CN101752569A - Application of nickel-molybdenum carbide in production of anode of microbial fuel cell - Google Patents
Application of nickel-molybdenum carbide in production of anode of microbial fuel cell Download PDFInfo
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- CN101752569A CN101752569A CN201010019271A CN201010019271A CN101752569A CN 101752569 A CN101752569 A CN 101752569A CN 201010019271 A CN201010019271 A CN 201010019271A CN 201010019271 A CN201010019271 A CN 201010019271A CN 101752569 A CN101752569 A CN 101752569A
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- 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
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses application of nickel-molybdenum carbide in the production of the anode of a microbial fuel cell. Compared with molybdenum carbide, due to the doped nickel, the crystal formation of the nickel-molybdenum carbide is more complete, the degree of crystallinity is improved, and the specific surface area is enlarged. When used as an anode catalyst, the nickel-molybdenum carbide can easily catalyze the oxidation of products produced in microbial fermentation, and can greatly improve the electric energy output of a microbial fuel cell. Compared with the conventional Pt catalyst, the nickel-molybdenum carbide has the advantages of low price and wide scope of sources. The microbial fuel cell assembled with the nickel-molybdenum carbide as the anode catalyst can operate stably for a long term, and has high power output.
Description
Technical field
The invention belongs to the manufacturing field of microbiological fuel cell, be specifically related to nickel-molybdenum carbide is used to prepare anode of microbial fuel cell, and this anode is further used for preparing microbiological fuel cell.
Background technology
In the last few years, a new technology---microbiological fuel cell (MFCs) is surging forward, it is the product that microbial technique combines with battery technology, be a kind ofly to utilize microbe the chemical energy in the organic substance to be converted into the Blast Furnace Top Gas Recovery Turbine Unit (TRT) of electric energy, have generating and waste treatment double effects as catalyst.Except that high concentrated organic wastewater, MFCs can also be with the generating that acts as a fuel of pollutants such as sanitary sewage, human and animal excreta.Therefore it is an advanced biomass energy utilization technologies that development potentiality is huge, is expected to become the pillar technology that following debirs are handled.The basic principle of MFC is: organic substance acts as a fuel in the anaerobism anode chamber by microbiological oxidation, the electronics that produces is caught and passes to galvanic anode by microbe, electronics arrives negative electrode by external circuit, thereby form the loop and produce electric current, and proton arrives negative electrode by exchange membrane, with the oxygen water generation reaction.
The potential advantage of microbiological fuel cell self makes people very good to its development prospect, but it is lower than the fuel battery power density of other types that microbiological fuel cell produces, long-time running poor stability and cost of manufacture be high to limit its practical application, and its research at present also is in laboratory or lab scale level.Though in recent years owing to the efficiently application of electrogenesis iron-reducing bacterium, advanced electrode material, and the optimization of operational factor, make the MFC performance rapidly improve, maximum power output is from initial mWm
-3Level is brought up to 10 present～100Wm
-3But, (it is generally acknowledged that stablizing power output reaches 1kWm from practical application
-3The time) still have than big gap.Expensive proton exchange membrane, Pt catalyst also widespread usage in MFC.Up to now, reported that unique MFC battery pile that comes into operation is USN's research center development, as the electric power system of automatic meterorological oceanographic buoy, stable power output is 36mW (annual energy output is equivalent to 26 joint alkaline dry batteries), but involve great expense, spend 2500 dollars approximately.
The present Research of MFC and the subject matter that faces have determined the electric energy output that focuses on improving MFC, the reduction cost cost to its research.Summarize bibliographical information both domestic and external, main direction of studying can be summed up as: (1) electrogenesis microbe; (2) barrier film; (3) anode electron donor and electrode material; (4) cathode electronics acceptor and electrode material; (5) battery structure; (6) service conditionss such as temperature, pH, organic concentration and external resistance.Bacterization amount the having the greatest impact of adsorbing on the anode electrode material to its power density.Develop the power density that a kind of new anode material can further improve MFC, this is a great challenge.What the essential nature of the anode-catalyzed mechanism of MFC was not only biology also is an electrochemical process.In the past few years, some scientists are by modifying the anode material that improves MFC with different chemical catalysts.
