CN106784829A - A kind of preparation method for loading Graphene and the anode of microbial fuel cell of ferrous disulfide compound - Google Patents
A kind of preparation method for loading Graphene and the anode of microbial fuel cell of ferrous disulfide compound Download PDFInfo
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- CN106784829A CN106784829A CN201710015899.8A CN201710015899A CN106784829A CN 106784829 A CN106784829 A CN 106784829A CN 201710015899 A CN201710015899 A CN 201710015899A CN 106784829 A CN106784829 A CN 106784829A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
A kind of preparation method for loading Graphene and the anode of microbial fuel cell of ferrous disulfide compound, belongs to environment, material, energy field, and methods described step is as follows：（1）Ferric trichloride and thiourea solution are dropwise instilled in the graphene oxide dispersion in reactor, stirred, sealed reactor, the h of hydro-thermal reaction 12 ~ 24 between temperature is for 140 DEG C ~ 200 DEG C obtains hydrogel sample；（2）Hydrogel sample is washed with deionized for several times, is crushed after freeze-drying and is obtained Graphene and ferrous disulfide compound nano-powder；（3）By Nafion solution that nano-powder and concentration are 5% and isopropanol, deionized water mix concussion it is uniform after, be coated on carbon cloth, carbon cloth is fixed with fixture, and carbon cloth dries prepared anode.It is an advantage of the invention that synthesis step very simple, obtains particle morphology uniformly, graphene sheet layer is stacked to form pore structure prosperity, chemical property and good biocompatibility, and good performance is obtained in that as the anode of microbiological fuel cell.
Description
Technical field
The invention belongs to environment, material, energy field, and in particular to one kind load Graphene and ferrous disulfide compound
Anode of microbial fuel cell preparation method.
Background technology
Microbiological fuel cell is a kind of emerging bioelectrochemistry technology, and it can be produced while degradation of organic substances
Electric energy.This makes it be had broad application prospects on the fields such as sewage disposal, restoration of the ecosystem and bioenergy.In microorganism
In fuel cell, the electricity-producing microorganism metabolism of anode attachment produces extracellular electronics, will by electron medium or nm-class conducting wire etc.
, to anode, electronics reaches negative electrode through external circuit and electron acceptor occurs reduction reaction for electron transmission.Electricity-producing microorganism is micro- life
The core of thing fuel cell, anode as electricity-producing microorganism carrier, its material character significantly affect microorganism metabolism and
Extracellular electron transfer process.The anode of microbiological fuel cell is gone back in addition to needing to meet the requirement of traditional chemical battery electrode
Good biocompatibility is needed to have, beneficial to bacterial load and promotes electro transfer, this is proposed to traditional electrode material
Challenge.In order that anode can preferably play a role, researcher attempts being modified on traditional anode material, reaches
Improve its specific surface area and then increase the adhesion amount of bacterium, improve the purpose of its biocompatibility and electron transmission ability.So
And most of materials there are problems that synthesis program complexity, severe reaction conditions, therefore, find one kind be easy to large quantities of
Amount synthesis, the material of good biocompatibility is extremely urgent.
The content of the invention
The invention aims to overcome the deficiencies in the prior art, there is provided one kind load Graphene and curing
The preparation method of the microbiological fuel cell of iron complexes.Under hydrothermal conditions, fabricated in situ Graphene is combined with ferrous disulfide
Thing, ferrous disulfide nano particle uniform load is on graphene sheet layer.Graphene fold in itself formation duct have it is larger
Specific surface area, beneficial to the growth of microorganism.The compound of synthesis mixes by lyophilized, crushing with binding agent, is coated in collector
（Anode surface）On, obtain the anode of microbiological fuel cell.
To achieve the above object, the technical scheme taken is as follows for the present invention：
A kind of preparation method for loading Graphene and the anode of microbial fuel cell of ferrous disulfide compound, methods described is specific
Step is as follows：
Step one：During ferric trichloride and thiourea solution dropwise to instill the graphene oxide dispersion in reactor, and stir equal
After even, sealed reactor, the h of hydro-thermal reaction 12 ~ 24 between temperature is for 140 DEG C ~ 200 DEG C obtains hydrogel sample；
Step 2：The hydrogel sample is washed with deionized for several times, is crushed after freeze-drying and is obtained Graphene and two sulphur
Change iron complexes nano-powder；
Step 3：Nafion solution that the nano-powder and concentration are 5% and isopropanol, deionized water are mixed into concussion equal
After even, it is coated on carbon cloth, carbon cloth is fixed with fixture, carbon cloth is obtained anode after drying.
