CN109761235A - A kind of synthetic method of biological material walnut shell carbon material nitrating and its application in terms of anode of microbial fuel cell - Google Patents
A kind of synthetic method of biological material walnut shell carbon material nitrating and its application in terms of anode of microbial fuel cell Download PDFInfo
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- CN109761235A CN109761235A CN201811294045.9A CN201811294045A CN109761235A CN 109761235 A CN109761235 A CN 109761235A CN 201811294045 A CN201811294045 A CN 201811294045A CN 109761235 A CN109761235 A CN 109761235A
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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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- 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
Abstract
The invention discloses a kind of synthetic method of biological material walnut shell carbon material nitrating and its applications in terms of anode of microbial fuel cell, step is to wash walnut shell, it dries and is crushed, broken walnut shell is activated in the aqueous solution of activator, it then takes out and dries, by the high-temperature calcination under inert gas range of dried product, by the product acid elution after carbonization, it is washed with deionized again until neutral, product after washing is dry, obtain walnut shell carbon material, carbon material is fully ground from different urea, a small amount of deionized water is added to be stirred and dry at room temperature, by mixture high-temperature calcination under an inert gas, the extra unreacted urea of filtering and washing, obtain nitrogen-doped carbon material.Advantages of the present invention: using walnut shell as carbon source, urea is nitrogen source, has preferable biocompatibility and biggish specific surface area, reduces anode activation overpotential, and microbiological fuel cell power density significantly improves.
Description
Technical field
The present invention relates to material science and technology fields, more particularly to a kind of biological material walnut shell carbon material nitrating
Synthetic method and its application in terms of anode of microbial fuel cell.
Background technique
With the excessive development and utilization of fossil energy, non-renewable resources and the energy are increasingly in short supply, appoint of heap of stone depend on for existence
Ecological environment increasingly deteriorates, and energy crisis is extremely urgent with problem of environmental pollution.In face of such situation, countries in the world are all to clear
The development of clean, reproducible green energy resource proposes more urgent requirement.Microbiological fuel cell (Microbial Fuel
Cells, MFCs) it is one and can be realized the device that energy is converted and has production capacity, it can will contain in complicated organic biomass
Chemical energy is converted into electric energy, therefore causes global extensive concern.
Biomass carbon material is using the renewable waste such as stalk, corncob, rice husk, sawdust as raw material, in the item of anoxic
A kind of carbon material prepared under part, and it is widely used in the industries such as catalysis, biological culture and environmental protection.Biomass carbon materials
The emerging development of material because its with big specific surface area, the chemical property of temperature, good conductivity, prepare it is simple and cheap etc.
Advantage, using with good prospect in terms of microbiological fuel cell.
Castoff walnut shell is utilized herein, by synthesizing Biomass with easy steps such as uric acid mixing high temperature cabonizations
Nitrating carbon material is applied to anode of microbial fuel cell, and nitrating carbon material N-C is because it is with good biocompatibility
And biggish specific surface area, the attachment for not only improving anode electricity-producing microorganism reduces anode activation overpotential again, so that micro- life
The electricity production power density of object fuel cell significantly improves.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of synthesis of biological material walnut shell carbon material nitrating
Method and its application in terms of anode of microbial fuel cell are directly biomass source using walnut shell, pass through simple carbon
The method being combined to prepares the miscellaneous carbon material of nitrating, and the N-C material of preparation is used as to the electrode material of microbiological fuel cell,
So that microorganism generates higher electric energy.
The present invention adopts the following technical scheme: a kind of synthetic method of biological material walnut shell carbon material nitrating, including
Following steps,
1), walnut shell is washed, dries and is crushed；
2) broken walnut shell is activated in the aqueous solution of activator, then take out and is dried；
3) it, by the high-temperature calcination under inert gas range of dried product, by the product acid elution after carbonization, then uses
Deionized water washing is dry by the product after washing until neutrality, obtains walnut shell carbon material；
4) carbon material is fully ground from different urea, a small amount of deionized water is added and is stirred and dries at room temperature；
5), by mixture high-temperature calcination under an inert gas, the extra unreacted urea of filtering and washing obtains nitrogen-doped carbon
Material.