Transition metal carbide mainly utilizes its high mechanical hardness and high-melting-point in traditional research, but they also are used to catalysis ammonia synthesis and decomposition, hydrogenolysis, isomerization, methanation catalyst, reactions such as hydrogenation now gradually.Because transition metal carbide is generally the IV group, it has the chemical property and the electronic property of platinum class existing reported literature.The activity that surpasses original active metal after the carburizing of bibliographical information IV group transition metal carbide.Existing many at present relevant transition metal carbides are applied to the research of hydrogen fuel cell.For example, being studied maximum is exactly tungsten carbide and molybdenum carbide.
Eelctro-catalyst has developed into bimetallic research subsequently, to promote the double-function catalyzing performance.Some studies show that the activity of nickel molybdenum carbide (NiMoC) in hydroxide reaction (HOR) is because the nickel-molybdenum alloy after the carburizing.On the other hand, nickel electrode has been used in the anode material of fused carbonate and Solid Oxide Fuel Cell, because it can at high temperature provide sufficient activity.
We show MO at research work in the past
2C can improve the performance, particularly power density of MFC as anode catalyst.Nickel-molybdenum carbide is not studied as yet as the MFC anode catalyst.The traditional several different synthetic methods of transition metal carbide are: carbothermic method under inert environments, temperature programming reaction method, chemical gaseous phase deposition method, high temperature synthetic method, ultrasonic synthetic method etc.These preparation method's complexity, the condition strictness.
Summary of the invention
Primary and foremost purpose of the present invention is to overcome the deficiency that prior art exists, a kind of cheapness, wide material sources and environmental friendliness are provided, the catalyst carbonization nickel molybdenum (NiMoC) of the simple catalysis hydroxide of preparation technology especially prepares the application in the anode of microbiological fuel cell at the preparation microbiological fuel cell.
For achieving the above object, technical scheme of the present invention is as follows:
The nickel-molybdenum carbide catalyst is applied to prepare anode of microbial fuel cell as the substitute of noble metal catalyst.
A kind of concrete mode as above-mentioned application the invention provides a kind of anode of microbial fuel cell, comprises the catalyst layer that conductive substrates and its surface have, and contains nickel-molybdenum carbide in the described catalyst layer.
For the performance that makes anode of microbial fuel cell of the present invention is better, adopt following prioritization scheme:
The preferred carbon felt of described conductive substrates (Carbon felt), graphite paper or carbon cloth.
Described catalyst layer is the mixture of nickel-molybdenum carbide and adhesive preferably.Wherein, the preferred 6%-48% of the mass content of described binding agent in mixture, more preferably 30%.
Described binding agent then is preferably any one or the two or more mixtures among polytetrafluoroethylene, polyvinylidene fluoride and the Nafion.
The present invention also provides above-mentioned any preparation method of anode of microbial fuel cell, it is characterized in that may further comprise the steps:
(1) preparation nickel-molybdenum carbide;
(2) with nickel-molybdenum carbide and binding agent mixing;
(3) be applied in pasty mixture on the conductive substrates equably;
(4) oven dry.
Wherein, in the step (1), the preferred following method of preparation nickel-molybdenum carbide catalyst:
(1) with molybdic acid and NiCl
26H
2(mol ratio Ni: Mo=1: 3) be dissolved in the ethylene glycol, brute force is stirred to NiCl to O in 60 ℃
26H
2O dissolves fully.Then, Mo: C=1: 2-1 in molar ratio: 4 add carbon sources (being the carbon source commonly used of metal carbides preparation field, as starch, sucrose or glucose etc.).After carbon source is heated dissolving, stir solvent, about 130 ℃, be condensed into the solvent of viscosity, form the parent fragment when again the solvent of viscosity being heated to 190 ℃.
(2) fragment is placed in the inherent alumina tube furnace of graphite boat and anneals, and temperature is 900 ℃, and under inertia body (as Ar gas) protection, annealing time is 2h.Be cooled to room temperature, promptly prepared navy blue nickel-molybdenum carbide sample powder.
The present invention and then a kind of microbiological fuel cell is provided comprises anode chamber, film negative electrode and external circuit three parts, and the anode chamber comprises anolyte, anode and electrogenesis microbe, and described anode is above-mentioned any anode of microbial fuel cell.
As preferably, the negative electrode of microorganism fuel cell is the Pt/C negative electrode.