In the present invention, 5% Nafion solution is binding agent, can also be using PTFE aqueous dispersions, PDMS etc. as bonding
Agent；
In the present invention, using carbon cloth as anode substrate, can also be using carbon paper or carbon felt as anode substrate.
The present invention is relative to the beneficial effect of prior art：（1）One step fabricated in situ Graphene is combined with ferrous disulfide
Thing modifies traditional anode, makes full use of Graphene high-specific surface area and ferrous disulfide to carry out the compatibility of extracellular electricity production bacterium
The performance of microbiological fuel cell is improved, anode current transfger impedance is reduced, is accelerated microbiological fuel cell and is started and improve
Power output；（2）The synthesis step ten for being particularly advantageous in that electrode applicator Graphene and ferrous disulfide compound of this method
Divide simple, obtain particle morphology uniformly, graphene sheet layer stacks to form pore structure prosperity, chemical property and bio-compatible are good,
Good performance is obtained in that as the anode of microbiological fuel cell；（3）Prepared anode is applied to various types of micro-
Biological fuel cell includes microbiological fuel cell, edaphon fuel cell and the phytomicroorganism fuel electricity of aqueous medium
Pond etc., and it is not only restricted to the configuration of microbiological fuel cell and the type of cathode electronics acceptor；（4）It is graphene coated with
Its electro transfer impedance of the electrode of ferrous disulfide compound is not significantly less than doing the collector modified and only coat oxygen reduction
The electrode of graphite alkene.
To sum up, the present invention relates to a kind of adjustable ferrous disulfide of ratio and the anode of microbial fuel cell of graphene complex
Preparation method.The method obtains the gas of different mechanical strengths based on hydro-thermal method simple and easy to get, by the ratio of raw material
Gel load prepares anode of microbial fuel cell on a current collector.The method technique is simple and easy to do, sufficient raw, gained
The particle size range of the middle ferrous disulfide nano particle of ferrous disulfide and graphene aerogel between the nm of 10 nm to 90, average chi
Very little is 37 nm, and in the case of unsupported microorganism, electro transfer impedance is in 12 Ω, the electricity of loading microorganisms for the anode of preparation
Sub- transfger impedance is in 66 Ω.Graphene is prepared in the present invention has flourishing loose structure, particle shape with ferrous disulfide compound
Looks are uniform, and the electrode of modification has good electro-chemical activity.Due to prepared load Graphene and ferrous disulfide compound
Anode have specific surface area higher, preferable biocompatibility and chemical property, be used as various types of negative electrodes
Microbiological fuel cell anode, be adapted to mixed bacterial and it is various it is extracellular electricity production bacterium pure bacterium load growth.This method it is aobvious
Work advantage is simple its electrode fabrication step, and the material of coating is readily synthesized, and the anode of preparation is adapted to growth of microorganism, can
Accelerating microbiological fuel cell can start and obtain voltage and power density higher.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrogram of Graphene and ferrous disulfide compound；
Fig. 2 is the biomembrane scanning electron microscope diagram of Graphene and growth on ferrous disulfide compound and the anode of preparation；
Fig. 3 is Graphene and ferrous disulfide compound transmission electron microscope figure；
Fig. 4 is that the anode for preparing be not inoculated with and is loading the AC impedance figure of biomembrane；
Fig. 5 is the power density curve map of the battery of assembling.
Specific embodiment
Technical scheme is further described with reference to the accompanying drawings and examples, but is not limited thereto,
It is every technical scheme to be modified or equivalent, without deviating from the spirit and model of technical solution of the present invention
Enclose, all should cover in protection scope of the present invention.
Specific embodiment one：A kind of preparation side for loading Graphene and the anode of microbial fuel cell of ferrous disulfide compound
Method, methods described is comprised the following steps that：
Step one：During ferric trichloride and thiourea solution dropwise to instill the graphene oxide dispersion in reactor, and stir equal
After even, sealed reactor is 140 DEG C ~ 200 DEG C in temperature（Optimum temperature is 180oC）Between hydro-thermal reaction 12 ~ 24 h hours
（Optimum reacting time is 12 h）, obtain hydrogel sample；
Step 2：The hydrogel sample is washed with deionized for several times, is crushed after freeze-drying and is obtained Graphene and two sulphur
Change iron complexes nano-powder；X-ray crystal diffraction test is carried out to it, ferrous disulfide can be learnt for marcasite and
Two kinds of crystal formations of pyrite（Fig. 1）；It can be seen that complicated rich from the Graphene for preparing with ferrous disulfide compound scanning electron microscope (SEM) photograph
Rich Graphene duct（Fig. 2 Image to lefts）；As can be seen that in gained ferrous disulfide and graphene aerogel from transmission electron microscope
Between 10nm to 90nm, average grain diameter is 37nm (Fig. 3) to the particle size range of ferrous disulfide nano particle.
