CN105762371B - A kind of biomass alkaline fuel cell anode and preparation method with electron transit mediator - Google Patents
A kind of biomass alkaline fuel cell anode and preparation method with electron transit mediator Download PDFInfo
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- CN105762371B CN105762371B CN201610237824.XA CN201610237824A CN105762371B CN 105762371 B CN105762371 B CN 105762371B CN 201610237824 A CN201610237824 A CN 201610237824A CN 105762371 B CN105762371 B CN 105762371B
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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- 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
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Abstract
The invention discloses a kind of biomass alkaline fuel cell anodes and preparation method with electron transit mediator, are prepared as：(1) water, ultrasonic disperse is added to filter to graphene film and carbon nanotube, it is dry, obtain mixed carrier GNPs CNTs；(2) mixed carrier and 2 hydroxyl Isosorbide-5-Nitrae naphthoquinones aqueous solutions are mixed, ethylene glycol is added, ultrasonic disperse is adjusted pH, ultrasonic disperse to heat, stood；It filters, washs, it is dry, obtain catalyst；(3) absolute ethyl alcohol is added in catalyst, ptfe emulsion, ultrasonic disperse is added in ultrasonic disperse；Stirring, obtains dope；Dope tiling is pressed into foam nickel surface, roll-in straticulation to get.The present invention prepares a kind of biomass alkaline fuel cell anode with electron transit mediator using cheap and easy to get and functional 2 hydroxyl Isosorbide-5-Nitrae naphthoquinones, and the electricity generation performance of battery can be made to greatly improve；Production cost can be reduced, the reaction time is shortened.
Description
Technical field
The invention belongs to field of fuel cell technology, particularly relate to a kind of biomass alkalinity with electron transit mediator
Anode of fuel cell and preparation method.
Background technology
Biomass alkaline fuel cell is a kind of will to be stored in biomass fuel and oxidant in alkaline environment
Chemical energy is converted into the device of electric energy by the redox reaction of anode and cathode.It has energy conversion efficiency it is high,
Environmental pollution is small, can for a long time continuously power supply, it is applied widely many advantages, such as, have become the hot spot in energy research field,
Receive the favor of many researchers.
Core component of the anode catalyst as biomass alkaline fuel cell has to improving battery performance and stability
Highly important effect.With the development of alkaline fuel cell, the catalyst for being used for anode is also greatly improved, such as
Pinchas Schechner et al. (Schechner P, Kroll E, Bubis E, Chervinsky S, Zussman E.J
Electrochem Soc 2007；154:B942-B948. anode) is made using silver-colored spindle fiber；L.An et al. (An L, Zhao
TS,Shen SY,Wu QX,Chen R.J Power Sources 2011；196:Cheap anion 186-190.) is used
Exchange membrane prevents oxygen from being reacted therewith by cathode arrival anode to improve battery performance；Cindy X.Zhao et al.
(Chen JY,Zhao CX,Zhi MM,Wang KW,Deng LL,Xu G.Electrochim Acta 2012；66:133-
138.) doing anode and cathode using the nickel foam that catalyst poisoning will not occur makes battery performance improve 6 times；Debika Basu etc.
People (Basu D, Basu S.Electrochim Acta 2010；55:5775-5779.) by platinum, rubidium, activated carbon through ultrasonic vibration
With anode is made after heating water bath；Jinyao Chen et al. (Chen JY, Zhao CX, Zhi MM, Wang KW, Deng LL,
Xu G.Electrochim Acta 2012；66:133-138.) anode will be made in silver load and nickel foam；But each is catalyzed
The shortcomings that agent has its own.First, although to make catalyst catalytic performance good for common noble metal such as gold, platinum, property also compared with
For stabilization, but it is expensive, it is impossible to be used in large-scale industrialization production, in addition research shows that these noble metals and its being easy
Catalytic site is lost by the intermediate product package of reaction process, and so that catalytic activity is reduced even and loses catalytic activity, this is also
It is usually described catalyst poisoning phenomenon.Although current research shows that the noble metals such as palladium, ruthenium can avoid catalyst poisoning asks
Topic, improves battery performance but still there are problems that in price.And for being concerned in recent years based on nano material
Elctro-catalyst nickel, nickel oxide, nickel hydroxide and other metallic additions nano material, such as carbon nanotube, graphene and Ti/
The materials such as TiO2 be used to make that anode catalyst is highly effective to improve battery performance, but its manufacture craft is more complex.At present
It is eager to explore a kind of non-precious metal catalyst that can be used in alkaline environment.Therefore, a kind of new electron transit mediator of research will
It, which is fixed on anode, will be seemed with to improve its performance for catalysis biomass alkaline fuel cell and be highly desirable.
