CN106929549A - A kind of method that utilization self assembly conductive biological membrane electrode reduces carbon dioxide production acetic acid - Google Patents
A kind of method that utilization self assembly conductive biological membrane electrode reduces carbon dioxide production acetic acid Download PDFInfo
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- CN106929549A CN106929549A CN201710156662.1A CN201710156662A CN106929549A CN 106929549 A CN106929549 A CN 106929549A CN 201710156662 A CN201710156662 A CN 201710156662A CN 106929549 A CN106929549 A CN 106929549A
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- carbon dioxide
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- acetic acid
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/40—Preparation of oxygen-containing organic compounds containing a carboxyl group including Peroxycarboxylic acids
- C12P7/54—Acetic acid
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
- C12N1/36—Adaptation or attenuation of cells
Abstract
The invention discloses the method that a kind of self assembly conductive biological membrane electrode reduction carbon dioxide produces acetic acid, comprise the following steps：(1) by toward addition inhibitor chloromethane in inoculum, then continuously in H2/CO2Carry out biological domestication under atmosphere, and constantly shorten and turn over the time of connecing, obtain domestication from oxygen animalcule.(2) using carbon felt as electrode, the culture medium grown from oxygen animalcule and suitable micro-organisms for then being obtained in inoculation step (1) thereto, in H2/CO2After being reacted 5~7 days under atmosphere, new culture medium is replaced by, and under same atmosphere, after reacting 3~5 days, then be used for this conductive biological membrane electrode in bioelectrochemistry reduction carbon dioxide product acetic acid by the conductive biological membrane electrode needed for obtaining.Biological membrane electrode preparation process is simple of the invention, high catalytic efficiency, can effectively improve the electron transport rate of biological-cathode, so that enhanced biological electrochemically reducing carbon dioxide produces the efficiency of acetic acid.
Description
Technical field
The invention belongs to electrode material technical field, and in particular to a kind of self assembly conductive biological membrane electrode and its preparation side
Method and purposes.
Background technology
The energy fuel and other kinds organic chemistry product that fossil resources are provided support mankind's warp over nearly 200 years
Ji and social development.However, the abuse of the mankind makes non-renewable fossil resource move towards exhausted.More seriously,
The greenhouse gases CO that increasing evidence will be caused using fossil fuel2Discharge, linked up with Global climate change.
And on the other hand, CO2Be on the earth most extensively with cheap carbon resource.Therefore, develop CO2It is converted into fuel or high level chemistry
The technology of product will provide tool potential solution for the supply of regenerative resource and material.
In current existing CO2In transformation technology, bioelectrochemistry technology (Microbial Electrosynthesis,
MES) it is a kind of emerging strategy.MES technologies are originated as energy by the use of the electronics on electrode using electric autotrophic microbe, with
CO2As sole carbon source, the production process of many carbon fine chemicals or the energy is reduced into.It is solid compared to other carbon dioxide
Determine technology, microorganism electro synthesis can by microorganism be directly produced out needs organic matter and be secreted into it is extracellular, without opposite
Material is processed further carrying out production, reduces energy consumption and waste water in treatment biomass process, it is to avoid treatment is biological
To the influence of environment in matter degradation process.In addition, fixing CO compared to biological photosynthesis2, MES reduction CO2Only need to one very
Small area can carry out the intensive manufacture energy and chemicals, not compete soil with grain-production.In MES, biomembrane is
Refer to microorganism to resist change and the toxicity of external environment, it is intended to when solid table is contacted, to exocytosis polymer such as
Polysaccharide etc. helps it to stick to the surface of solids, and the microbial aggregate for being formed.Electric autotrophic microbe is just main in MES system
There is electrode surface in the form of biomembrane.However, the electric conductivity of biomembrane itself and bad, it is impossible to efficient transmission electricity
Son, makes electric autotrophic microbe to obtain enough electron reduction CO2, this is the low Main Bottleneck of MES production efficiencys.
The content of the invention
The technical problems to be solved by the invention are directed to shortcomings and deficiencies of the prior art, there is provided a kind of self assembly is conductive
The preparation method of biological membrane electrode, so as to improve the yield of carbon dioxide synthesis of acetic acid.
