CN107570166A - A kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method and application - Google Patents
A kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method and application Download PDFInfo
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- CN107570166A CN107570166A CN201710791408.9A CN201710791408A CN107570166A CN 107570166 A CN107570166 A CN 107570166A CN 201710791408 A CN201710791408 A CN 201710791408A CN 107570166 A CN107570166 A CN 107570166A
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Abstract
The application of elutriation oxygen is electrolysed the invention discloses a kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method and based on the catalyst, belongs to nano-catalytic, nano material, Metal-organic frame material technical field.Aspartic acid aqueous slkali and copper nitrate manganese nitrate cobalt nitrate solution room temperature are blended its key step, filter and dry, the nano-fibre supported Co of Cu MOF (II) and Mn (II) ion nanofiber, i.e. CuMnCo MOF nanofibers is made;The heating of CuMnCo MOF nanofibers air atmosphere is made.The raw materials used cost of the catalyst preparation is low, and preparation technology is simple, and energy consumption of reaction is low, has prospects for commercial application.The catalyst is used for efficient catalytic electrolysis elutriation oxygen, has good analysis oxygen electro catalytic activity and electrochemical stability.
Description
Technical field
The present invention relates to a kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method and by the catalyst
For being electrolysed the application of elutriation oxygen, belong to nano-catalytic, nano material, Metal-organic frame material technical field.
Background technology
As the increasingly raising of people's material life and Industry Development Level, environmental pollution and energy crisis are continuous worsening.
Counted according to 2003, the Gt of whole world Recoverable Gas Reserves 2.4, the Gt of crude oil 138.3, add up to 140.7 Gt, by annual output 3.2
Gt is calculated, and can be stored up to adopt and is limited in year 44 years.Aeronautics and Astronautics, chemical industry, ship, automobile use oil, the whole world to the height of oil according to
Once relying causes oil shortage, All Around The World, which will face, to shut down.Also, fossil fuel contains carbon, dust and sulphur etc., burning
Environment is unavoidably polluted afterwards.Mankind's demand growing day by day to the energy, fossil fuel are petered out, and find a kind of cleaning energy
Source substitute is extremely urgent.Obtaining the clean and effective energy (hydrogen and oxygen) turns into the focus of modern scientific research.Water is ground
One of most abundant resource of hydrogeneous oxygen element on ball, generation of hydrogen by dissociation of water and oxygen, hydrogen exothermic combustion are changed into water again, should
Process regeneration, cleaning and green.The reaction of electrocatalytic decomposition water includes liberation of hydrogen (hydrogen evolution reaction, HER)
With analysis oxygen (oxygen evolution reaction, OER) two half-reactions, wherein, liberation of hydrogen faster, and analyses oxygen and is related to bond cleavage 4
Individual O-H covalent bonds, two hydrones lose four electronics and power consumption generation O-O covalent bonds, it is necessary to overcome higher energy barrier ability
Realize.Therefore, scholar has paid many effort, efficient oxygen-separating catalyst is developed.In the system much explored, iridium dioxide
(IrO2) and ruthenic oxide (RuO2) it is considered as most effective.However, their rare and expensive prices, it is actual extensively to limit its
Application, therefore, efficient, inexpensive and earth rich content the base metal oxygen-separating catalyst of exploitation, reduce analysis oxygen electric consumption into
For an opportunities and challenges.
