CN109713326A - The porous carbon coating eight of Heteroatom doping vulcanizes the application of nine cobalt composite catalysts - Google Patents
The porous carbon coating eight of Heteroatom doping vulcanizes the application of nine cobalt composite catalysts Download PDFInfo
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- CN109713326A CN109713326A CN201910110004.8A CN201910110004A CN109713326A CN 109713326 A CN109713326 A CN 109713326A CN 201910110004 A CN201910110004 A CN 201910110004A CN 109713326 A CN109713326 A CN 109713326A
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- heteroatom doping
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Abstract
The invention discloses a kind of porous carbon coating Co of Heteroatom doping9S8Application of the composite catalyst in electrocatalytic oxidation reduction reaction belongs to composite catalyst and electrocatalytic oxidation reduction and zinc-air battery technical field.The composite catalyst, for presoma, is obtained with three hetero atom mixed matching cobalt-based metal-organic framework materials (writing a Chinese character in simplified form are as follows: Co-MOF) of nitrogen oxygen sulphur by carbonization, is used for efficient electric catalytic oxidation-reduction.In 0.1 mol L‑1Potassium hydroxide electrolyte in, the hydrogen reduction half wave potential of the catalyst is 0.78 V, and limiting diffusion current is 5.45 mA cm‑2.Pass through the cyclic charging and discharging test of 48 h with the zinc and air cell that prepared catalyst assembles, charging/discharging voltage difference shows that prepared catalyst has very strong stability, have higher practical application value there is no significantly changing.
Description
Technical field
The present invention relates to composite catalyst and electro-catalysis and zinc-air battery technical fields, and in particular to a kind of hetero atom
Adulterate porous carbon coating Co9S8Application of the composite catalyst in electrocatalytic oxidation reduction reaction and zinc-air battery.
Background technique
The mistake that the sustainable growth of global energy requirements and the mankind supply fossil fuel (such as coal, oil and natural gas)
Degree, which relies on, makes the mankind just gradually fall into energy crisis.Although wind energy and solar energy are developed, have to these clean energy resourcies
It is current maximum technical problem that effect ground, which utilizes,.Therefore, electrochemical energy storage technology is come into being.Battery is a kind of important electrification
Energy storage technology is learned, chargeable zinc-air battery is considered as one of most promising energy-storage system, because it is with higher
Theoretical energy density, inexpensive and higher safety.Its is very widely used, such as portable electronic product and electric car.
In cell reaction, for positive redox reactions because of slower dynamic process, higher overpotential is system
The about key factor of metal-air battery exploitation.And effective catalyst can overcome its deficiency, thus, new and effective positive oxygen is also
The research and development of former catalysts are always the hot topic in the field.Currently, precious metal material (such as: platinum, palladium etc.) it is activity
Highest is also most common electrocatalytic oxidation reducing catalyst, but its high cost, low reserves and in catalytic reaction process
The disadvantages of middle easy in inactivation, seriously limits the extensive use of such material, also counteracts the fast development of field of batteries.
Metal organic frame (MOFs) material has the controllability and crystalline state of unique structure diversity, construction unit
The advantages such as uniform sequential distribution of each element, are concerned in recent years in MOFs material.Template is sacrificed as presoma or certainly using MOFs
Preparing porous carbon-based compound material by pyrolysis processing is even more the extensive concern by scientist.Largely organic based on metal
New material in the research of the various composite carbon sills of frame (MOFs) precursor preparation, applied to electrocatalytic oxidation reduction
Increase year by year.It is based especially on hetero atom (nitrogen phosphate and sulfur etc.) the doping porous carbon of metal organic frame (MOFs) precursor preparation
The material of matrix carried metal compound has largely been used in the research of electrocatalytic oxidation reduction.It is reported that Heteroatom doping
Porous carbon materials carrying transition metal sulfide has very strong catalytic activity in electro-catalysis oxygen evolution reaction field, however in electrocatalytic oxidation
The research in the fields such as reduction and metal-air battery is also fewer.Therefore, the compound how miscellaneous original of New high-efficient low-cost is developed
Sub- doped porous carbon material coats transient metal sulfide nano material, for electrocatalytic oxidation reduction and metal-air battery
Positive electrode plays a significant role to the research and development of catalyst in the promotion field and realistic meaning.
