The purple sample of structure；
Step S3: there is the purple sample of the fine nanometer package assembly of fold and nickel source dopant to add the surface that step S2 is obtained
Enter into ethyl alcohol and stir under room temperature 6 ~ 8h, repeatedly vacuum drying obtains having the shallow of hollow structure afterwards with ethyl alcohol centrifuge washing
Green sample；
Step S4: by the obtained light green color sample with hollow structure of step S3 and magnesium source doping agent be added in ethyl alcohol and in
6 ~ 8h is stirred under room temperature, repeatedly vacuum drying obtains hollow and surface with the fine nanometer assembling of fold afterwards with ethyl alcohol centrifuge washing
The dodecahedron shape zinc and air cell catalyst of structure, the average grain diameter of the catalyst are 500nm, and shell thickness is 15 ~ 20nm.
Further preferably, presoma MOF described in step S2 and fold fine structure directed agents sulfur alcohol compound and three
The mass ratio of phenyl phosphorus is 2.5:2:1；Surface described in step S3 have the fine nanometer package assembly of fold purple sample with
The mass ratio of nickel source dopant is 3:1；The mass ratio of magnesium source doping agent described in step S4 and nickel source dopant is 2.5:1.
Application of the zinc and air cell catalyst of the present invention in catalysis zinc and air cell ORR, OER and HER reaction, catalysis
The fine nanometer package assembly of the fold on agent surface increases the specific surface area of catalyst, and then increases catalyst and electrolyte
Contact area makes catalyst fully play its activity, and element sulphur and being introduced into for P elements increase in effective catalytic activity
The heart and improve the delocalized of carbon atom charge, improve the catalytic activity of catalyst, in catalyst simultaneously containing W metal, Co and
Mg has simultaneously effectively played the synergistic effect between them, has good ORR, OER and HER catalytic activity.
Compared with the prior art, the present invention has the following advantages:
1, the present invention successfully synthesizes a kind of using MOF as the zinc and air cell bifunctional electrocatalyst of presoma, sulfur alcohol compound
The ligand that addition with triphenyl phosphorus keeps it original with presoma MOF forms Competition, changes the surface presoma MOF office
The coordination environment in portion, so that synthesized sample surfaces form the fine nanometer package assembly of fold, which increase catalysis
The specific surface area of agent increases its contact area with electrolyte, to improve the electrocatalysis characteristic of catalyst, while sulphur member
The introducing of element and P elements increases effective catalytic active center and improves the delocalized of carbon atom charge, therefore improves and urge
The catalytic activity of agent.
2, the introducing of nickel source dopant is acted on by its stronger and ligand, can generate corrasion to make to be catalyzed
Agent forms hollow structure, this also effectively increases the specific surface area of material, increases the contact area with electrolyte, improves
The electrocatalysis characteristic of catalyst.
3, the specific adding manner and ratio of magnesium makes it on this basis instead of the nickel and cobalt of part in catalyst
It obtains and has preferably played synergistic effect between each metal component, the dispersibility of catalyst is improved, to improve catalyst
Catalytic activity.
Detailed description of the invention
Fig. 1 is the SEM figure that catalyst is made in embodiment 1；
Fig. 2 is the SEM figure that catalyst is made in comparative example 1；
Fig. 3 is the SEM figure that catalyst is made in comparative example 2；
Fig. 4 is the ORR polarization curve of embodiment 1, embodiment 2 and comparative example 1, catalyst obtained by comparative example 2 and comparative example 3；
Fig. 5 is the OER polarization curve of embodiment 1, embodiment 2 and comparative example 1, catalyst obtained by comparative example 2 and comparative example 3；
Fig. 6 is the HER polarization curve of embodiment 1, embodiment 2 and comparative example 1, catalyst obtained by comparative example 2 and comparative example 3.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Electro-chemical test uses three electrode body of Solartron 1287(Solartron Analytical, England) type
The half-cell of system carries out.To be coated with the glass-carbon electrode of catalyst as working electrode, wherein catalyst be embodiment 1, comparative example 1,
Final catalyst obtained by comparative example 2 and comparative example 3, is respectively 1cm to electrode and reference electrode2Platinized platinum and Ag/AgCl
Saturated calomel electrode, electrolyte are 0.1M KOH aqueous solution.To keep catalyst well attached on glass-carbon electrode, secondary water is used
Cleaning glass-carbon electrode is simultaneously dried at room temperature for.The preparation step of thin layer catalyst is as follows on electrode: 5mg catalyst being taken to add 0.5mL
Perfluorinated sulfonic acid (PFSA) solution that ethyl alcohol and 50 μ L mass concentrations are 5%, ultrasonic disperse about 30min take 15 μ L with microsyringe
It is coated on bright and clean glass-carbon electrode, can be tested after being dried at room temperature for, electric performance test through the uniform suspension of ultrasonic disperse
As a result as shown in Figure 4, Figure 5 and Figure 6.