Step 3：Nafion solution that the nano-powder and concentration are 5% and isopropanol, deionized water are mixed into shake
After swinging uniformly, it is coated on carbon cloth, carbon cloth is fixed with fixture, carbon cloth is obtained anode after drying（Can also be coated in carbon paper or
In carbon felt）.
With the anode assembling dual chamber for preparing（100mL/ rooms）Microbiological fuel cell investigates anode performance, with hydrothermal reduction
Carbon cloth anode and compareed without the carbon cloth anode for passing through modification that redox graphene is modified, find its maximum for obtaining
Power density（3.5W/cm2）It is significantly higher than carbon cloth anode（2.8W/cm2）With the anode of coating redox graphene（3.2W/
cm2）（Fig. 5）, a thick layer of biomembrane is covered on electrode（Fig. 2 Image to rights）.The ripe anode of biomembrane is exchanged
Impedance measuring, load Graphene is 66 Ω with the carbon cloth anode current transfger impedance of ferrous disulfide compound, significantly less than simple
Load the carbon cloth anode (129 Ω) of Graphene（Fig. 4）.
Specific embodiment two：A kind of load Graphene described in specific embodiment one is micro- with ferrous disulfide compound
The preparation method of biological fuel cell anode, in step one, ferric trichloride is 6.8 with the mol ratio of thiocarbamide:5, thiocarbamide quality is
The 2.0*10 of graphene oxide quality3Times.
Specific embodiment three：A kind of load Graphene described in specific embodiment one is micro- with ferrous disulfide compound
The preparation method of biological fuel cell anode, in step 3, every milligram of nano-powder uses the Nafion solution of 7.5 μ L5%
（Binding agent）, isopropanol and deionized water be no less than Nafion solution volume 1/2 and 1/7 respectively, and can be suitable according to actual conditions
Amount increases.
Specific embodiment four：A kind of load Graphene described in specific embodiment one is micro- with ferrous disulfide compound
The preparation method of biological fuel cell anode, in step one, at 140 DEG C ~ 200 DEG C（Optimum temperature is 180oC）Under hydrothermal condition,
In 12 ~ 24 h reaction time, ferric trichloride and thiourea solution reaction generate ferrous disulfide, generation and the oxidation of the ferrous disulfide
The reduction of Graphene is synchronous carrying out.
Specific embodiment five：A kind of load Graphene described in specific embodiment one is micro- with ferrous disulfide compound
The preparation method of biological fuel cell anode, in step one, the substitute of sulphur source is other in hydro-thermal bar in the thiourea solution
S can be discharged under part2-Sulphur source.
Specific embodiment six：A kind of load Graphene described in specific embodiment one is micro- with ferrous disulfide compound
The preparation method of biological fuel cell anode, in step 3, described fixture is wire or electrode holder.
Specific embodiment seven：A kind of load Graphene described in specific embodiment six is micro- with ferrous disulfide compound
The preparation method of biological fuel cell anode, in step 3, described wire is titanium silk.
（Other can also be selected stable in properties in anolyte and dissolved on a small quantity substantially not poison microorganism
In the wire or electrode holder of effect it is a kind of come fixed anode）.