Compared with prior art, the present invention has following beneficial effect:
The manufacture craft that the inventive method prepares nickel-molybdenum carbide is simple, and is cheap, safety, and environmental protection, the operating time is short.And the change carbon source, do not change its crystal formation, only change its degree of crystallinity.The doping of nickel makes that the crystal formation of molybdenum carbide catalyst is more regular, improves its degree of crystallinity; Compare with the molybdenum carbide catalysis electrode of bibliographical information, the oxidation of the easier catalysis microbial fermentation product of nickel-molybdenum carbide has improved the electric energy of MFCs greatly and has exported, and approximately is 2 times of its power output; The wide material sources of nickel-molybdenum carbide, cheap; Its stability is strong, for the commercial applications of MFCs is laid good basis.
Description of drawings
Fig. 1 is the comparison of the XRD standard diagram (a) of prepared nickel-molybdenum carbide sample (S) XRD figure of the present invention and molybdenum carbide.
Fig. 2 is the comparison of the XRD standard diagram (a) of prepared nickel-molybdenum carbide sample (G) XRD figure of the present invention and molybdenum carbide.
Fig. 3 is the sem photograph of nickel-molybdenum carbide sample (S).
Fig. 4 is the sem photograph of nickel-molybdenum carbide sample (G).
Fig. 5 is 6mgcm in neutral catholyte
-2NiMoC (S) is to the influence of single chamber battery power output;
Wherein, curve a is 6mgcm
-2NiMoC (S) catalysis electrode MFC output voltage is with the change curve of current density; Curve b is 6mgcm
-2NiMoC (S) catalysis electrode MFC power density is with the change curve of current density.
Fig. 6 is 6mgcm in neutral catholyte
-2NiMoC (G) is to the influence of single chamber battery power output;
Wherein, curve c is 6mgcm
-2NiMoC (G) catalysis electrode MFC output voltage is with the change curve of current density; Curve d is 6mgcm
-2NiMoC (G) catalysis electrode MFC power density is with the change curve of current density.
Embodiment
Below in conjunction with embodiment, the present invention is done detailed description further, but implementation of the present invention is not limited thereto.
The first step: Preparation of Catalyst
Nickel-molybdenum carbide
1, with molybdic acid and NiCl
26H
2(mol ratio Ni: Mo=1: 3) be dissolved in the ethylene glycol, brute force is stirred to NiCl to O in 60 ℃
26H
2O dissolves fully.Then, Mo: C=1 in molar ratio: 3.5 add starch in the mixture.After starch is heated dissolving, stir solvent, about 130 ℃, be condensed into the solvent of viscosity, form the parent fragment when again the solvent of viscosity being heated to 190 ℃.
2, fragment is placed in the inherent alumina tube furnace of graphite boat and anneals, and temperature is 900 ℃, and under the Ar protection, annealing time is 2h.Be cooled to room temperature, get the navy blue powder, be nickel-molybdenum carbide.
The XRD standard diagram (a) of prepared nickel-molybdenum carbide sample (S) XRD figure and molybdenum carbide more as shown in Figure 1.
Second step: physics characterizes
SEI voltage 25kV, electric current 10 are carried out in the SEM test on Japan's JSM-6380LV ESEM of science instrument
-1A.Fig. 3 is the sem photograph of nickel-molybdenum carbide sample (S).
The 3rd step: the preparation of base electrode
With prepared NiMoC (S) powder 108mg, add 1ml binding agent (30%～60%) polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF) mixing, stir into pasty state and ultrasonic dispersion; Pasty mixture is applied on the carbon felt equably, and 100 ℃ of oven dry promptly get 6mg/cm then
2NiMoC (S) catalysis electrode.
The 4th step: preparation Pt/C negative electrode
The Pt/C negative electrode stirred into pasty state and ultrasonic dispersion 30 minutes by commercial Pt/C of 20wt% and 5wt%Nafion binding agent.Pasty mixture is applied in carbon paper (3.0cm * 3.0cm, Pt/C carrying capacity 0.5 ± 0.2mg/cm equably
2) on, 100 ℃ of oven dry are promptly then.To be loaded with Pt/C cathode catalysis electrode cation-exchange membrane (one side that scribbles catalyst contacts with film) is 115 ℃ in temperature, and pressure is hot pressing 3 minutes under the 14MPa, takes out and is cooled to room temperature.
The 5th step: single chamber battery performance test
MFCs anolyte: 0.1g/L KCl, 0.25g/L NH
4Cl, the phosphate buffer of 10mM pH=7.0,10mL vitamin solution, 10mL trace element solution, 2g/L glucose.It is stand-by to sterilize.