In order to solve the above technical problems, the present invention is adopted the technical scheme that：One kind is using self assembly conductive biological film electricity
The method that bioelectrochemistry reduces carbon dioxide production acetic acid is improved in pole, comprises the following steps：
(1) from the domestication of oxygen animalcule：Under the mixed-gas atmosphere of hydrogen and carbon dioxide, initial inoculum is added
In PETC solution, inhibitor is added, cultivated 5~7 days, obtain the first generation from oxygen animalcule, with the first generation from oxygen animalcule to connect
Kind of thing adds and carry out in PETC solution the first round to turn over to connect, and it is 3 times, 4~6 days each reaction time that the first round turns over the number of times for connecing；It
After carry out the second wheel and turn over to connect, it is 3 times, 2~4 days each reaction time that the second wheel turns over the number of times for connecing；Third round is carried out again afterwards to turn over
Connect, it is 3 times, 1~2 day each reaction time that third round turns over the number of times for connecing；More than turn over and connect incubation in hydrogen and carbon dioxide
Mixed-gas atmosphere under carry out；Finally obtain domestication from oxygen animalcule；
(2) preparation of conductive biological membrane electrode：In the reactor, under the mixed-gas atmosphere of hydrogen and carbon dioxide,
Using carbon felt as electrode, with PETC solution as cathode solution, obtain in inoculation step (1) thereto from oxygen animalcule, reaction 5
After~7 days, fresh PETC solution is changed, add graphene oxide, then after reacting 3~5 days, obtain the conductive biological of self assembly
Membrane electrode；
(3) bioelectrochemistry reduction carbon dioxide produces acetic acid：In the battery, using carbon felt as anode, obtained with step (2)
The reactor is separated into cathode chamber and anode by the conductive biological membrane electrode of the self assembly arrived as negative electrode with PEM
Room, with PTEC solution as catholyte and anolyte, externally-applied potential, is continuously passed through 100% carbon dioxide, in 20~30 DEG C of conditions
Lower reaction, produces acetic acid.
In step (1), the inoculum is the mixture of one or more of anaerobic sludge, bed mud, soil, is preferably detested
Oxygen sludge, the inoculum comprise at least Proteobacteria (Proteobacteria), Firmicutes (Firmicutes),
Bacteroidetes (Bacteroidetes), Spirochaetes (conveyor screw door), the inhibitor are chlorine that mass ratio is 1~5%
Change the methane aqueous solution, the preferably chloromethane aqueous solution of mass ratio 1~2% and turns over and connects the culture medium for using and be at the inoculation
PETC solution.
In step (1), the inoculation and to turn over the temperature that connects be 20~30 DEG C.
In step (2), the temperature of the inoculation is 20~30 DEG C.
In step (1), the inoculum concentration being inoculated with first is volume ratio 2~6%, preferably 5~6%.
In step (1), described turning over connects each inoculum concentration for volume ratio 5~6%；Wherein, when the first round turns over the reaction for connecing
Between be preferably 5~6 days；Second wheel turns over reaction time for connecing and is preferably 3~4 days；Third round is turned over the reaction time for connecing and is preferably 1.5
~2 days.
In step (2), the inoculum concentration of the inoculation is volume ratio 5~6%.
In step (2), concentration of the graphene oxide in water is 0.1~1mg/ml, preferably 0.5mg/ml.
Current potential described in step (3) is -0.85~-1.2V, preferably -1.05V relative to Ag/AgCl electrodes.
In step (1)~(3), the formula of described PETC solution is as follows：NH4Cl 0.5~2g/L, KCl 0.1~
0.3g/L,MgSO4·7H2O 0.1~0.3g/L, NaCl 0.5~1g/L, KH2PO40.1~0.3g/L, CaCl20.01~
0.03g/L, NaHCO30.5~2g/L, pH=6.5~7.5, solvent is water.
In step (1) and (2), the volume ratio of hydrogen and carbon dioxide is in the mixed gas of the hydrogen and carbon dioxide
60~80:40~20, preferably volume ratio 80:20.