Embodiment 1
What the present embodiment was recorded is a kind of preparation for loading Graphene and the anode of microbial fuel cell of ferrous disulfide compound
Method, methods described is comprised the concrete steps that：
Step one；Under conditions of stirring, the trichlorine that dropwise addition is pre-mixed in pre-synthesis graphene oxide dispersion
Change iron and thiourea solution, using the reactor of 23 mL, total liquid volume is 17.5 mL in reactor, and stone is aoxidized containing 42 mg
Black alkene, 0.675 g FeCl3·6H2O、0.19 g (NH2)2CS, 12 h are reacted at 180 DEG C, and graphene oxide is in hydrothermal condition
Under be reduced to redox graphene.Other equations being related to during this are：
(NH2)2CS + 2H2O = CO2 + H2S + 2NH3
2Fe3+ + 2S2-= FeS2 + Fe2+
After reaction by hydrogel sample with deionized water washing by soaking for several times, after freeze-drying crush, obtain Graphene and two sulphur
Change iron nano sized powder sample；The Graphene of generation and the mechanical strength of ferrous disulfide compound hydrogel form are found through overtesting
Difference, is anode assembling microbiological fuel cell with it, and hydrogel can gradually expand finished breaking after bacterial load growth, therefore
The anode for preparing microbiological fuel cell is coated on traditional anode material as decorative material using the compound is crushed.
Step 2：Graphene and ferrous disulfide compound after 4 mg grindings are weighed in centrifuge tube, 15 μ L isopropyls are added
Alcohol, the Nafion solutions of 30 μ L 5%, 4 μ L deionized waters are mixed, and be vortexed concussion, and being coated in titanium silk with paintbrush fixes 1 cm2
Carbon cloth on, dry after be obtained anode.
Step 3：The x-ray diffractometers of RIGAKU D/Max 3400 are respectively adopted：Cu-K α/40KV/100mA, analyze sample
Product crystal structure and thing phase；Hitachi S-4800 type SEM（SEM）With the type transmitted electrons of ZEISS LEO 922
Microscope（TEM）, observe the pattern and pore structure of nano-particle.Using the SI1287 electrochemical operations of AMETEK Solartron
Stand with SI1260 impedances instrument to determine the AC impedance of electrode；Battery voltage acquisition is recorded：The type data acquisitions of Keithley 2700
Device.
Embodiment 2：
It is the stainless steel outer sleeve of 23 mL, the reactor of polytetrafluoroethyllining lining that reaction in the present embodiment uses total working volume,
According to the graphene oxide concentration for determining to graphene oxide is added dropwise in reactor, while adding liquor ferri trichloridi and thiocarbamide
Solution, the concentration according to graphene oxide determines the concentration of liquor ferri trichloridi and thiourea solution.Total liquid volume in reactor
It is 17.5 mL, contains 21mg GO, 0.675 g FeCl3·6H2O、0.19 g (NH2)2CS.Reactor is put into electric heating air blast
Drying box, 12 h is reacted at 180 DEG C and obtains hydrogel product, standby after for several times with deionized water washing by soaking.Remaining step
It is same as Example 1.
The anode for preparing is suitable for the microbiological fuel cell of seeded with pure bacterium and mixed bacteria, and does not receive battery
The limitation of configuration and anode and cathode electrolyte.
Embodiment 3：
Reference implementation example 2, according to the graphene oxide concentration for determining to quantitative graphene oxide is added dropwise in reactor, while
Add FeCl3Solution and (NH2)2CS solution, adds deionized water, it is ensured that total liquid volume is 17.5 mL in reactor, and is contained
There are 21 mg GO, 0.675 g FeCl3·6H2O、0.19 g (NH2)2CS.Reactor is put into electric drying oven with forced convection,
12 h are reacted at 180 DEG C and obtains hydrogel product, it is standby after for several times with deionized water washing by soaking.
The Graphene that will be made is put into -80 DEG C of min of ultra low temperature freezer precooling 30 with ferrous disulfide compound.After precooling
Graphene is put into lyophilized 12 h of freeze drier with ferrous disulfide compound.Weigh the Graphene and ferrous disulfide after 8 mg grindings
Compound adds 30 μ L isopropanols, the Nafion solutions of 60 μ L 5%, 8 μ L deionized waters to be mixed in centrifuge tube, its
Middle isopropanol and deionized water can appropriate dosages.30 min are shaken up on vortex mixer.1 is fixed with the titanium silk of the mm of diameter 0.3
cm2Carbon cloth, with paintbrush by mixed suspension uniform application on carbon cloth two sides, 30 DEG C of oven for drying are standby.
Embodiment 4：
Reference implementation example 2, the fixed form of electrode is to be fixed instead of titanium silk using conventional stainless steel electrode folder in this example
Anode.
