CN109921040A - The carbon-based elctro-catalyst of a kind of Ni, Fe doping and its preparation and application - Google Patents
The carbon-based elctro-catalyst of a kind of Ni, Fe doping and its preparation and application Download PDFInfo
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- CN109921040A CN109921040A CN201711314202.3A CN201711314202A CN109921040A CN 109921040 A CN109921040 A CN 109921040A CN 201711314202 A CN201711314202 A CN 201711314202A CN 109921040 A CN109921040 A CN 109921040A
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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
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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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 present invention relates to the preparation methods that elctro-catalyst is precipitated in the carbon-based oxygen of a kind of Ni, Fe doping, specifically a kind of Ni, Fe mass content that the transition metal in the elctro-catalyst on unformed mesoporous carbonitride, the catalyst accounts for entire catalyst with the form high dispersive that is coordinated with nitrogen are 5%~60%.By adjusting the type and doping of transition metal, elctro-catalyst is precipitated in the available oxygen with greater activity.This method has the advantages that easy, easy to implement, production cost is low etc..
Description
Technical field
The invention belongs to catalyst and its preparation technical fields, are used for secondary metals air fuel more particularly to one kind
Catalyst and its preparation and application is precipitated in oxygen under battery, electrolyzed alkaline water hydrogen producer and other alkaline conditions.
Background technique
Secondary metals air-fuel battery realizes energy stores by the electrochemical oxidation and reduction reaction of solid metallic, with
Other energy storage technologies, which are compared, has that cheap, energy density is high, safety is good, the advantages such as pollution-free, and helping to solve can be again
The raw energy generates electricity by way of merging two or more grid systems, realizes the important state basic policy of energy-saving and emission-reduction.And how quickly Hydrogen Energy is used as most promising clean energy resource, pass through
Ji ground hydrogen manufacturing is one of current research hotspot.Electrolyzed alkaline water hydrogen producing technology is more mature one of hydrogen producing technology.However mesh
Before, secondary metals air-fuel battery and electrolyzed alkaline water hydrogen producer all suffer from the lower problem of efficiency, need to develop height
Catalyst is imitated to reduce the overpotential of oxygen evolution reaction on oxygen electrode.
Long-term practice and scientific research proves, in alkaline medium, the transition metal elements such as Ni, Fe are to oxygen evolution reaction
Catalytic activity with higher.Oxygen is precipitated elctro-catalyst and with the transition metal hydroxides such as Ni, Fe or oxyhydroxide is at present
It is main, it is largely heavy by coprecipitation (Adv.Energy Mater.2016,1600621) or electrolysis in strong alkali solution
Product prepares (J.Am.Chem.Soc.2014,136,6744).The preparation condition of strong basicity has stronger corrosivity, not to environment
It is friendly；And it is uneven by the catalyst material structure that both the above method prepares, it is easy split-phase
(J.Am.Chem.Soc.2015,137,1305), is unfavorable for being mass produced.In addition to this, transition metal hydroxide or hydroxyl
Base oxide does not have pore structure abundant usually, thus the gas generated in reaction process be easy to be attached to catalyst surface to
Subsequent mass transfer is influenced, the further progress of reaction is unfavorable for.Correlative study person proposes that metal-doped carbon nitride material is one
Kind has promising catalysis material, however research at present is limited in single metal-doped material more, active lower.Divide accordingly
Analysis, the promotion that catalytic performance can be able to achieve by adulterating bimetallic.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of that present invention to provide one kind be applied to secondary metals air-fuel battery,
Catalyst and its preparation and application is precipitated in oxygen under electrolyzed alkaline water hydrogen producer and other alkaline conditions.
To achieve the above object, the present invention is realized using scheme in detail below:
A kind of carbon-based elctro-catalyst of Ni, Fe doping, specifically a kind of Ni, Fe with nitrogen coordination mode high dispersive in
Elctro-catalyst on unformed mesoporous carbonitride, the ratio between amount of Ni, Fe substance is 0:1~1:0 in the catalyst, and transition metal accounts for
The mass content of entire catalyst is 5%~60%.