Embodiment 1
Step S1: 249mg cobalt nitrate and 328mg 2-methylimidazole are added in 50mL methanol and are uniformly mixed, room temperature
For 24 hours, with ethyl alcohol centrifuge washing, vacuum drying obtains presoma MOF to lower standing afterwards for several times；
Step S2: by obtained presoma MOF, 25mg 2-mercaptobenzothiazole of 37.5mg step S1 and 12.5mg triphenyl phosphorus
It is added in 40mL ethyl alcohol and passes through heating water bath to 90 DEG C of reaction 7h, repeatedly vacuum drying obtains table afterwards with ethyl alcohol centrifuge washing
Face has the purple sample of the fine nanometer package assembly of fold；
Step S3: the surface that 90mg step S2 is obtained has the purple sample and 30mg nickel source of the fine nanometer package assembly of fold
Dopant nickel nitrate is added in 40mL ethyl alcohol and stirs 7h under room temperature, and with ethyl alcohol centrifuge washing, repeatedly vacuum drying is obtained afterwards
Light green color sample with hollow structure；
Step S4: the obtained light green color sample with hollow structure of step S3 and 75mg magnesium source doping agent magnesium nitrate are added to
7h is stirred in 40mL ethyl alcohol and under room temperature, repeatedly vacuum drying obtains hollow and surface with fold afterwards with ethyl alcohol centrifuge washing
The dodecahedron shape zinc and air cell catalyst of fine nanometer package assembly, the average grain diameter of the catalyst are 500nm, shell thickness
For 15 ~ 20nm, as shown in Figure 1.
Comparative example 1
Step S1: 249mg cobalt nitrate and 328mg 2-methylimidazole are added in 50mL methanol and are uniformly mixed, room temperature
For 24 hours, with ethyl alcohol centrifuge washing, vacuum drying obtains presoma MOF to lower standing afterwards for several times；
Step S2: by obtained presoma MOF, 25mg 2-mercaptobenzothiazole of 37.5mg step S1 and 12.5mg triphenyl phosphorus
It is added in 40mL ethyl alcohol and passes through heating water bath to 90 DEG C of reaction 7h, repeatedly vacuum drying obtains table afterwards with ethyl alcohol centrifuge washing
Face has the purple sample of the fine nanometer package assembly of fold；
Step S3: the surface that 90mg step S2 is obtained has purple sample and the 75mg magnesium source of the fine nanometer package assembly of fold
Dopant magnesium nitrate is added in 40mL ethyl alcohol and stirs 7h under room temperature, and with ethyl alcohol centrifuge washing, repeatedly vacuum drying is obtained afterwards
Surface has the solid dodecahedron shape final catalyst of fine nanometer package assembly, as shown in Figure 2.
Comparative example 2
Step S1: 249mg cobalt nitrate and 328mg 2-methylimidazole are added in 50mL methanol and are uniformly mixed, room temperature
For 24 hours, with ethyl alcohol centrifuge washing, vacuum drying obtains presoma MOF to lower standing afterwards for several times；
Step S2: by obtained presoma MOF, 25mg 2-mercaptobenzothiazole of 37.5mg step S1 and 12.5mg triphenyl phosphorus
It is added in 40mL ethyl alcohol and passes through heating water bath to 90 DEG C of reaction 7h, repeatedly vacuum drying obtains table afterwards with ethyl alcohol centrifuge washing
Face has the purple sample of the fine nanometer package assembly of fold；
Step S3: the surface that 90mg step S2 is obtained has the purple sample and 30mg nickel source of the fine nanometer package assembly of fold
Dopant nickel nitrate is added in 40mL ethyl alcohol and stirs 7h under room temperature, and with ethyl alcohol centrifuge washing, repeatedly vacuum drying is obtained afterwards
Final catalyst without magnesium component.
Comparative example 3
Step S1: 249mg cobalt nitrate and 328mg 2-methylimidazole are added in 50mL methanol and are uniformly mixed, room temperature
For 24 hours, with ethyl alcohol centrifuge washing, vacuum drying obtains presoma MOF to lower standing afterwards for several times；
Step S2: presoma MOF and 30mg the nickel source dopant nickel nitrate that 37.5mg step S1 is obtained is added to 40mL ethyl alcohol
In and under room temperature stir 7h, with ethyl alcohol centrifuge washing, repeatedly vacuum drying obtains the light yellow sample with hollow structure afterwards；
Step S3: the light yellow sample with hollow structure that step S2 is obtained is added to magnesium source doping agent magnesium nitrate
Stir 7h in 50mL methanol and under room temperature, with ethyl alcohol centrifuge washing repeatedly afterwards vacuum drying obtain surface it is smooth have 12
The final catalyst of face body structure.