The single chamber MFC anode chamber of 5mL Friedlander suspension inoculation being gone into to be equipped with above-mentioned aseptic anolyte is an anode with NiMoC (S)/carbon felt respectively, is made by commercial Pt/C of 20wt% and 5%Nafion binding agent with the Pt/C negative electrode.This MFC is inserted 1000 ohm of outer resistance circuits, the opening entry electricity generation process, move three periodic voltage output rules stable after, the output voltage when being changed external resistance and recorded the different extrernal resistance of MFC by resistance box is tried to achieve power output, the drafting polarization curve is as scheming.NiMoC (S)/carbon felt anode cell power output (2890mW/m
3, curve 6-b), this is because nickel-molybdenum carbide catalysis hydroxide is quickened the speed of MFC anode transmission electronic.The price of nickel-molybdenum carbide material is then more much lower than platinum, makes it have more application prospect.
The first step: Preparation of Catalyst
1, with molybdic acid and NiCl
26H
2(Ni: Mo=1: 3) be dissolved in the ethylene glycol, brute force is stirred to NiCl to O in 60 ℃
26H
2O dissolves fully.Then, incite somebody to action Mo: C=1 in molar ratio: 2 glucose add in the mixture, preparation precursor G.After glucose is heated dissolving, stir solvent, about 130 ℃, be condensed into the solvent of viscosity, form the parent fragment when again the solvent of viscosity being heated to 190 ℃.
2, fragment is placed in the inherent alumina tube furnace of graphite boat and anneals, and temperature is 900 ℃, and under the Ar protection, annealing time is 2h.Be cooled to room temperature, promptly get the navy blue powder.The XRD standard diagram (a) of prepared nickel-molybdenum carbide sample (G) XRD figure and molybdenum carbide more as shown in Figure 2.
Second step: physics characterizes
Step such as embodiment 1, Fig. 4 are the sem photograph of nickel-molybdenum carbide sample (G).
The 3rd step: the preparation of base electrode
NiMoC (G) powder 108mg is added 1mL binding agent (30%～60% polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF)) mixing, stir into pasty state and ultrasonic dispersion; Pasty mixture is applied on the carbon felt equably, and 100 ℃ of oven dry promptly get 6mg/cm then
2NiMoC (G) catalysis electrode.
The 4th step: preparation Pt/C negative electrode
Step such as embodiment 1
The 5th step: single chamber battery performance test
Step such as embodiment 1
This MFC polarization curve is as Fig. 8.Power output (the 4670mW/m of battery when being anode material with NiMoC (G)
3, curve 8-d) approximately be 2 times (seeing Table 1) with NiMoC (S)/carbon felt catalyticing anode battery power output.
The contrast of the different anode MFCs of table 1 electricity generation performance
Embodiment 3
The first step: Preparation of Catalyst
1, with molybdic acid and NiCl
26H
2(Ni: Mo=1: 1) be dissolved in the ethylene glycol, brute force is stirred to NiCl to O in 80 ℃
26H
2O dissolves fully.Then, Mo: C=1 in molar ratio: 4 add in the mixture preparation precursor s with sucrose.After sucrose is heated dissolving, stir solvent, about 100 ℃, be condensed into the solvent of viscosity, form the parent fragment when again the solvent of viscosity being heated to 150 ℃.
2, fragment is placed in the inherent alumina tube furnace of graphite boat and anneals, and temperature is 800 ℃, and under the Ar protection, annealing time is 4h.Be cooled to room temperature, promptly get the navy blue powder.
Second step: physics characterizes
Step such as embodiment 1
The 3rd step: the preparation of base electrode
Step such as embodiment 1
The 4th step: preparation Pt/C negative electrode
Step such as embodiment 1
The 5th step: single chamber battery performance test
Step such as embodiment 1
After tested, all performance of gained electrode and battery is similar to Example 1.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. the application of nickel-molybdenum carbide in the preparation anode of microbial fuel cell.
2. an anode of microbial fuel cell comprises the catalyst layer that conductive substrates and its surface have, and it is characterized in that: contain nickel-molybdenum carbide in the described catalyst layer.
3. anode of microbial fuel cell according to claim 2 is characterized in that: described conductive substrates is carbon felt, graphite paper or carbon cloth.