The preparation method of the carbon-based elctro-catalyst of Ni, Fe doping, including following preparation step:
(1) by the NiCl of certain mass2·6H2O and FeCl3·6H2O is poured into a certain amount of solvent, is stirred at room temperature molten
Solution；
(2) ligand of certain mass is poured into step 1 acquired solution, stirring is evaporated at 80 DEG C；
(3) step 2 gained sample is ground, is roasted at a certain temperature in tube furnace with certain heating rate, roasted
Atmosphere is N2, soaking time is 0.5h~8h after reaching maturing temperature；
(4) catalyst after roasting is taken out, after pickling, washing, drying, it is spare that grinding weighs storage.
Solvent described in step (1) is one or both of water, dehydrated alcohol mixture；NiCl in the solvent2·
6H2O and FeCl3·6H2The amount concentration of the total material of O is 0.2~0.8M；NiCl2·6H2O and FeCl3·6H2The amount of the substance of O
The ratio between be 1:0~0:1.
Ligand described in step (2) is the mixture of one or more of urea, dicyandiamide, melamine；Institute
Stating the ratio between amount of substance of ligand and metal is 1:1~24:1.
Heating rate described in step (3) is 1~10 DEG C/min；Maturing temperature is 400~800 DEG C；Roast soaking time
For 0.5~8h.
Carbonitride is similar to graphited carbonitride (g-C3N4), wherein the atom content of nitrogen is greater than 30%.
The acid of pickling is one of hydrochloric acid, sulfuric acid, nitric acid, oxalic acid or a variety of, and pH is 1 to 3.
The carbon-based elctro-catalyst of Ni, Fe doping is secondary metals air-fuel battery, electrolyzed alkaline water hydrogen producer
And catalyst is precipitated in the oxygen under other alkaline conditions.
Compared with prior art, the carbon-supported catalysts of novel Ni, Fe doping of the present invention have the advantage that
1. the incorporation of double base metal has been obviously improved catalytic performance compared with single metal-doped materials；
2. preparation method is simple, it is conducive to large-scale production；
3. structure is uniform, the regulation to catalytic performance can be realized by modulation tenor and ratio；
4. having pore structure more abundant, be conducive to gas transfer；
5. the catalyst has a wide range of application, can be used as secondary metals air-fuel battery, electrolyzed alkaline water hydrogen producer with
And catalyst is precipitated in the oxygen under other alkaline conditions.
Detailed description of the invention
Fig. 1 is the XRD spectra of the carbon-supported catalysts of Ni, Fe doping prepared according to embodiment 2,8,9,10,11,12.
Fig. 2 is the XPS spectrum figure of the carbon-supported catalysts of Ni, Fe doping prepared according to embodiment 2.
Fig. 3 is that the TEM of the carbon-supported catalysts of Ni, Fe doping prepared according to embodiment 2 schemes.
Fig. 4 is that the carbon-supported catalysts of Ni, Fe doping prepared according to embodiment 2,8,9,10,11,12 are saturated in oxygen
Polarization curve is precipitated in oxygen in 1M KOH electrolyte.
Specific embodiment:
The present invention is described in detail below with reference to embodiment.Certain present invention is not limited in these specific implementations
Example.
Embodiment 1:
Weigh 1mmol NiCl2·6H2O is scattered in 5ml deionized water, ultrasonic disperse 0.5h；It is bis- to add 24mmol
Cyanamide is in above-mentioned solution, and stirring is evaporated at 80 DEG C.After sample is ground.With the heating speed of 1 DEG C/min in tube furnace
After rate rises to 400 DEG C, 0.5h is kept the temperature.It takes out after cooling down with furnace, is repeatedly washed with 1M HCl and deionized water, is dried in vacuo
Target product can be obtained.The ratio between amount of Ni, Fe substance is 1:0 in catalyst, and the total mass fraction of metal is 5%.
Embodiment 2:
Weigh 1.75mmol NiCl2·6H2O and 1.75mmol FeCl3·6H2O is scattered in 5ml deionized water, is surpassed
Sound disperses 0.5h；12mmol dicyandiamide is added in above-mentioned solution, stirring is evaporated at 80 DEG C.After sample is ground.?
After rising to 600 DEG C in tube furnace with the heating rate of 2.5 DEG C/min, 4h is kept the temperature.Taken out after cooling down with furnace, with 1M HCl and go from
Sub- water is repeatedly washed, and target product can be obtained in vacuum drying.The ratio between amount of Ni, Fe substance is 1:1, metal in catalyst
Total mass fraction be 28%.