Preferably, activator described in step 2) is ZnCl2Solution, the ZnCl2Solution concentration is 5mol/L, institute
The temperature for stating activation processing is 180 DEG C, and the activation processing time is 12h.
Preferably, it is 600 DEG C, 800 DEG C, 1000 DEG C, heating that the condition of the step 3) high temperature cabonization, which is carburizing temperature,
Rate is 5 DEG C/min, and the condition of high temperature cabonization is that carbonization time is 2h, and the inert gas is N2Or Ar, the hydrochloric acid are dense
Degree is 1mol/L.
Preferably, the mass ratio of carbon material and urea described in step 4) is 1:2,1:5,1:8.
Preferably, temperature described in step 5) be 600 DEG C, 800 DEG C, 1000 DEG C, the heating rate be 10 DEG C/
Min, the extra urea deionized water of the washing.
A kind of biomass nitrogen-doped carbon material is applied in anode of microbial fuel cell, is included the following steps,
A, by the nitrogen-doped carbon material obtained by any preparation method of claim 1 to 6 and corresponding solvent
Adhesive is made by mixing into slurries and is coated in long 2cm, on the carbon cloth of wide 1cm, anode of microbial fuel cell is fabricated to, with common carbon
Cloth electrode is assembled in together in same anode chamber；
B, use carbon brush as microorganism fuel cell cathode, two pole room of yin-yang is linked by proton exchange membrane and is built into
For H-type microbial fuel cell unit, temperature is 28 DEG C~35 DEG C, configures good corresponding microorganism growth-promoting media and is injected into anode chamber
In and catholyte injection cathode chamber in；
C, link voltage data collector, the external resistance voltage value of acquisition in machine every five minutes, according to external resistance voltage
The variation of value regularly replaces catholyte and anolyte；
D, by the culture of a period of time, under conditions of reducing external resistance value, filter out anti-current pass through it is micro-
Biological flora, then the stable microbial film that grows into is carried on anode microorganism, can further progress correlated performance test.
Preferably, the pH value of catholyte and anolyte described in step c is neutrality.
Preferably, reduction external resistance value described in step d is replacement dispatch from foreign news agency resistance value, and should be from 1000 Ω down
Drop, filters out the microbial flora that anti-high current passes through.
The present invention has the advantage that: (1) for the present invention using walnut shell as raw material, cheap, amount greatly, belongs to renewable energy
It is widely used；(2) using walnut shell as carbon source, using urea as nitrogen source, a kind of N doping biomass carbon material N-C has been invented, because of it
With preferable biocompatibility and biggish specific surface area, anode activation overpotential is advantageously reduced, so that Microbial fuel
The power density of battery is significantly improved.
Detailed description of the invention
Fig. 1 is the synthetic method of a kind of biological material walnut shell carbon material nitrating of the present invention and its in Microbial fuel electricity
In terms of the anode of pond using N-C-800 DEG C of adsorption desorption curve graph.
Fig. 2 is the synthetic method of a kind of biological material walnut shell carbon material nitrating of the present invention and its in Microbial fuel electricity
The current density comparison diagram of anode of microbial fuel cell in application in terms of the anode of pond.
Specific embodiment
The preferred embodiment of the present invention is described in detail with reference to the accompanying drawing, so that advantages and features of the invention energy
It is easier to be readily appreciated by one skilled in the art, so as to make a clearer definition of the protection scope of the present invention.
A kind of synthetic method of biological material walnut shell carbon material nitrating, includes the following steps,
1), walnut shell is washed, dries and is crushed；
2) broken walnut shell is activated in the aqueous solution of activator, then take out and is dried；
3) it, by the high-temperature calcination under inert gas range of dried product, by the product acid elution after carbonization, then uses
Deionized water washing is dry by the product after washing until neutrality, obtains walnut shell carbon material；
4) carbon material is fully ground from different urea, a small amount of deionized water is added and is stirred and dries at room temperature；
5), by mixture high-temperature calcination under an inert gas, the extra unreacted urea of filtering and washing obtains nitrogen-doped carbon
Material.
Preferably, activator described in step 2) is ZnCl2Solution, the ZnCl2Solution concentration is 5mol/L, institute
The temperature for stating activation processing is 180 DEG C, and the activation processing time is 12h.