Summary of the invention
The purpose of the present invention is to provide a kind of Heteroatom doping porous carbon materials to coat Co9S8Nano-particles reinforcement type is urged
Agent is (referred to as: Co9S8@TDC) application in electrocatalytic oxidation reduction reaction and metal-air battery.
To achieve the purpose of the present invention, it includes the heteroatomic organic ligand 4 of nitrogen oxygen sulphur three, 4'- (sulfo group two that the present invention, which selects,
Thiobis (4,1- phenylene)) three hetero atom of nitrogen oxygen sulphur constructed of two pyridines and assistant ligand terephthalic acid (TPA) and soluble cobalt
Mixed matching cobalt-based metal-organic framework materials (writing a Chinese character in simplified form are as follows: Co-MOF) be a kind of compound electrocatalytic oxidation of precursor preparation also
Raw catalyst (Co9S8@TDC), it is used for electrocatalytic oxidation reduction reaction and zinc-air battery.
The efficient electric catalytic oxidation-reduction catalyst is prepared via a method which:
(1) respectively by 4,4'- (two thiobis of sulfo group (4,1- phenylene)) two pyridines, terephthalic acid (TPA), soluble cobalt
It is soluble in water, n,N-Dimethylformamide and the reaction of water heated constant temperature is added, after reaction, is down to room temperature to system temperature and obtains
To compound A.
(2) compound A obtained in step (1) is filtered, with n,N-Dimethylformamide, after drying before Co-MOF
Drive body.
(3) it by the resulting Co-MOF precursor breakdown mill of step (2), calcines under nitrogen atmosphere, gained powder ultrasonic
Washing obtains target product after then using deionized water and ethanol washing, drying.
4,4'- (two thiobis of sulfo group (4,1- phenylene)) two pyridines in step (1), cobalt nitrate and terephthalic acid (TPA) rub
Your ratio is 3:4:1.5, and the volume ratio of solvent for use n,N-Dimethylformamide and water is 2:1.
The temperature of step (3) presoma calcining is 600-900 DEG C, and heating rate is 10 DEG C/min.
The preferred cobalt nitrate of soluble cobalt.
It is applied the composite material as catalyst in terms of electrocatalytic oxidation reduction reaction and zinc-air battery.
Above-mentioned application method is as follows:
1. electrocatalytic oxidation reduction reaction: adulterating the Co of porous carbon load with prepared nitrogen oxygen sulphur three9S8Compound material is work
The catalyst for making electrode is tested using three-electrode system for its catalytic oxidation-reduction reactivity worth.With silver-silver chloride (Ag/
AgCl) electrode is reference electrode, graphite rod is auxiliary electrode, and potassium hydroxide aqueous solution is electrolyte, preferably 0.1mol L-1。
2. zinc-air battery is tested: the Co loaded with prepared Heteroatom doping porous carbon9S8Compound material is catalyst,
Coated in anode is used as in nickel foam, it is diaphragm among positive and negative anodes that zine plate, which is cathode, and anode is sky with air contact side
Gas diffusion layer, electrolyte are potassium hydroxide aqueous solution and zinc acetate aqueous solution mixed solution, preferably 6mol L-1Potassium hydroxide and
0.2mol L-1Zinc acetate.
The invention has the advantages that: the electrocatalytic oxidation reducing material is that have with three hetero atom mixed matching cobalt-based metal of nitrogen oxygen sulphur-
Machine frame frame material (Co-MOF) is presoma, and the porous carbon coating Co of Heteroatom doping is prepared into after carbonization9S8It is compound to urge
Agent.Carbon-based frame specific surface area with higher, micropore, mesoporous, macropore and the multistage pore property deposited.These structural advantages can
To provide bigger contact area for catalyst, the more active sites of exposure provide better mass transfer channel, at the same nitrogen, oxygen,
Doping of three hetero atom of sulphur in carbon matrix can increase the active site of catalyst, improve the electric conductivity of catalyst thus into one
Step promotes its catalytic activity, and combines the excellent catalytic activity of metal sulfide.By the effective compound of the two and into one
Step improves the electro catalytic activity of target material, can apply in electrocatalytic oxidation reduction reaction and zinc-air battery research neck
Domain has important value and realistic meaning.Experiments verify that catalyst prepared by the present invention is with more preferable than platinum carbon catalyst
Stability and the ability that there is extraordinary methanol tolerance to poison.In electrocatalytic oxidation reduction application, with the precious metal catalysts such as platinum carbon
Agent is suitable compared to catalytic effect, half wave potential 0.78V, and limiting diffusion current is 5.45mA cm-2.In zinc-air battery application
In, current density is 10 and 100mA cm-2When, cell voltage is respectively 1.20V and 0.85V, and battery maximum power density is
101.5mW cm-2.There is preferable application effect compared to current noble metal catalyst.