In the present invention, efficiently from oxygen animalcule, the electronics that fixed carbon dioxide is produced is used as reducing power using hydrogen
In the oxy radical on redox graphene, it is often more important that these microorganisms can be while redox graphene, will
Graphene is self-assembled on electrode, and while biological reducing graphene oxide, Graphene utilizes its mesh space structure
It is final to obtain conductive biological membrane electrode to be captured from oxygen animalcule.
The present invention is specifically tamed by microorganism, and acquisition can be used to prepare the efficient from the micro- life of oxygen of conductive biological membrane electrode
Thing；, come the bioelectrode of self assembly acquisition graphene modified, carried out on simplified electrode nanometer-material-modified using from oxygen animalcule
Problem；Using autotrophic microbe while redox graphene, the stone with electro-chemical activity can be self-assembly of
Black alkene hydridization biomembrane, the electron transmission performance outside extracellular microbial is lifted from the angle of biological film conductivity, is carried so as to reach
Bioelectrochemistry high fixes the purpose of the efficiency of carbon dioxide.
Beneficial effect：Biological membrane electrode preparation process is simple of the invention, high catalytic efficiency, can effectively improve biological-cathode
Electron transport rate so that enhanced biological electrochemically reducing carbon dioxide produce acetic acid efficiency.
Brief description of the drawings
Fig. 1 is the flora abundance distribution that the present invention is based on door from oxygen animalcule；
Fig. 2 schemes for the SEM of conductive biological membrane electrode；
Fig. 3 is that the bioelectrochemistry of control group and conductive biological film group is produced acetic acid and changed with time figure；
Fig. 4 is that the bioelectrochemical system extrinsic current of control group and conductive biological film group changes with time figure；
Fig. 5 is the ac impedance spectroscopy of control group and conductive biological film group.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
Apply the content described by example and be merely to illustrate the present invention, without should also without limitation on sheet described in detail in claims
Invention.
Embodiment 1：From oxygen animalcule domestication, specific domestication step is as follows:
Anaerobic sludge is added in the solution rich in culture medium, the H that has friendly relations in advance is added to by certain inoculum concentration2、CO2
Ratio is 80:In the anaerobism bottle of 20 mixed gas, culture medium is PETC solution, and the formula of wherein PETC solution is:1g/L
NH4Cl,0.1g/L KCl,0.2g/L MgSO4·7H2O,0.8g/L NaCl,0.1g/L KH2PO4,0.02g/L CaCl2,1g/
L NaHCO3, pH=7.0.
It is subsequently adding the chloromethane aqueous solution that mass ratio is 2%, after reaction 7 days, then is linked into by 5% inoculum concentration
In the anaerobism bottle stated, react 5 days, then turn over again and connect, after being repeated 3 times, or turned over and connect by 5% inoculum concentration, in the reaction time
It is reduced to 3 days, after repeating 3 times, then is turned over 5% inoculum concentration and connect, and the time is reduced to 1.5 days, after being repeated 3 times, obtains
Required is efficient from oxygen animalcule.This is efficiently carried out into flora analysis from oxygen animalcule, as a result as shown in Figure 1, it can be seen that
Most significant three doors in the flora that obtains of screening, by its abundance from high to low, respectively Proteobacteria (mycetozoans
Door), Firmicutes (Firmicutes) and Bacteroidetes (Bacteroidetes).
Embodiment 2：It is prepared by conductive biological membrane electrode
Put into anaerobism bottle as electrode using carbon felt, cathode solution is PETC solution, and be inoculated with 5% and screened by (1)
What is obtained is efficient from oxygen animalcule, leads to after hydrogen and carbon dioxide (80/20, v/v) react 7 days, reaction solution is replaced by new
PETC solution, and the graphene oxide of 0.5mg/ml is added, then have friendly relations H2、CO2Ratio is 80:20 hydrogen and carbon dioxide, instead
After answering 5 days, solution becomes black, the conductive biological membrane electrode needed for obtaining.Fig. 2 is the conductive biological membrane electrode for preparing,
It can be seen that Graphene is wrapped in microorganism, good attached person is on carbon felt electrode.