Zinc and air cell catalyst obtained by the present invention has good ORR, OER and HER catalytic activity.From Fig. 4 ~ 6
As can be seen that obtained by comparative example in electric performance test result, with corrugationless fine nanostructur or without nickel source dopant or
The catalyst of no magnesium source doping agent is compared, and catalyst made from embodiment 1 has maximum limiting current density, further relates to this
Catalyst has best ORR, OER and HER catalytic activity；The fine nanometer group of the fold of one side zinc and air cell catalyst surface
Assembling structure increases the specific surface area of catalyst, therefore increases the contact area of catalyst and electrolyte, keeps catalyst abundant
Performance its activity, furthermore the introducing of element sulphur and P elements increases effective catalytic active center and improves carbon atom charge
It is delocalized, thus improve the catalytic activity of catalyst；Contain W metal, Co in another aspect bifunctional electrocatalyst simultaneously
And Mg and the synergistic effect between them is effectively played.The electro catalytic activity performance of zinc and air cell catalyst produced by the present invention
It is excellent, it is a kind of zinc and air cell catalyst with broad prospect of application.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (4)
1. a kind of preparation method of zinc and air cell catalyst, it is characterised in that detailed process are as follows: introduce fold on presoma MOF
Fine structure directed agents introduce element sulphur and P elements, then divide while so that its surface is formed fold fine nanometer package assembly
Not Yin Ru nickel source dopant and magnesium source doping agent, at normal temperature synthesize zinc and air cell catalyst, wherein presoma MOF be ZIF-
67, fold fine structure directed agents are sulfur alcohol compound and triphenyl phosphorus, which is 2-mercaptobenzothiazole
Or 2-mercaptobenzimidazole, nickel source dopant are nickel nitrate, magnesium source doping agent is magnesium nitrate.
2. the preparation method of zinc and air cell catalyst according to claim 1, it is characterised in that specific steps are as follows:
Step S1: 249mg cobalt nitrate and 328mg 2-methylimidazole are added in 50mL methanol and are uniformly mixed, room temperature
For 24 hours, with ethyl alcohol centrifuge washing, vacuum drying obtains presoma MOF to lower standing afterwards for several times；
Step S2: presoma MOF and fold fine structure directed agents that step S1 is obtained are added in ethyl alcohol and pass through water-bath
90 DEG C of 6 ~ 8h of reaction are heated to, repeatedly vacuum drying obtains surface with the fine nanometer assembling knot of fold afterwards with ethyl alcohol centrifuge washing
The purple sample of structure；
Step S3: there is the purple sample of the fine nanometer package assembly of fold and nickel source dopant to add the surface that step S2 is obtained
Enter into ethyl alcohol and stir under room temperature 6 ~ 8h, repeatedly vacuum drying obtains having the shallow of hollow structure afterwards with ethyl alcohol centrifuge washing
Green sample；
Step S4: by the obtained light green color sample with hollow structure of step S3 and magnesium source doping agent be added in ethyl alcohol and in
6 ~ 8h is stirred under room temperature, repeatedly vacuum drying obtains hollow and surface with the fine nanometer assembling of fold afterwards with ethyl alcohol centrifuge washing
The dodecahedron shape zinc and air cell catalyst of structure, the average grain diameter of the catalyst are 500nm, and shell thickness is 15 ~ 20nm.
3. the preparation method of zinc and air cell catalyst according to claim 2, it is characterised in that: forerunner described in step S2
The mass ratio of body MOF and fold fine structure directed agents sulfur alcohol compound and triphenyl phosphorus is 2.5:2:1；Described in step S3
It is 3:1 that surface, which has the purple sample of the fine nanometer package assembly of fold and the mass ratio of nickel source dopant,；Described in step S4
The mass ratio of the agent of magnesium source doping and nickel source dopant is 2.5:1.
4. zinc and air cell catalyst made from method described in any one of -3 is in catalysis zinc and air cell according to claim 1
Application in ORR, OER and HER reaction, the fine nanometer package assembly of the fold of catalyst surface increase the specific surface of catalyst
Product, and then the contact area of catalyst and electrolyte is increased, so that catalyst is fully played its activity, element sulphur and P elements
Introducing increase effective catalytic active center and improve the delocalized of carbon atom charge, the catalysis for improving catalyst is living
Property, the synergistic effect between them containing W metal, Co and Mg and has effectively been played in catalyst simultaneously, have good ORR,
OER and HER catalytic activity.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110265670A (en) * | 2019-06-10 | 2019-09-20 | 北京化工大学 | A kind of method of Subjective and Objective strategy synthetic nitrogen, the double-doped carbon-based dual purpose catalyst of other hetero atoms |
| CN110586159A (en) * | 2019-09-10 | 2019-12-20 | 辽宁星空钠电电池有限公司 | Method for preparing full-hydrolysis catalyst with nickel monoatomic double-active-site |
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Cited By (2)
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Application publication date: 20181218 |