Preferably, it is 600 DEG C, 800 DEG C, 1000 DEG C, heating that the condition of the step 3) high temperature cabonization, which is carburizing temperature,
Rate is 5 DEG C/min, and the condition of high temperature cabonization is that carbonization time is 2h, and the inert gas is N2Or Ar, the hydrochloric acid are dense
Degree is 1mol/L.
Preferably, the mass ratio of carbon material and urea described in step 4) is 1:2,1:5,1:8.
Preferably, temperature described in step 5) be 600 DEG C, 800 DEG C, 1000 DEG C, the heating rate be 10 DEG C/
Min, the extra urea deionized water of the washing.
A kind of biomass nitrogen-doped carbon material is applied in anode of microbial fuel cell, is included the following steps,
A, by the nitrogen-doped carbon material obtained by any preparation method of claim 1 to 6 and corresponding solvent
Adhesive is made by mixing into slurries and is coated in long 2cm, on the carbon cloth of wide 1cm, anode of microbial fuel cell is fabricated to, with common carbon
Cloth electrode is assembled in together in same anode chamber；
B, use carbon brush as microorganism fuel cell cathode, two pole room of yin-yang is linked by proton exchange membrane and is built into
For H-type microbial fuel cell unit, temperature is 28 DEG C~35 DEG C, configures good corresponding microorganism growth-promoting media and is injected into anode chamber
In and catholyte injection cathode chamber in；
C, link voltage data collector, the external resistance voltage value of acquisition in machine every five minutes, according to external resistance voltage
The variation of value regularly replaces catholyte and anolyte；
D, by the culture of a period of time, under conditions of reducing external resistance value, filter out anti-current pass through it is micro-
Biological flora, then the stable microbial film that grows into is carried on anode microorganism, can further progress correlated performance test.
Preferably, the pH value of catholyte and anolyte described in step c is neutrality.
Preferably, reduction external resistance value described in step d is replacement dispatch from foreign news agency resistance value, and should be from 1000 Ω down
Drop, filters out the microbial flora that anti-high current passes through.
Case study on implementation
1. the preparation of walnut shell carbon material: walnut shell is impregnated supersound washing in deionized water, drying under the conditions of 60 DEG C
For 24 hours and ball milling；The good material of ball milling is put into the ZnCl of 5mol/L2In solution, mixed liquor capacity holds no more than inner liner of reaction kettle
The 70% of amount carries out 12 hours of 180 DEG C of hydro-thermal reactions, filters and dries for 24 hours after reaction under the conditions of 80 DEG C；It will dry
Product afterwards is calcined under atmosphere of inert gases, is warming up to 600 DEG C, 800 DEG C, 1000 DEG C from room temperature with 5 DEG C/min, and respectively
2h is kept at a temperature of its, cooled to room temperature is black cellular solid after taking-up, and grinding is stand-by.
2. the synthesis of walnut shell nitrating carbon material: by the urea (quality of walnut shell carbon material and different quality obtained by (1)
Than a small amount of deionized water being added and is sufficiently mixed for 1:2,1:5,1:8).After being dried in vacuo under the conditions of 40 DEG C, grind into powder is set
It in high temperature process furnances, is calcined under atmosphere of inert gases, is warming up to 600 DEG C, 800 DEG C, 1000 from room temperature with 10 DEG C/min
DEG C, and 3h is kept at a temperature of its, cooled to room temperature.
3. the removal of the extra urea of walnut shell nitrating carbon material: the product deionized water ultimately generated in (2) centrifugation is washed
It washs, and drying is for 24 hours, final to obtain walnut shell nitrating carbon material under 120 DEG C of vacuum conditions.
4. application of the walnut shell nitrating carbon material in terms of anode of microbial fuel cell: by carbon material and corresponding solvent
And adhesive is made by mixing into slurries and is uniformly applied to surplus to be fabricated to electrode on the carbon cloth of 2*1cm, with plain carbon cloth group
Loaded in same anode of microbial fuel cell room.Common carbon brush is cathode, and two pole room of yin-yang and proton exchange membrane are assembled into H-type
Microbial fuel cell unit, external circuit chain connecting resistance.Under the conditions of 28 DEG C~32 DEG C of room temperature, by configured catholyte and sun
Pole liquid injects corresponding yin, yang pole room respectively.The voltage value of an external resistance was acquired by voltage data collector every five minutes,
According to the variation of external resistance voltage value, catholyte and anolyte are regularly replaced, until microorganism, which stablizes growth, can carry out correlation
The test of performance.