Embodiment 3：Conductive biological membrane electrode bioelectrochemistry reduction carbon dioxide produces acetic acid
The specific number of assembling steps and ruuning situation of Bioelectrochemical device are as follows：
(1) carbon felt anode and the conductive biological membrane electrode prepared are respectively put into anode chamber and cathode chamber
(2) anode chamber and the interior PETC solution all added in embodiment 1 of cathode chamber, use potentiostat between negative electrode and anode
The current potential of additional -1.05V (relative to silver/silver chlorate), is then continuously passed through 100% carbon dioxide, 25 DEG C of reaction temperature.
The carbon felt negative electrode of Graphene is not added with as control using manufacturing process, its preparation method as embodiment 2, simply
Without graphene oxide, all of bioelectrochemical system is continuously run 40 days, timing sampling, determines the concentration of acetic acid.By
Fig. 3 can be seen that, by the reaction of 40 days, its gas concentration lwevel was 4.9 ± 0.1g L to control group-1, and conductive biological film group
Gas concentration lwevel is 7.1 ± 0.3g L-1, it is 1.4 times of control group.Fig. 4 shows the curent change situation in course of reaction,
Where it can be seen that the electric current of conductive biological film group will be higher than control group in whole course of reaction, its latter stage electricity in reaction
Stream (absolute value) is 6.8 ± 0.5mA, and control group only has 4.7 ± 0.3mA.Electricity further has been carried out to bioelectrochemical system
Chemical impedance is analyzed, and as seen from Figure 5, the internal resistance of control group is 456.8 Ω, and the internal resistance of conductive biological film group is 12.3 Ω,
Reduce 37 times.It can thus be seen that internal resistance when conductive biological film of the invention can effectively reduce reaction, when improving reaction
The electric current of time, so as to be conducive to bioelectrochemistry to produce the raising of acetic acid efficiency.
Embodiment 4：From oxygen animalcule domestication, specific domestication step is as follows:
Anaerobic sludge is added in the solution rich in culture medium, the H that has friendly relations in advance is added to by certain inoculum concentration2、CO2
Ratio is 60:In the anaerobism bottle of 40 mixed gas, culture medium is PETC solution, and the formula of wherein PETC solution is:1g/L
NH4Cl,0.1g/L KCl,0.2g/L MgSO4·7H2O,0.8g/L NaCl,0.1g/L KH2PO4,0.02g/L CaCl2,1g/
L NaHCO3, pH=7.0.
It is subsequently adding the chloromethane aqueous solution that mass ratio is 1%, after reaction 7 days, then is linked into by 6% inoculum concentration
In the anaerobism bottle stated, react 6 days, then turn over again and connect, after being repeated 3 times, or turned over and connect by 6% inoculum concentration, in the reaction time
It is reduced to 4 days, after repeating 3 times, then is turned over 5% inoculum concentration and connect, and the time is reduced to 2 days, after being repeated 3 times, obtains institute
Need from oxygen animalcule.
Embodiment 5：It is prepared by conductive biological membrane electrode
Put into anaerobism bottle as electrode using carbon felt, cathode solution is PETC solution, and be inoculated with 6% and screened by (1)
Obtain from oxygen animalcule, lead to after hydrogen and carbon dioxide (80/20, v/v) react 5 days, reaction solution is replaced by new PETC
Solution, and the graphene oxide of 0.5mg/ml is added, then have friendly relations H2、CO2Ratio is 80:20 hydrogen and carbon dioxide, reaction 3
After it, solution becomes black, the conductive biological membrane electrode needed for obtaining.
Embodiment 6：Conductive biological membrane electrode bioelectrochemistry reduction carbon dioxide produces acetic acid
The specific number of assembling steps and ruuning situation of Bioelectrochemical device are as follows：
(1) carbon felt anode and the conductive biological membrane electrode prepared are respectively put into anode chamber and cathode chamber
(2) anode chamber and the interior PETC solution all added in embodiment 1 of cathode chamber, use potentiostat between negative electrode and anode
The current potential of additional -0.85V (relative to silver/silver chlorate), is then continuously passed through 100% carbon dioxide, 20 DEG C of reaction temperature.