Metal organic complex has porosity height, specific surface area is big, duct is regular, aperture is adjustable, synthesis is convenient, can root
According to target to be chemically modified, the advantages that structure-rich is various and easily designed, therefore, absorb and separate, catalysis in gas
The various aspects such as reaction, sensing material, photoelectric material, insoluble drug release obtain a wide range of applications.At present, come from MOFs precursors or
The research of the functional material of template is increasing, for example, porous carbon, metal oxide, metal/carbon and metal oxide/carbon are received
Rice material has been reported, constructed 3D metal oxides, for efficient ultracapacitor, lithium ion battery and hydrogen reduction,
Show excellent property.2014, Chaikittisilp and his team reported prepare electricity by precursor of MOFs first
Catalyst is used for the report of decomposition water, and they use class zeolite Co-MOF (zeolitic imidazolate framework-
9, ZIF-9) nanoporous Co is prepared for precursorxOy- C composite electro-catalysis OER.Because of the side of direct high temperature pyrolysis MOFs precursors
Method frequently results in framework and collapses and reunite, therefore, at present frequently with an innovative strategy be to utilize such as graphene, more walls
The nano carbon material load MOFs of CNT (multiwalled carbon nanotubes, CNTs), then pass through high temperature pyrolysis
C-base composte material elctro-catalyst is prepared, to prevent product from reuniting and improve its specific surface area.For example, 2016, Aijaz and he
Team by Co-MOF in H2The reduction of atmosphere high temperature and oxidizing roasting, have been made a kind of Co@Co3O4Nano-particle is embedded in carbon and received
The carbon polyhedron high activity oxygen-separating catalyst of the N doping of mitron grafting.Although MOFs species is various, easily prepared and transformation
For the elctro-catalyst MOFs precursors of controlled morphologies, limited amount, at present, using three-dimensional (3D) MOFs crystallites or nanocrystal before
Body prepares the research of oxygen-separating catalyst it has been reported that as far as we know, oxygen-separating catalyst is prepared based on one-dimensional MOFs nanofibers
Research have no report.
The content of the invention
One of technical assignment of the present invention is to make up the deficiencies in the prior art, there is provided a kind of composite carbon and transition elements
Oxide nano catalyst preparation method, the raw materials used cost of this method is low, and preparation technology is simple, and energy consumption of reaction is low, has work
Industry application prospect.
The two of the technical assignment of the present invention are to provide the purposes of composite carbon and the transition elements oxide of mutually nanocatalyst,
Will the composite carbon and transition elements oxide of mutually nanocatalyst be used for catalytic electrolysis elutriation oxygen, the catalyst has good analysis
Oxygen electro catalytic activity and electrochemical stability.
To achieve the above object, the technical solution adopted by the present invention is as follows:
1. a kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method, step are as follows:
Copper nitrate, manganese nitrate and cobalt nitrate are codissolved in 15-18 mL water, obtain copper nitrate-manganese nitrate-nitric acid of blueness clarification
Cobalt mixed liquor;0.40 mmol L-Aspartic acid and 0.50-0.58 mmol sodium hydroxides are dissolved in 2.0-4.0 mL water, obtained
To the aspartic acid aqueous slkali of clarification;Aspartic acid aqueous slkali is added in copper nitrate-manganese nitrate-cobalt nitrate mixed liquor, room
Warm 5min, generation precipitation;Filtered after 1h, 60 DEG C of dryings, the nano-fibre supported Mn of Cu-MOF (II) are made and Co (II) ion is received
Rice fiber, i.e. CuMnCo-MOF nanofibers;CuMnCo-MOF nanofibers are placed in diamond heating, obtain composite carbon and mistake
Cross element oxide nanocatalyst;
1)The copper nitrate, manganese nitrate and cobalt nitrate, amount is than being 1:3:1, the dosage of copper nitrate is 1.5-2.6 mmol;
2)The Cu-MOF nanofibers, chemical formula are [CuL (H2O)] n, L are aspartic acid H2L L (II) ion;Cu-
One cellular construction of MOF nanofibers, by Cu (II) ion center, L (II) ion and a H2O molecule structures
Into;
3)The CuMnCo-MOF nanofibers, it is by a width of 90-160 nm in footpath, a length of 400-900 um Cu-MOF Nanowires
Tie up load C o (II) and Mn (II) ion composition;
4)Composite carbon and the transition elements oxide of mutually nanocatalyst, it is by semiconductor CuO, MnO2And Co2O3Nano-particle is born
It is loaded in the filamentary composites formed on carbon crystallite, it is wide 80-130 nm of fiber footpath, long 300-850 μm;
5)The CuMnCo-MOF nanofibers are placed in diamond heating, are carried out under air atmosphere, heating rate be 3-5 DEG C/
Min, 250-300 DEG C is heated to, is incubated 1.5-2.5 h, then, room temperature is cooled to 2 DEG C/min rate of temperature fall.