Embodiment 3:
Weigh 4mmol FeCl3·6H2O is scattered in 5ml ethyl alcohol, ultrasonic disperse 0.5h；Add 4mmol dicyandiamide in
In above-mentioned solution, stirring is evaporated at 80 DEG C.After sample is ground.With the heating rate liter of 2.5 DEG C/min in tube furnace
To after 600 DEG C, 4h is kept the temperature.It takes out after cooling down with furnace, is repeatedly washed with 1M HCl and deionized water, vacuum drying can obtain
To target product.The ratio between amount of Ni, Fe substance is 0:1 in catalyst, and the total mass fraction of metal is 58.9%.
Embodiment 4:
Weigh 1.75mmol NiCl2·6H2O and 1.75mmol FeCl3·6H2O is scattered in 5ml deionized water, is surpassed
Sound disperses 0.5h；24mmol urea is added in above-mentioned solution, stirring is evaporated at 80 DEG C.After sample is ground.In pipe
After rising to 600 DEG C in formula furnace with the heating rate of 10 DEG C/min, 4h is kept the temperature.It is taken out after cooling down with furnace, with 1M HCl and deionization
Water is repeatedly washed, and target product can be obtained in vacuum drying.The ratio between amount of Ni, Fe substance is 1:1 in catalyst, metal
Total mass fraction is 22%.
Embodiment 5:
Weigh 1.75mmol NiCl2·6H2O and 1.75mmol FeCl3·6H2O is scattered in 5ml deionized water, is surpassed
Sound disperses 0.5h；24mmol melamine is added in above-mentioned solution, stirring is evaporated at 80 DEG C.After sample is ground.
After rising to 600 DEG C in tube furnace with the heating rate of 2.5 DEG C/min, 4h is kept the temperature.It takes out after cooling down with furnace, with 1M HCl and goes
Ionized water is repeatedly washed, and target product can be obtained in vacuum drying.The ratio between amount of Ni, Fe substance is 1:1, gold in catalyst
The total mass fraction of category is 11%.
Embodiment 6:
Weigh 1.75mmol NiCl2·6H2O and 1.75mmol FeCl3·6H2O is scattered in 5ml deionized water, is surpassed
Sound disperses 0.5h；12mmol dicyandiamide is added in above-mentioned solution, stirring is evaporated at 80 DEG C.After sample is ground.?
After rising to 800 DEG C in tube furnace with the heating rate of 2.5 DEG C/min, 4h is kept the temperature.Taken out after cooling down with furnace, with 1M HCl and go from
Sub- water is repeatedly washed, and target product can be obtained in vacuum drying.The ratio between amount of Ni, Fe substance is 1:1, metal in catalyst
Total mass fraction be 50%.
Embodiment 7:
Weigh 1.75mmol NiCl2·6H2O and 1.75mmol FeCl3·6H2O is scattered in 5ml deionized water, is surpassed
Sound disperses 0.5h；12mmol dicyandiamide is added in above-mentioned solution, stirring is evaporated at 80 DEG C.After sample is ground.?
After rising to 600 DEG C in tube furnace with the heating rate of 2.5 DEG C/min, 8h is kept the temperature.Taken out after cooling down with furnace, with 1M HCl and go from
Sub- water is repeatedly washed, and target product can be obtained in vacuum drying.The ratio between amount of Ni, Fe substance is 1:1, metal in catalyst
Total mass fraction be 28%.
Embodiment 8:
Weigh 3.5mmol NiCl2·6H2O is scattered in 5ml deionized water, ultrasonic disperse 0.5h；Add 12mmol
Dicyandiamide is in above-mentioned solution, and stirring is evaporated at 80 DEG C.After sample is ground.With the liter of 2.5 DEG C/min in tube furnace
After warm rate rises to 600 DEG C, 4h is kept the temperature.It takes out after cooling down with furnace, is repeatedly washed with 1MHCl and deionized water, vacuum is dry
It is dry that target product can be obtained.The ratio between amount of Ni, Fe substance is 1:0 in catalyst, and the total mass fraction of metal is 28%.