Invention content
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of biomass alkalinity combustion with electron transit mediator
Expect galvanic anode.
Second object of the present invention is to provide a kind of biomass alkaline fuel cell anode with electron transit mediator
Preparation method.
Technical scheme of the present invention is summarized as follows:
A kind of preparation method of the biomass alkaline fuel cell anode with electron transit mediator, includes the following steps：
(1) it is 1 in mass ratio：4 ratio, weighs graphene film and carbon nanotube is placed in container, and distilled water is added, makes
Distilled water did not had graphene film and carbon nanotube, 25~30min of ultrasonic disperse to filter, and in 110 DEG C of dry 1h, obtains mixing and carries
Body, the graphene film are referred to as GNPs, and the carbon nanotube is referred to as CNTs, and the mixed carrier is referred to as GNPs-CNTs；
(2) it is 1 in mass ratio：1~2 ratio, the 2- of GNPs-CNTs and a concentration of 30mM hydroxyls-Isosorbide-5-Nitrae naphthoquinones is water-soluble
Liquid mixes, and ethylene glycol is added, and the ethylene glycol is 1-2 times of 2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones aqueous solution volume, and ultrasonic disperse 15~
20min adjusts pH to 8.5 with NaOH aqueous solutions, and 15~20min of ultrasonic disperse, is subsequently placed in 700W micro-wave ovens and heats again
5~10min is stood after 60s；It filters and is washed with distilled water, it is dry, it obtains 2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones and is supported on GNPs-CNTs
Catalyst；
(3) catalyst that step (2) obtains is placed in container, absolute ethyl alcohol is added, absolute ethyl alcohol is made not have described urge
Ptfe emulsion, the sum of the graphene film and carbon nanotube and polytetrafluoro is added in agent, 25~30min of ultrasonic disperse
The mass ratio of vac emulsion is 1：0.5~0.8,25~30min of ultrasonic disperse；It is warming up to 70-75 DEG C of stirring, obtains dope；
Dope tiling is pressed into foam nickel surface, 2~4mm thin layers are rolled on roll squeezer, are obtained with electron transit mediator
Biomass alkaline fuel cell anode.
A kind of biomass alkaline fuel cell anode with electron transit mediator prepared by the above method.
Advantages of the present invention：
1. the present invention prepares one kind using -1,4 naphthoquinones of electron transit mediator 2- hydroxyls cheap and easy to get and of good performance and carries
The biomass alkaline fuel cell anode of electron transit mediator, can be such that the electricity generation performance of biomass alkaline fuel cell greatly improves,
Suitable for large-scale production；
2. compared to the method that more traditional noble metal catalyst improves electric weak performance, galvanic anode used in the present invention can
Production cost is reduced, and shortens the reaction time, improves battery performance.
Description of the drawings
Fig. 1 is the power density curve graph of the biomass alkaline fuel cell corresponding to different anodes.
Fig. 2 is the electron transmission liquid solution various concentration of two kinds of better performances than corresponding power density curve.
Specific implementation mode
With reference to specific embodiment, the present invention is further illustrated.
Graphene film guide number Ps in each embodiment, carbon nanotube abbreviation CNTs, mixed carrier guide number Ps-CNTs；
It is pointed out in ptfe emulsion product introduction：Polytetrafluoroethylene solids content is in the left and right 60% (wt).