Detailed description of the invention
Fig. 1 is powder x-ray diffraction (PXRD) the map a and monocrystalline mould of Co-MOF presoma synthesized in step (1)
Quasi- PXRD map b comparison diagram；
Fig. 2 is catalyst Co prepared by the present invention9S8Powder x-ray diffraction (PXRD) phenogram of@TDC-900, a- are
Synthetic catalyst of the present invention, b- Co9S8#86-2273。
Fig. 3 is the scanning electron microscope (a) and transmission electron microscope picture (b, c) that catalyst prepared by the present invention amplifies different multiples；
A) scanning electron microscope shows that resulting materials are loose porous structure, b in) in transmission electron microscope be shown in loose matrix load it is very much
Nano particle.C) for by carbon-coated Co9S8The lattice diffraction fringe of nano particle.
Fig. 4 is catalyst Co prepared by the present invention9S8Nitrogen adsorption isotherm of@TDC-900 at a temperature of 77K, illustration
For according to the pore size distribution curve of the calculated catalyst of adsorption isotherm.
Fig. 5 is catalyst Co prepared by the present invention9S80.1mol L of the@TDC in oxygen saturation and nitrogen saturation-1Hydrogen-oxygen
Change the cyclic voltammetry curve in potassium solution.
Fig. 6 is the 1.0mol L that catalyst prepared by the present invention is saturated in oxygen under different calcination temperatures-1Potassium hydroxide
Linear scan polarization curve in solution, rotating disk electrode (r.d.e) revolving speed are 1600 revs/min.
Fig. 7 is catalyst Co prepared by the present invention9S8@TDC-900 is as working electrode active material in 1.0mol L-1
Linear scan polarization curve in potassium hydroxide solution after 3000 coils scan cycle volt-ampere.
Active material Co prepared by Fig. 89S8@TDC-900 tests the tolerance of methanol.
Fig. 9 is test zinc and air cell schematic device.
Figure 10 be assembled using catalyst prepared by the present invention as positive electrode zinc and air cell electric discharge polarization curve and
Power density curve.
Figure 11 is the zinc and air cell cyclical stability test assembled using catalyst prepared by the present invention as positive electrode,
Charging and discharging currents density is 5mAcm-2。
Specific embodiment
Below by example, the present invention is described further:
Embodiment 1: the porous carbon materials cladding Co of Heteroatom doping is synthesized9S8Composite catalyst
(1) by tri- nitric hydrate cobalt of 13mg and 2.5mg terephthalic acid (TPA) acid and 11.2mg 4,4'- (two thiobis of sulfo group
(4,1- phenylene)) two pyridinium dissolutions are in 1mL n,N-Dimethylformamide and 0.5mL deionized water.Then in 90 DEG C of conditions
Under be stirred at reflux 48h and obtain red crystals.Through filtering, washed three times with n,N-Dimethylformamide, before being obtained after vacuum drying
It drives body (Co-MOF).
(2) presoma (Co-MOF) crystal obtained in 200mg step (1) is smashed and ground, is placed in quartz boat, by stone
Ying Zhou is placed in tube furnace, first lead to nitrogen 30min exhaust furnace air, then under nitrogen atmosphere tube furnace with 10 DEG C/min
Rate be warming up to 900 DEG C, and in 900 DEG C of calcining at constant temperature 3h.Cooled to room temperature obtains black porous solid, through dilute salt
Then sour supersound washing is centrifuged repeatedly washing for several times with deionized water and ethyl alcohol, target product is obtained after drying and grinding.