Embodiment 9:
Weigh 0.7mmol NiCl2·6H2O and 2.8mmol FeCl3·6H2O is scattered in 5ml deionized water, ultrasound
Disperse 0.5h；12mmol dicyandiamide is added in above-mentioned solution, stirring is evaporated at 80 DEG C.After sample is ground.In pipe
After rising to 600 DEG C in formula furnace with the heating rate of 2.5 DEG C/min, 4h is kept the temperature.It is taken out after cooling down with furnace, with 1M HCl and deionization
Water is repeatedly washed, and target product can be obtained in vacuum drying.The ratio between amount of Ni, Fe substance is 1:4 in catalyst, metal
Total mass fraction is 28%.
Embodiment 10:
Weigh 1.225mmol NiCl2·6H2O and 2.275mmol FeCl3·6H2O is scattered in 5ml deionized water,
Ultrasonic disperse 0.5h；12mmol dicyandiamide is added in above-mentioned solution, stirring is evaporated at 80 DEG C.After sample is ground.
After rising to 600 DEG C in tube furnace with the heating rate of 2.5 DEG C/min, 4h is kept the temperature.It takes out after cooling down with furnace, with 1M HCl and goes
Ionized water is repeatedly washed, and target product can be obtained in vacuum drying.The ratio between amount of Ni, Fe substance is 1 in catalyst:
1.86, the total mass fraction of metal is 28%.
Embodiment 11:
Weigh 2.8mmol NiCl2·6H2O and 0.7mmol FeCl3·6H2O is scattered in 5ml deionized water, ultrasound
Disperse 0.5h；12mmol dicyandiamide is added in above-mentioned solution, stirring is evaporated at 80 DEG C.After sample is ground.In pipe
After rising to 600 DEG C in formula furnace with the heating rate of 2.5 DEG C/min, 4h is kept the temperature.It is taken out after cooling down with furnace, with 1M HCl and deionization
Water is repeatedly washed, and target product can be obtained in vacuum drying.The ratio between amount of Ni, Fe substance is 4:1 in catalyst, metal
Total mass fraction is 28%.
Embodiment 12:
Weigh 3.5mmol FeCl3·6H2O is scattered in 5ml deionized water, ultrasonic disperse 0.5h；Add 12mmol
Dicyandiamide is in above-mentioned solution, and stirring is evaporated at 80 DEG C.After sample is ground.With the liter of 2.5 DEG C/min in tube furnace
After warm rate rises to 600 DEG C, 4h is kept the temperature.It takes out after cooling down with furnace, is repeatedly washed with 1MHCl and deionized water, vacuum is dry
It is dry that target product can be obtained.The ratio between amount of Ni, Fe substance is 0:1 in catalyst, and the total mass fraction of metal is 28%.
Comparative example 1:
Comparative example is the carbon nitride material for being not incorporated into Ni or Fe.Its preparation process and example 1 be not substantially close to but being added
Metal salt.Catalytic activity is precipitated in resulting materials anaerobic.
Fig. 1 is the XRD spectra of the carbon-supported catalysts of Ni, Fe doping prepared according to embodiment 2,8,9,10,11,12.From
As can be seen that not occurring crystalline state substance in sample in figure.
Fig. 2 is the XPS spectrum figure of the carbon-supported catalysts of Ni, Fe doping prepared according to embodiment 2.It can be seen from the figure that
The base material of sample is carbonitride, and Fe is+trivalent, and Ni is+divalent.
Fig. 3 is that the TEM of the carbon-supported catalysts of Ni, Fe doping prepared according to embodiment 2 schemes.It can be seen from the figure that sample
Occur in product without metal amorphous material, is consistent with XRD result, thus it is speculated that the metal in sample is largely the shape to be coordinated with nitrogen
For formula high dispersive in carbon substrate, structure is uniform.Material has apparent meso-hole structure, facilitates gas transfer.
Fig. 4 is that the carbon-supported catalysts of Ni, Fe doping prepared according to embodiment 2,8,9,10,11,12 are saturated in oxygen
Polarization curve is precipitated in oxygen in 1M KOH electrolyte.From figure it can be found that by modulation Ni, Fe ratio, may be implemented to urging
Change the regulation of performance, wherein best proportion is in 1:1 or so.