Embodiment 1
A kind of preparation method of the biomass alkaline fuel cell anode with electron transit mediator, includes the following steps：
(1) 0.2g GNPs and 0.8g CNTs accurately are weighed to be placed in beaker, distilled water is added, distilled water is made not have GNPs
And CNTs, ultrasonic disperse 30min, it filters, 110 DEG C of dry 1h, obtain mixed carrier GNPs-CNTs in baking oven；
(2) by GNPs-CNTs and a concentration of 30mM electron transit mediators aqueous solution according to mass ratio 1：1 be placed in beaker mix
It closes, ethylene glycol is added, ethylene glycol is 2 times, ultrasonic disperse 15min of electron transit mediator aqueous solution volume, with NaOH aqueous solution tune
PH to 8.5 is saved, again ultrasonic disperse 15min, is subsequently placed in after heating 60s in 700W micro-wave ovens and stands 10min；It filters and uses steaming
Distilled water is washed, dry, obtains the catalyst that electron transit mediator is supported on GNPs-CNTs；
Electron transit mediator is respectively：
Dimethyl diaminophenazine chloride, 2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones, 1,5- dichloroanthraquinone, methylene blue, anthraquinone, methyl viologen,
It is abbreviated as：NR- dimethyl diaminophenazine chlorides, NQ-2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones, DA-1,5- dichloroanthraquinones, MB- methylene blues, AQ- anthracenes
Quinone,
MV- methyl viologens, Bare- do not add any electron transit mediator, are replaced with the water of same volume；
(3) catalyst that step (2) obtains is placed in beaker, absolute ethyl alcohol is added, absolute ethyl alcohol is made not have described urge
Ptfe emulsion, the matter of the sum of the GNPs and CNTs and ptfe emulsion is added in agent, ultrasonic disperse 30min
Amount is than being 1：0.5, ultrasonic disperse 30min；75 DEG C of stirrings are warming up to, dope is obtained；Cut the circle of a diameter of 2cm or so
Dope tiling is pressed into foam nickel surface, 3mm thin layers is rolled on roll squeezer, obtains passing with electronics by shape nickel foam
Pass the biomass alkaline fuel cell anode of body.
Embodiment 2
The power density curve of alkaline fuel cell corresponding to different anodes
Fig. 1 show the power density curve of the battery corresponding to seven kinds of different anodes of the preparation of embodiment 1.Wherein Bare
Curve is the blank control group for not adding any electron transit mediator.To avoid error, each anode equal horizontal survey 3 times adds
Error line is added, has kept data more accurate and reliable.Battery used is dual chamber glucose fuel cell, and anode is respectively embodiment 1
The electrode of preparation, cathode are air diffusion electrode, and concentration of glucose is 1M in battery, and KOH concentration is 3M.In Fig. 1 in NR-
Red, the NQ-2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones of property, DA-1,5- dichloroanthraquinones, MB- methylene blues, AQ- anthraquinones, MV- methyl viologens, Bare-
Blank control group)
Power density is followed successively by 7.39W/m2、9.95W/m2、7.07W/m2、9.37W/m2、6.70W/m2、10.05W/m2With
4.56W/m2.As can be seen that compared with the blank control group for not adding any electron transit mediator, it is added to the sun of electron transit mediator
Pole can increase substantially battery performance, and wherein better performances is the anode for being added to 2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones and methyl viologen,
Its power density is respectively 9.95W/m2And 10.05W/m2.(MB- methylene blues are unstable).
Embodiment 3
The power density curve of alkaline fuel cell corresponding to different anodes
The electron transit mediator of two kinds of better performances is obtained from embodiment 2：2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones and methyl viologen, change it
Mass ratio with GNPs-CNTs, prepare anode also according to the method for embodiment 1.Fig. 2 a be GNPs-CNTs with it is a concentration of
The methyl viologen aqueous solution mass ratio of 30mM is respectively 1:1、1:2、1；Cell power density curve corresponding to 3, Fig. 2 b are
GNPs-CNTs and -1,4 naphthoquinones aqueous solution mass ratio of a concentration of 30mM2- hydroxyls are respectively 1:1、1:2、1:Battery corresponding to 3
Power density curve.To avoid error, each anode equal horizontal survey 3 times is added to error line, data is made more accurately may be used
It leans on.Battery used and embodiment 2 are identical.GNPs-CNTs and a concentration of 30mM crystal violets are can be seen that from the test result of Fig. 2
Smart aqueous solution mass ratio is respectively 1:1、1:2、1；Battery maximum power density corresponding to 3 is respectively 10.05W/m2、
17.95W/m2And 18.01W/m2；GNPs-CNTs and -1,4 naphthoquinones aqueous solution mass ratio of a concentration of 30mM2- hydroxyls are respectively 1:1、
1:2、1:Battery maximum power density corresponding to 3 distinguishes 9.95W/m2、16.10W/m2And 4.26W/m2。
Methyl viologen also has ecological environment prodigious harmfulness, therefore studies have shown that Viologen Compounds have toxicity
Without protection.