Not limited to this, any change or replacement expected without creative work should all be covered in guarantor of the invention
Within the scope of shield.Therefore, protection scope of the present invention should be determined by the scope of protection defined in the claims.
Claims (8)
1. a kind of synthetic method of biological material walnut shell carbon material nitrating, it is characterised in that: include the following steps,
1), walnut shell is washed, dries and is crushed；
2) broken walnut shell is activated in the aqueous solution of activator, then take out and is dried；
3), by the high-temperature calcination under inert gas range of dried product, by the product acid elution after carbonization, then spend from
Sub- water washing is dry by the product after washing until neutrality, obtains walnut shell carbon material；
4) carbon material is fully ground from different urea, a small amount of deionized water is added and is stirred and dries at room temperature；
5), by mixture high-temperature calcination under an inert gas, the extra unreacted urea of filtering and washing obtains N doping carbon materials
Material.
2. a kind of synthetic method of biological material walnut shell carbon material nitrating according to claim 1, which is characterized in that
Activator described in its step 2) is ZnCl2Solution, the ZnCl2Solution concentration is 5mol/L, the temperature of the activation processing
It is 180 DEG C, the activation processing time is 12h.
3. a kind of synthetic method of biological material walnut shell carbon material nitrating according to claim 1, which is characterized in that
The condition of its step 3) high temperature cabonization is that carburizing temperature is 600 DEG C, 800 DEG C, 1000 DEG C, and heating rate is 5 DEG C/min, high
The condition of temperature carbonization is that carbonization time is 2h, and the inert gas is N2Or Ar, the concentration of hydrochloric acid are 1mol/L.
4. a kind of synthetic method of biological material walnut shell carbon material nitrating according to claim 1, which is characterized in that
The mass ratio of carbon material described in its step 4) and urea is 1:2,1:5,1:8.
5. a kind of synthetic method of biological material walnut shell carbon material nitrating according to claim 1, which is characterized in that
Temperature described in its step 5) is 600 DEG C, 800 DEG C, 1000 DEG C, and the heating rate is 10 DEG C/min, and the washing is more
Remaining urea deionized water.
6. a kind of biomass nitrogen-doped carbon material is applied in anode of microbial fuel cell, it is characterised in that: include the following steps,
A, by the nitrogen-doped carbon material obtained by any preparation method of claim 1 to 6 and corresponding solvent bonding
Agent is made by mixing into slurries and is coated in long 2cm, on the carbon cloth of wide 1cm, is fabricated to anode of microbial fuel cell, with plain carbon cloth electricity
Pole is assembled in together in same anode chamber；
B, use carbon brush as microorganism fuel cell cathode, two pole room of yin-yang is linked by proton exchange membrane and builds as H
Type microbial fuel cell unit, temperature configure good corresponding microorganism growth-promoting media and are injected into anode chamber at 28 DEG C~35 DEG C,
And in catholyte injection cathode chamber；
C, link voltage data collector, the external resistance voltage value of acquisition in machine every five minutes, according to external resistance voltage value
Variation regularly replaces catholyte and anolyte；
D, the microorganism that anti-current passes through is filtered out under conditions of reducing external resistance value by the culture of a period of time
Flora, then the stable microbial film that grows into is carried on anode microorganism, can further progress correlated performance test.
7. a kind of biomass nitrogen-doped carbon material according to claim 6 is applied in anode of microbial fuel cell, special
Sign is that the pH value of catholyte described in step c and anolyte is neutrality.
8. a kind of biomass nitrogen-doped carbon material according to claim 6 is applied in anode of microbial fuel cell, special
Sign is that reduction external resistance value described in step d is replacement dispatch from foreign news agency resistance value, and should filter out from 1000 Ω toward decline
The microbial flora that anti-high current passes through.
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Application publication date: 20190517 |