2. composite carbon as described above and transition elements oxide of mutually nanocatalyst answering as electrolysis water oxygen-separating catalyst
With step is as follows:
6mg composite carbons and transition elements oxide of mutually nanocatalyst are scattered in 250 μ L isopropanols, 720 μ L water and 30 μ
L, in 5 wt% perfluorinated resin solution, room temperature 120W ultrasound 10-15min, uniform mixed liquor is made;The 6 μ L mixed liquors are added dropwise
Onto glass-carbon electrode, drying at room temperature, composite carbon and transition elements oxide of mutually nanocatalyst working electrode is made;
Using three-electrode electro Chemical work station, composite carbon and transition elements oxide of mutually nanocatalyst working electrode, Pt pieces (5
The mm of the mm of mm × 5 × 0.1) it is that Ag/AgCl electrodes be reference electrode to electrode, in electrolyte is the 0.5 M KOH aqueous solution
Test the water-based energy of electrocatalytic decomposition.
Above-mentioned carbon-based copper cobalt/cobalt oxide nanometer sheet electrolysis elutriation oxygen, as current density, J=10mA/cm2When, current potential 1.48
V vs RHE;Tafel slope is 65mV dec-1, illustrate that the material efficiently analyses oxygen catalytic activity;Before circulation 500 times
Afterwards, such material polarization curve does not find obvious change, shows that catalyst has good stability.
The beneficial technique effect of the present invention:
1. composite carbon and transition elements oxide of mutually nanocatalyst that the present invention obtains are by one-dimensional metal organic framework
CuMnCo-MOF nanofibers, the 250-300 DEG C of heating pyrolysis generation of air atmosphere condition, preparation process technique is simple, simple and easy to control,
Product preparation efficiency is high, is easy to industrialize.
2. the invention provides a kind of composite carbon and transition elements oxide of mutually nanocatalyst as the oxygen catalysis of electrolysis elutriation
The application of agent.Because the catalyst is by CuO, MnO2And Co2O3Semi-conductor nano particles are supported on the nanometer formed on carbon crystallite
Fiber, regular appearance, single scattered, specific surface area is high, exposes more and different avtive spots, has played CuO, MnO2With
Co2O3The synergy of semi-conductor nano particles and carbon crystallite so that the catalysis analysis oxygen based on the composite, catalytic efficiency
High and stability is good.
Embodiment
With reference to embodiment, the invention will be further described, but protection scope of the present invention is not only limited to implement
Example, the change that professionals in the field is made to technical solution of the present invention, all should belong in protection scope of the present invention.
Embodiment 1
A kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method
By 1.5 mmol copper nitrates, amount is than being 1:3:1 copper nitrate, manganese nitrate and cobalt nitrate is codissolved in 15-18 mL water, obtains
Copper nitrate-manganese nitrate-cobalt nitrate mixed liquor of blueness clarification;By 0.40 mmol L-Aspartic acid and 0.50 mmol hydrogen-oxygens
Change sodium and be dissolved in 2.0 mL water, the aspartic acid aqueous slkali clarified;Aspartic acid aqueous slkali is added to copper nitrate-nitric acid
In manganese-cobalt nitrate mixed liquor, room temperature 5min, generation precipitation;Filtered after 1h, 60 DEG C of dryings, it is nano-fibre supported that Cu-MOF is made
Mn (II) and Co (II) ion nanofiber, i.e. CuMnCo-MOF nanofibers;CuMnCo-MOF nanofibers are placed in tubular type
Heated under stove air atmosphere, heating rate is 3 DEG C/min, is heated to 250 DEG C, is incubated 1.5 h, then, is cooled with 2 DEG C/min
Speed is cooled to room temperature, and composite carbon and transition elements oxide of mutually nanocatalyst is made.