2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones is a kind of ancient natural dye, can be extracted from plant, and in chemical constitution, it is
One unique small molecule is free of ionic group, is defined according to the international convention of persistence chemicals, belongs to degradable in soil
Organic matter.
Embodiment 4
A kind of preparation method of the biomass alkaline fuel cell anode with electron transit mediator, includes the following steps：
(1) 0.2g GNPs and 0.8g CNTs accurately are weighed to be placed in beaker, distilled water is added, distilled water is made not have GNPs
And CNTs, ultrasonic disperse 25min, it filters, 110 DEG C of dry 1h, obtain mixed carrier GNPs-CNTs in baking oven；
(2) by GNPs-CNTs and -1,4 naphthoquinones aqueous solution of a concentration of 30mM2- hydroxyls according to mass ratio 1：1 is placed in beaker
Ethylene glycol is added in mixing, and ethylene glycol is 1 times, ultrasonic disperse 18min of 2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones water volume, with NaOH aqueous solutions
PH to 8.5 is adjusted, again ultrasonic disperse 18min, is subsequently placed in after heating 60s in 700W micro-wave ovens and stands 5min；It filters and is used in combination
Water washing is distilled, it is dry, obtain the catalyst that 2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones is supported on GNPs-CNTs；
(3) catalyst that step (2) obtains is placed in beaker, absolute ethyl alcohol is added, absolute ethyl alcohol is made not have described urge
Ptfe emulsion, the matter of the sum of the GNPs and CNTs and ptfe emulsion is added in agent, ultrasonic disperse 25min
Amount is than being 1：0.7, ultrasonic disperse 25min；70 DEG C of stirrings are warming up to, dope is obtained；Cut the circle of a diameter of 2cm or so
Dope tiling is pressed into foam nickel surface, 2mm thin layers is rolled on roll squeezer, obtains passing with electronics by shape nickel foam
Pass the biomass alkaline fuel cell anode of body.
Embodiment 5
A kind of preparation method of the biomass alkaline fuel cell anode with electron transit mediator, includes the following steps：
(1) 0.2g GNPs and 0.8g CNTs accurately are weighed to be placed in beaker, distilled water is added, distilled water is made not have GNPs
And CNTs, ultrasonic disperse 28min, it filters, 110 DEG C of dry 1h, obtain mixed carrier GNPs-CNTs in baking oven；
(2) by GNPs-CNTs and -1,4 naphthoquinones aqueous solution of a concentration of 30mM2- hydroxyls according to mass ratio 1：1 is placed in beaker
Ethylene glycol is added in mixing, and ethylene glycol is 1.5 times of 2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones water volume, ultrasonic disperse 20min, water-soluble with NaOH
Liquid adjusts pH to 8.5, again ultrasonic disperse 20min, is subsequently placed in after heating 60s in 700W micro-wave ovens and stands 8min；It filters simultaneously
It is washed with distilled water, it is dry, obtain the catalyst that 2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones is supported on GNPs-CNTs；
(3) catalyst that step (2) obtains is placed in beaker, absolute ethyl alcohol is added, absolute ethyl alcohol is made not have described urge
Ptfe emulsion, the matter of the sum of the GNPs and CNTs and ptfe emulsion is added in agent, ultrasonic disperse 28min
Amount is than being 1：0.8, ultrasonic disperse 28min；73 DEG C of stirrings are warming up to, dope is obtained；Cut the circle of a diameter of 2cm or so
Dope tiling is pressed into foam nickel surface, 4mm thin layers is rolled on roll squeezer, obtains passing with electronics by shape nickel foam
Pass the biomass alkaline fuel cell anode of body.