Embodiment 2: the porous carbon coating Co of Heteroatom doping prepared by the present invention9S8Compound material is as electro-catalysis
The performance test of agent
By 4mg Co of the present invention9S8@TDC catalyst is added in 100 μ L n,N-Dimethylformamide solution, and 10 μ L matter are added
The Nafion solution that percentage is 5% is measured, obtains finely dispersed catalyst slurry after ultrasonic disperse 30min.By 10 μ L slurries
Drop coating is in rotating disk electrode (r.d.e) and is dried at room temperature for.Electrocatalysis characteristic test uses three-electrode system, with silver-silver chloride
(Ag/AgCl) electrode is reference electrode, platinum filament is auxiliary electrode, 0.1mol L-1Potassium hydroxide aqueous solution is electrolyte.Tester
Device is Pine company Wavedriver10 constant potential/electric current instrument, MSR rotating disk electrode (r.d.e) device.
As shown in figure 5, the 0.1mol L with nitrogen saturation-1Cyclic voltammogram in potassium hydroxide solution is compared, in oxygen
Prepared catalyst has obviously oxygen reduction peak under conditions of saturation.
As shown in fig. 6, in the 0.1mol L of oxygen saturation-1In potassium hydroxide solution, electrode revolving speed is 1600 revs/min of item
Under part, the catalyst that different carburizing temperatures obtain has apparent oxygen reduction electric current.Wherein Co9S8@TDC-900 has best
Electrocatalytic oxidation reducing property, half wave potential similar with the catalytic effect of noble metal catalyst (platinum carbon, mass fraction 20%)
For 0.78V, limiting diffusion current is 5.45mA cm-2。
As shown in figure 8, in the 0.1mol L of oxygen saturation-1In potassium hydroxide solution, electrode revolving speed is 1600 revs/min of item
Under part.When methanol is added into system, the catalytic current of platinum carbon catalyst is substantially reduced, and catalyst prepared by the present invention
(Co9S8@TDC-900) catalytic current does not change substantially other than by slight interference, illustrate and noble metal catalyst phase
Than the ability that catalyst prepared by the present invention has extraordinary methanol tolerance to poison.
Embodiment 3: the porous carbon coating Co of Heteroatom doping prepared by the present invention9S8Composite catalyst is in zinc and air cell
In application.
It tests in conjunction with Fig. 9 with zinc and air cell schematic device.Cathode is zine plate, and anode is the prepared catalysis of the load present invention
The nickel foam of agent.Electrolyte is 6mol L-1Potassium hydroxide aqueous solution is separated by diaphragm between positive and negative anodes, and anode is contacted with air
It is on one side gas diffusion layers, gas diffusion layers are prepared by conductive black and polytetrafluoroethylene (PTFE).
Figure 10 is the polarized discharge curve and corresponding function of the zinc and air cell device assembled with prepared catalyst
Rate densogram, current density are 10 and 100mA cm-2When, cell voltage is respectively 1.20V and 0.85V, battery maximum work
Rate density is 101.5mW cm-2。
Shown in Figure 11, the zinc and air cell that the catalyst prepared by the present invention assembles passes through the cycle charge-discharge of 45h
Test, charging/discharging voltage difference show that prepared catalyst has very strong stability there is no significantly changing, have compared with
High practical application value.
Claims (6)
1. the porous carbon coating Co of Heteroatom doping9S8The application of composite catalyst, which is characterized in that as catalyst by its
It applies in electrocatalytic oxidation reduction reaction or zinc-air battery:
The Heteroatom doping porous carbon encapsulates Co9S8Composite catalyst is prepared via a method which:
(1) respectively by two thiobis of 4,4'-(sulfo group (4,1- phenylene)) two pyridines, terephthalic acid (TPA), soluble cobalt be dissolved in
In water, n,N-Dimethylformamide and the reaction of water heated constant temperature is added, after reaction, is down to room temperature to system temperature
Close object A；
(2) compound A obtained in step (1) is filtered, with n,N-Dimethylformamide, obtains Co-MOF forerunner after drying
Body；
(3) it by the resulting Co-MOF precursor breakdown mill of step (2), calcines under nitrogen atmosphere, the washing of gained powder ultrasonic,
Then target product is obtained after using deionized water and ethanol washing, drying.
2. the porous carbon coating Co of Heteroatom doping as described in claim 19S8The application of composite catalyst, feature exist
In the soluble cobalt is cobalt nitrate.
3. the porous carbon coating Co of Heteroatom doping as claimed in claim 1 or 29S8The application of composite catalyst, feature
Be, 4,4'-(sulfo group, two thiobis (4,1- phenylene) in step (1)) two pyridines, cobalt salt and terephthalic acid (TPA) molar ratio
For 3:4:1.5, the solvent n,N-Dimethylformamide and water volume ratio are 2:1.