Claims (10)
1. elctro-catalyst is precipitated in a kind of carbon-based oxygen of Ni, Fe doping, it is characterised in that: Ni and/or Fe is high in the form being coordinated with N
Being scattered in total metal mass score on unformed carbon nitride material is 5%~60%；The carbonitride is g-C3N4, wherein nitrogen
Atom content is greater than 30%.
2. elctro-catalyst is precipitated in the carbon-based oxygen of Ni, Fe doping as described in claim 1, it is characterised in that: golden in the catalyst
Belong to account for entire catalyst mass content it is more excellent be 20%~40%；The quality that metal accounts for entire catalyst in the catalyst contains
Measuring optimal is 20%~30%.
3. elctro-catalyst is precipitated in the carbon-based oxygen that Ni, Fe as described in claim 1,2 or 3 are adulterated, it is characterised in that: the catalyst
The ratio between amount of substance of middle Ni, Fe is 1:4~4:1；: the more excellent of the amount of the substance of Ni, Fe is 1:1~4 in the catalyst:
1。
4. the preparation method that elctro-catalyst is precipitated in a kind of carbon-based oxygen of the doping of Ni, Fe described in claim 1-3, it is characterised in that:
Including following preparation step,
(1) NiCl is prepared in solvent2·6H2O and/or FeCl3·6H2The salting liquid of O；
(2) ligand containing C and N is added in step (1) resulting solution, stirs and is evaporated at 40-100 DEG C；
(3) will be roasted in inert atmosphere after the grinding of sample obtained by step (2), up to maturing temperature after soaking time be 0.5h~
8h；
(4) after successively carrying out pickling, washing, drying to the sample after roasting, electro-catalysis is precipitated in the carbon-based oxygen for obtaining Ni, Fe doping
Agent.
5. the preparation method that elctro-catalyst is precipitated in the carbon-based oxygen of Ni, Fe doping as claimed in claim 4, it is characterised in that: step
(1) solvent described in is one or both of water, dehydrated alcohol mixture；The amount concentration of metal total material is in the solvent
0.2~0.8M.
6. the preparation method that elctro-catalyst is precipitated in the carbon-based oxygen of Ni, Fe doping as claimed in claim 4, it is characterised in that: step
(2) ligand described in is the mixture of one or more of urea, dicyandiamide, melamine；The ligand of the addition
The ratio between amount of substance belonged to GOLD FROM PLATING SOLUTION is 1:1~24:1.
7. the preparation method that elctro-catalyst is precipitated in the carbon-based oxygen of Ni, Fe doping as claimed in claim 4, it is characterised in that: step
(3) heating rate of roasting described in is 1~10 DEG C/min；Maturing temperature is 400~800 DEG C.
8. the preparation method that elctro-catalyst is precipitated in the carbon-based oxygen of Ni, Fe doping as claimed in claim 4, it is characterised in that: step
(3) inert atmosphere is one or more of nitrogen, argon gas, helium, neon.
9. the preparation method that elctro-catalyst is precipitated in the carbon-based oxygen of Ni, Fe doping as claimed in claim 4, it is characterised in that: step
(4) pickling is one of hydrochloric acid, sulfuric acid, nitric acid, oxalic acid or a variety of, and the pH of the acid is 1 to 3.
10. the application that elctro-catalyst is precipitated in a kind of carbon-based oxygen of the doping of Ni, Fe described in claim 1-3, it is characterised in that: described
Catalyst is precipitated in secondary metals air-fuel battery or electrolyzed alkaline water hydrogen production process in oxygen.
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| CN110459775A (en) * | 2019-08-12 | 2019-11-15 | 苏州大学 | Light inorganic element doping nickel-base material and the preparation method and application thereof |
| CN111330620A (en) * | 2020-03-11 | 2020-06-26 | 中国科学技术大学 | Intercalation type graphite-like carbon nitride composite material, preparation method and application thereof |
| CN111359651A (en) * | 2020-04-26 | 2020-07-03 | 浙江大学 | Transition metal-nitrogen coordinated carbon gel electrocatalyst and preparation method and application thereof |
| CN114534765A (en) * | 2022-03-02 | 2022-05-27 | 浙江大学 | Partially graphitized carbon nitride supported noble metal material, preparation method and application |
| CN116154200A (en) * | 2022-12-30 | 2023-05-23 | 郑州大学 | Multi-metal atom supported carbon nitride catalyst and application thereof |
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