It is demonstrated experimentally that the power density of the biomass alkaline fuel cell anode with electron transit mediator of embodiment 4,5
With the biomass alkaline fuel cell anode with electron transit mediator (electron transit mediator is -1,4 naphthoquinones of 2- hydroxyls) of embodiment 1
Power density it is close.
Claims (2)
1. a kind of preparation method of the biomass alkaline fuel cell anode with electron transit mediator, it is characterized in that including following step
Suddenly：
(1) it is 1 in mass ratio：4 ratio, weighs graphene film and carbon nanotube is placed in container, and distilled water is added, makes distillation
Water did not had graphene film and carbon nanotube, 25~30min of ultrasonic disperse to filter, dry, obtained mixed carrier, the graphene
Piece is referred to as GNPs, and the carbon nanotube is referred to as CNTs, and the mixed carrier is referred to as GNPs-CNTs；
(2) it is 1 in mass ratio：1~2 ratio mixes the 2- of GNPs-CNTs and a concentration of 30mM hydroxyls-Isosorbide-5-Nitrae naphthoquinones aqueous solution
It closes, ethylene glycol is added, the volume of the ethylene glycol is 1-2 times of 2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones aqueous solution volume, ultrasonic disperse 15~
20min adjusts pH to 8.5, again 15~20min of ultrasonic disperse, be subsequently placed in 700W micro-wave ovens after heating 60s and stand 5~
10min；It filters and is washed with distilled water, it is dry, obtain the catalyst that 2- hydroxyls-Isosorbide-5-Nitrae naphthoquinones is supported on GNPs-CNTs；
(3) catalyst that step (2) obtains is placed in container, absolute ethyl alcohol is added, absolute ethyl alcohol is made not have the catalyst,
Ptfe emulsion, the sum of the graphene film and carbon nanotube and polytetrafluoroethylene (PTFE) breast is added in 25~30min of ultrasonic disperse
The mass ratio of liquid is 1：0.5~0.8,25~30min of ultrasonic disperse；It is warming up to 70-75 DEG C of stirring, obtains dope；It will be sticky
Object tiling is pressed into foam nickel surface, and 2~4mm thin layers are rolled on roll squeezer, obtains the biomass with electron transit mediator
Alkaline fuel cell anode.
2. a kind of biomass alkaline fuel cell anode with electron transit mediator prepared by method of claim 1.
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| CN107895800B (en) * | 2017-10-24 | 2020-08-25 | 天津大学 | Method for preparing electrodeposited cobalt activated carbon anode by one-step method |
| CN109585886B (en) * | 2018-10-10 | 2021-12-07 | 天津大学 | Device and method for treating organic waste and using organic waste for power generation of alkaline fuel cell |
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| CN103286318A (en) * | 2013-04-03 | 2013-09-11 | 华中科技大学 | Preparation method of nano precious metal-carbon nano tube-graphene composite and nano precious metal-carbon nano tube-graphene composite product |
| CN104538641A (en) * | 2014-12-25 | 2015-04-22 | 天津大学 | Carbohydrate alkaline fuel cell anode and manufacturing method of carbohydrate alkaline fuel cell anode |
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2016
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|---|---|---|---|---|
| CN103286318A (en) * | 2013-04-03 | 2013-09-11 | 华中科技大学 | Preparation method of nano precious metal-carbon nano tube-graphene composite and nano precious metal-carbon nano tube-graphene composite product |
| CN104538641A (en) * | 2014-12-25 | 2015-04-22 | 天津大学 | Carbohydrate alkaline fuel cell anode and manufacturing method of carbohydrate alkaline fuel cell anode |
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| Hanyu Wang et al..High power density microbial fuel cell with flexible 3D graphene–nickel foam as anode.《Nanoscale》.2013,第5卷10283–10290. * |
| Three-Dimensional Graphene-Carbon Nanotube Hybrid for High-Performance Enzymatic Biofuel Cells;Kenath Priyanka Prasad et al.;《ACSAppl.Mater.Interfaces》;20140217;第6卷;第3387-3393页 * |
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