4. the porous carbon coating Co of Heteroatom doping as claimed in claim 1 or 29S8The application of composite catalyst, feature
It is, the temperature of step (3) presoma calcining is 600-900 DEG C, and heating rate is 10 DEG C/min.
5. the porous carbon coating Co of Heteroatom doping as claimed in claim 1 or 29S8The application of composite catalyst, feature
It is, as follows as elctro-catalyst working electrode application method:
(1) by the porous carbon coating Co of Heteroatom doping9S8Composite catalyst Co9S8N,N-Dimethylformamide is added in@TDC
In, Nafion solution is added, obtains finely dispersed catalyst slurry after ultrasonic disperse；Catalyst slurry drop-coated is being rotated
On disk electrode and it is dried at room temperature for；(2) three-electrode system is used, using silver-silver chloride (Ag/AgCl) electrode as reference electricity
Pole, graphite rod are auxiliary electrode, and potassium hydroxide aqueous solution is electrolyte.
6. the porous carbon coating Co of Heteroatom doping as claimed in claim 1 or 29S8The application of composite catalyst, feature exist
In as follows as zinc-air battery application method:
By the porous carbon coating Co of Heteroatom doping9S8Composite catalyst Co9S8@TDC is coated in nickel foam as battery just
Pole, zine plate are cathode, are diaphragm among positive and negative anodes, and anode is air diffusion layer with air contact side, and electrolyte is hydroxide
Aqueous solutions of potassium and zinc acetate aqueous solution；The gas diffusion layers are prepared by conductive black and polytetrafluoroethylene (PTFE).
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| CN112408496A (en) * | 2020-11-09 | 2021-02-26 | 邵阳学院 | Nitrogen and sulfur co-doped carbon @ FeS nanotube and preparation method and application thereof |
| CN113659161A (en) * | 2021-07-20 | 2021-11-16 | 广州大学 | Electrocatalyst and preparation method and application thereof |
| CN114583127A (en) * | 2022-02-28 | 2022-06-03 | 南京工业大学 | Method for preparing CoNi-S @3D-C nano composite material and modified battery diaphragm |
| CN114744339A (en) * | 2022-03-03 | 2022-07-12 | 广州优能达科技有限公司 | Solid zinc-air battery |
| CN115505962A (en) * | 2022-10-20 | 2022-12-23 | 中国石油大学(华东) | Ultrathin nickel-doped nonacobalt octasulfide composite molybdenum disulfide electrocatalytic material and preparation method thereof |
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| CN110600707A (en) * | 2019-09-25 | 2019-12-20 | 郑州大学 | High-capacity electrode material for high-nitrogen-doped carbon-coated metal sodium sulfide secondary battery and application of high-capacity electrode material |
| CN111729676A (en) * | 2020-07-27 | 2020-10-02 | 湖南理工学院 | Oxygen electrode catalyst Co9S8Preparation method and application of porous carbon composite material |
| CN112408496A (en) * | 2020-11-09 | 2021-02-26 | 邵阳学院 | Nitrogen and sulfur co-doped carbon @ FeS nanotube and preparation method and application thereof |
| CN113659161A (en) * | 2021-07-20 | 2021-11-16 | 广州大学 | Electrocatalyst and preparation method and application thereof |
| CN114583127A (en) * | 2022-02-28 | 2022-06-03 | 南京工业大学 | Method for preparing CoNi-S @3D-C nano composite material and modified battery diaphragm |
| CN114583127B (en) * | 2022-02-28 | 2023-05-09 | 南京工业大学 | Method for preparing CoNi-S@3D-C nanocomposite and modified battery diaphragm |
| CN114744339A (en) * | 2022-03-03 | 2022-07-12 | 广州优能达科技有限公司 | Solid zinc-air battery |
| CN115505962A (en) * | 2022-10-20 | 2022-12-23 | 中国石油大学(华东) | Ultrathin nickel-doped nonacobalt octasulfide composite molybdenum disulfide electrocatalytic material and preparation method thereof |
| CN115505962B (en) * | 2022-10-20 | 2024-01-30 | 中国石油大学(华东) | Ultra-thin nickel-doped cobalt octasulfide composite molybdenum disulfide electrocatalytic material and preparation method thereof |
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Application publication date: 20190503 |