Embodiment 2
A kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method
By 2.6 mmol copper nitrates, amount is than being 1:3:1 copper nitrate, manganese nitrate and cobalt nitrate is codissolved in 18 mL water, obtains blueness
Copper nitrate-manganese nitrate-cobalt nitrate mixed liquor of clarification;By 0.40 mmol L-Aspartic acid and 0.58 mmol sodium hydroxides
4.0 mL water are dissolved in, the aspartic acid aqueous slkali clarified;Aspartic acid aqueous slkali is added to copper nitrate-manganese nitrate-nitre
In sour cobalt mixed liquor, room temperature 5min, generation precipitation;Filtered after 1h, 60 DEG C of dryings, the nano-fibre supported Mn of Cu-MOF (II) are made
With Co (II) ion nanofiber, i.e. CuMnCo-MOF nanofibers;CuMnCo-MOF nanofibers are placed in tubular type stove air
Heated under atmosphere, heating rate is 5 DEG C/min, is heated to 300 DEG C, is incubated 2.5 h, then, cold with 2 DEG C/min rate of temperature fall
But room temperature is arrived, composite carbon and transition elements oxide of mutually nanocatalyst is made.
Embodiment 3
A kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method
By 2.0 mmol copper nitrates, than for 1:3:1 copper nitrate, manganese nitrate and cobalt nitrate amount is codissolved in 16.5 mL water, obtains indigo plant
Copper nitrate-manganese nitrate-cobalt nitrate mixed liquor of color clarification;By 0.40 mmol L-Aspartic acid and 0.54 mmol hydroxides
Sodium is dissolved in 3.0 mL water, the aspartic acid aqueous slkali clarified;By aspartic acid aqueous slkali be added to copper nitrate-manganese nitrate-
In cobalt nitrate mixed liquor, room temperature 5min, generation precipitation;Filtered after 1h, 60 DEG C of dryings, the nano-fibre supported Mn of Cu-MOF are made
(II) and Co (II) ion nanofiber, i.e. CuMnCo-MOF nanofibers;CuMnCo-MOF nanofibers are placed in tube furnace
Heated under air atmosphere, heating rate is 4 DEG C/min, is heated to 275 DEG C, is incubated 2.0 h, then, is cooled with 2 DEG C/min
Speed is cooled to room temperature, and composite carbon and transition elements oxide of mutually nanocatalyst is made.
Embodiment 4
Cu-MOF nanofibers described in embodiment 1-3, chemical formula are [CuL (H2O)] n, L are aspartic acid H2L L (II) from
Son;One cellular construction of Cu-MOF nanofibers, by Cu (II) ion center, L (II) ion and a H2O
Molecule is formed;The CuMnCo-MOF nanofibers, received by a width of 90-160 nm in footpath, a length of 400-900 um Cu-MOF
The fiber-loaded Co (II) of rice and Mn (II) ion composition;Composite carbon and the transition elements oxide of mutually nanocatalyst, it is by half
Conductor CuO, MnO2And Co2O3The filamentary composites that nanometer particle load is formed on carbon crystallite, the wide 80-130 of fiber footpath
It is nm, long 300-850 μm.
The application of the composite carbon of embodiment 5 and transition elements oxide of mutually nanocatalyst as electrolysis water oxygen-separating catalyst
By 6mg composite carbons made from embodiment 1 and transition elements oxide of mutually nanocatalyst, be scattered in 250 μ L isopropanols,
In 720 μ L water and 30 μ L, 5 wt% perfluorinated resin solution, room temperature 120W ultrasound 10-15min, uniform mixed liquor is made;Drop
Add 6 μ L mixed liquors to glass-carbon electrode, drying at room temperature, composite carbon and the work of transition elements oxide of mutually nanocatalyst is made
Electrode;
Using three-electrode electro Chemical work station, composite carbon and transition elements oxide of mutually nanocatalyst working electrode, Pt pieces (5
The mm of the mm of mm × 5 × 0.1) it is that Ag/AgCl electrodes be reference electrode to electrode, in electrolyte is the 0.5 M KOH aqueous solution
Test the water-based energy of electrocatalytic decomposition.
The step of embodiment 6 and method only receive composite carbon and transition elements oxide of mutually made from embodiment 1 with embodiment 5
Rice catalyst replaces with catalyst made from embodiment 2.
The step of embodiment 7 and method only receive composite carbon and transition elements oxide of mutually made from embodiment 1 with embodiment 5
Rice catalyst replaces with catalyst made from embodiment 3.
Composite carbon made from the embodiment 1-7 of embodiment 8 and transition elements oxide of mutually nanocatalyst electrolysis elutriation oxygen, when
Current density, J=10mA/cm2When, current potential is 1.48 V vs RHE;Tafel slope is 65mV dec-1, illustrate material height
The analysis oxygen catalytic activity of effect;Before and after circulation 500 times, such material polarization curve does not find obvious change, shows to be catalyzed
Agent has good stability.