4. anode of microbial fuel cell according to claim 2 is characterized in that: described catalyst layer is the mixture of nickel-molybdenum carbide and adhesive.
5. anode of microbial fuel cell according to claim 4 is characterized in that: the mass content of described binding agent in mixture is 6%-48%.
6. anode of microbial fuel cell according to claim 4 is characterized in that: described binding agent is any one or the two or more mixture among polytetrafluoroethylene, polyvinylidene fluoride or the Nafion.
7. according to the preparation method of each described anode of microbial fuel cell among the claim 3-6, it is characterized in that may further comprise the steps:
(1) preparation nickel-molybdenum carbide;
(2) with nickel-molybdenum carbide and binding agent mixing;
(3) be applied in pasty mixture on the conductive substrates equably;
(4) oven dry.
8. preparation method according to claim 7 is characterized in that: the described nickel-molybdenum carbide for preparing of step (1) adopts following method:
(1) with molybdic acid and NiCl
26H
2O is Ni in molar ratio: Mo=1: 1-1: 3 are dissolved in the ethylene glycol, and brute force is stirred to NiCl in 60-80 ℃
26H
2O dissolves fully; Then, Mo: C=1: 2-1 in molar ratio: 4 add carbon sources; After carbon source is heated dissolving, stir solvent, about 100-130 ℃, be condensed into the solvent of viscosity, form the parent fragment when again the solvent of viscosity being heated to 150-190 ℃;
(2) the parent fragment is placed in the inherent alumina tube furnace of graphite boat and anneals, and temperature is 800-900 ℃, and under inert gas shielding, annealing time is 2-4h; Be cooled to room temperature, promptly prepared navy blue nickel-molybdenum carbide sample powder.
9. a microbiological fuel cell comprises anode chamber, film negative electrode and external circuit three parts, and the anode chamber comprises anolyte, anode and electrogenesis microbe, it is characterized in that: described anode is each described anode of microbial fuel cell of claim 2-6.
10. microbiological fuel cell according to claim 9 is characterized in that: described negative electrode is the Pt/C negative electrode.
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Cited By (7)
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| CN105336964A (en) * | 2015-07-03 | 2016-02-17 | 同济大学 | Nitrogen-doped carbon nanotube/ carbonitride composite material preparation method and application |
| CN105642326A (en) * | 2016-01-28 | 2016-06-08 | 中国科学技术大学 | Porous-carbon loaded metal composite material and preparing method and application thereof |
| CN107164779A (en) * | 2017-04-10 | 2017-09-15 | 华东理工大学 | It is a kind of to be carried on nickel molybdenum base bimetallic carbide of nickel foam and its preparation method and application |
| CN107665996A (en) * | 2017-09-22 | 2018-02-06 | 常州信息职业技术学院 | Three-dimensional porous nickel doughnut electrode material, preparation method and the battery based on the electrode |
| CN108172852A (en) * | 2018-01-29 | 2018-06-15 | 广东工业大学 | A kind of anode of microbial fuel cell, preparation method and microbiological fuel cell |
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| CN105642326B (en) * | 2016-01-28 | 2018-09-07 | 中国科学技术大学 | A kind of porous carbon carried metal composite material and preparation method and application |
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| CN107665996A (en) * | 2017-09-22 | 2018-02-06 | 常州信息职业技术学院 | Three-dimensional porous nickel doughnut electrode material, preparation method and the battery based on the electrode |
| CN108172852A (en) * | 2018-01-29 | 2018-06-15 | 广东工业大学 | A kind of anode of microbial fuel cell, preparation method and microbiological fuel cell |
| CN109136973A (en) * | 2018-08-28 | 2019-01-04 | 南京工业大学 | A kind of base metal doping molybdenum carbide hydrogen-precipitating electrode and its preparation method and application |
| CN109136973B (en) * | 2018-08-28 | 2020-07-14 | 南京工业大学 | Non-noble metal doped molybdenum carbide hydrogen evolution electrode and preparation method and application thereof |
| CN113952961A (en) * | 2021-11-29 | 2022-01-21 | 重庆市三峡鱼复排水有限责任公司 | Preparation method of novel nickel-molybdenum alloy nanoparticles and method for treating wastewater by using novel nickel-molybdenum alloy nanoparticles |
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| CN101752569B (en) | 2011-12-14 |
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