Embodiment 5：
Reference implementation example 2, weighs the Graphene after 40 mg grindings with ferrous disulfide compound in centrifuge tube in this example, plus
Enter 150 μ L isopropanols, the Nafion solutions of 300 μ L 5%, 40 μ L deionized waters to be mixed, wherein isopropanol and deionization
Water can appropriate dosage.30 min are shaken up on vortex mixer.1 cm is fixed with the titanium silk of the mm of diameter 0.32Carbon felt, with drop
Pipe is dropwise added dropwise a small amount of mixed liquor to carbon felt, dries, and repeats the step and exhausts mixed liquor, and anode is obtained.
Embodiment 6：
Reference implementation example 2, to react in this example and obtain hydrogel product carrying out 18 h at 160 DEG C.
Claims (7)
1. a kind of preparation method of the anode of microbial fuel cell for loading Graphene and ferrous disulfide compound, its feature exists
In：Methods described is comprised the following steps that：
Step one：During ferric trichloride and thiourea solution dropwise to instill the graphene oxide dispersion in reactor, and stir equal
After even, sealed reactor, hydro-thermal reaction 12 ~ 24 h hours, obtains hydrogel sample between temperature is for 140 DEG C ~ 200 DEG C；
Step 2：The hydrogel sample is washed with deionized for several times, is crushed after freeze-drying and is obtained Graphene and two sulphur
Change iron complexes nano-powder；
Step 3：Nafion solution that the nano-powder and concentration are 5% and isopropanol, deionized water are mixed into concussion equal
After even, it is coated on carbon cloth, carbon cloth is fixed with fixture, carbon cloth is obtained anode after drying.
2. a kind of Graphene that loads according to claim 1 is with the anode of microbial fuel cell of ferrous disulfide compound
Preparation method, it is characterised in that：In step one, ferric trichloride is 6.8 with the mol ratio of thiocarbamide：5, thiocarbamide quality and graphite oxide
Alkene mass ratio is 2.0*103：1.
3. a kind of Graphene that loads according to claim 1 is with the anode of microbial fuel cell of ferrous disulfide compound
Preparation method, it is characterised in that：In step 3, every milligram of nano-powder uses the Nafion solution of 7.5 μ L5%（Bond
Agent）, isopropanol and deionized water be no less than Nafion solution volume 1/2 and 1/7 respectively.
4. a kind of anode of microbial fuel cell for loading Graphene and ferrous disulfide compound according to claim 1
Preparation method, it is characterised in that：In step one, under 140 DEG C ~ 200 DEG C hydrothermal conditions, in 12 ~ 24 h reaction time,
Ferric trichloride and thiourea solution reaction generation ferrous disulfide, the generation of the ferrous disulfide is synchronous with the reduction of graphene oxide
Carry out.
5. a kind of Graphene that loads according to claim 1 is with the anode of microbial fuel cell of ferrous disulfide compound
Preparation method, it is characterised in that：In step one, the substitute of sulphur source under hydrothermal conditions can for other in the thiourea solution
Release S2-Sulphur source.
6. a kind of Graphene that loads according to claim 1 is with the anode of microbial fuel cell of ferrous disulfide compound
Preparation method, it is characterised in that：In step 3, described fixture is wire or electrode holder.
7. a kind of Graphene that loads according to claim 6 is with the anode of microbial fuel cell of ferrous disulfide compound
Preparation method, it is characterised in that：In step 3, described wire is titanium silk.
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| CN107149935A (en) * | 2017-06-23 | 2017-09-12 | 哈尔滨工业大学 | A kind of preparation method of many iron sulfide of efficient out-phase class fenton catalyst core shell structure |
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| CN110823755A (en) * | 2019-11-19 | 2020-02-21 | 湖南博溥立材料科技有限公司 | Method for detecting anti-oxidation performance of coating material of prebaked electrolytic aluminum anode |
| CN111068718A (en) * | 2020-01-08 | 2020-04-28 | 济南大学 | Preparation of nano spherical sulfur-doped iron oxide and application of nano spherical sulfur-doped iron oxide in electrocatalytic nitrogen reduction |
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| CN111960477A (en) * | 2020-08-20 | 2020-11-20 | 辽宁科技大学 | Preparation method of all-solid-state supercapacitor electrode material |
| CN112086651A (en) * | 2020-09-21 | 2020-12-15 | 哈尔滨理工大学 | Synthetic method of WN-rGO nano particles and microbial fuel cell constructed by same |
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| CN114275822B (en) * | 2021-12-31 | 2023-12-22 | 吕梁学院 | Preparation method and application of iron-containing compound modified graphene nanocomposite with different morphologies and crystalline phases |
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