Claims (7)
1. a kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method, it is characterised in that step is as follows:
Copper nitrate, manganese nitrate and cobalt nitrate are codissolved in 15-18 mL water, obtain copper nitrate-manganese nitrate-nitric acid of blueness clarification
Cobalt mixed liquor;0.40 mmol L-Aspartic acid and 0.50-0.58 mmol sodium hydroxides are dissolved in 2.0-4.0 mL water, obtained
To the aspartic acid aqueous slkali of clarification;Aspartic acid aqueous slkali is added in copper nitrate-manganese nitrate-cobalt nitrate mixed liquor, room
Warm 5min, generation precipitation;Filtered after 1h, 60 DEG C of dryings, the nano-fibre supported Mn of Cu-MOF (II) are made and Co (II) ion is received
Rice fiber, i.e. CuMnCo-MOF nanofibers;CuMnCo-MOF nanofibers are placed in diamond heating, obtain composite carbon and mistake
Cross element oxide nanocatalyst.
2. composite carbon as claimed in claim 1 and transition elements oxide of mutually nanocatalyst preparation method, it is characterised in that institute
Copper nitrate, manganese nitrate and cobalt nitrate are stated, amount is than being 1:3:1, the dosage of copper nitrate is 1.5-2.6 mmol.
3. a kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method as claimed in claim 1, its feature exist
In the Cu-MOF nanofibers, chemical formula is [CuL (H2O)] n, L are aspartic acid H2L L (II) ion;Cu-MOF receives
One cellular construction of rice fiber, by Cu (II) ion center, L (II) ion and a H2O molecules are formed.
4. a kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method as claimed in claim 1, its feature exist
In the CuMnCo-MOF nanofibers, being by a width of 90-160 nm in footpath, a length of 400-900 um Cu-MOF nanofibers
Load C o (II) and Mn (II) ion composition.
5. a kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method as claimed in claim 1, its feature exist
In composite carbon and the transition elements oxide of mutually nanocatalyst, being by semiconductor CuO, MnO2And Co2O3Nanometer particle load
The filamentary composites formed on carbon crystallite, it is wide 80-130 nm of fiber footpath, long 300-850 μm.
6. a kind of composite carbon and transition elements oxide of mutually nanocatalyst preparation method as claimed in claim 1, its feature exist
In, the CuMnCo-MOF nanofibers are placed in diamond heating, are carried out under air atmosphere, heating rate be 3-5 DEG C/
Min, 250-300 DEG C is heated to, is incubated 1.5-2.5 h, then, room temperature is cooled to 2 DEG C/min rate of temperature fall.
7. composite carbon and transition elements oxide of mutually nanocatalyst prepared by preparation method as claimed in claim 1 are as electrolysis
The application of elutriation VPO catalysts.
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CN108671923A (en) * | 2018-05-10 | 2018-10-19 | 宁波大学 | Cu oxide/cobalt/cobalt oxide catalyst with core-casing structure and preparation method thereof for electrolysis water |
CN109252180A (en) * | 2018-09-19 | 2019-01-22 | 安徽师范大学 | A kind of ternary MOF nano-chip arrays material, preparation method and applications |
CN109647407A (en) * | 2019-02-12 | 2019-04-19 | 济南大学 | A kind of preparation method and application based on bimetallic MOF nanocrystalline composite material |
CN110586191A (en) * | 2019-09-18 | 2019-12-20 | 常州大学 | Oxygen evolution catalyst of CoCu-MOF/SNPC compounded by MOF material |
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CN109252180A (en) * | 2018-09-19 | 2019-01-22 | 安徽师范大学 | A kind of ternary MOF nano-chip arrays material, preparation method and applications |
CN109647407A (en) * | 2019-02-12 | 2019-04-19 | 济南大学 | A kind of preparation method and application based on bimetallic MOF nanocrystalline composite material |
CN110586191A (en) * | 2019-09-18 | 2019-12-20 | 常州大学 | Oxygen evolution catalyst of CoCu-MOF/SNPC compounded by MOF material |
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