Embodiment 7：Conductive biological membrane electrode bioelectrochemistry reduction carbon dioxide produces acetic acid
The specific number of assembling steps and ruuning situation of Bioelectrochemical device are as follows：
(1) carbon felt anode and the conductive biological membrane electrode prepared are respectively put into anode chamber and cathode chamber
(2) anode chamber and the interior PETC solution all added in embodiment 1 of cathode chamber, use potentiostat between negative electrode and anode
The current potential of additional -1.2V (relative to silver/silver chlorate), is then continuously passed through 100% carbon dioxide, 30 DEG C of reaction temperature.
The carbon felt negative electrode of Graphene is not added with as control using manufacturing process, its preparation method as embodiment 2, simply
Without graphene oxide, all of bioelectrochemical system is continuously run 40 days, timing sampling, determines the concentration of acetic acid.It is right
According to group by the reaction of 40 days, its gas concentration lwevel is 3.8 ± 0.1g L-1, and the gas concentration lwevel of conductive biological film group
It is 5.2 ± 0.1g L-1, it is 1.3 times of control group, it is 6.0 ± 0.5mA in the latter stage electric current (absolute value) of reaction, and is compareed
Group only has 4.1 ± 0.1mA.It can thus be seen that electric current when conductive biological film of the invention can improve reaction, is conducive to biology
Electrochemistry produces the raising of acetic acid efficiency.
Claims (9)
1. a kind of method that utilization self assembly conductive biological membrane electrode reduces carbon dioxide production acetic acid, it is characterised in that including
Following steps：
(1) from the domestication of oxygen animalcule：Under the mixed-gas atmosphere of hydrogen and carbon dioxide, initial inoculum is added into PETC
In solution, inhibitor is added, cultivated 5~7 days, the first generation from oxygen animalcule is obtained, with the first generation from oxygen animalcule as inoculum
Add and carry out in PETC solution the first round to turn over and connect, it is 3 times, 4~6 days each reaction time that the first round turns over the number of times for connecing；It is laggard
The wheel of row second is turned over and connect, and it is 3 times, 2~4 days each reaction time that the second wheel turns over the number of times for connecing；Carry out third round again afterwards and turn over to connect,
It is 3 times, 1~2 day each reaction time that three-wheel turns over the number of times for connecing；More than turn over the mixing for connecing incubation in hydrogen and carbon dioxide
Carried out under gas atmosphere；Finally obtain domestication from oxygen animalcule；
(2) preparation of conductive biological membrane electrode：In the reactor, under the mixed-gas atmosphere of hydrogen and carbon dioxide, with carbon
Felt as electrode, with PETC solution as cathode solution, obtain in inoculation step (1) thereto from oxygen animalcule, reaction 5~7
After it, fresh PETC solution is changed, add graphene oxide, then after reacting 3~5 days, obtain the conductive biological film of self assembly
Electrode；
(3) bioelectrochemistry reduction carbon dioxide produces acetic acid：In the battery, using carbon felt as anode, with what is obtained in step (2)
The reactor is separated into cathode chamber and anode chamber by the conductive biological membrane electrode of self assembly as negative electrode with PEM,
With PTEC solution as catholyte and anolyte, externally-applied potential, 100% carbon dioxide is continuously passed through, under the conditions of 20~30 DEG C
Reaction, produces acetic acid.
2. method according to claim 1, it is characterised in that in step (1), the inoculum be anaerobic sludge, bed mud,
The mixture of one or more of soil.
3. method according to claim 1, it is characterised in that in step (1), the inhibitor is that mass ratio is 1~5%
The chloromethane aqueous solution.
4. method according to claim 1, it is characterised in that in step (1), the temperature that the inoculation and turning over connects for 20~
30℃。
5., according to the method described in claim 1, it is characterised in that in step (2), the temperature of the inoculation is 20~30 DEG C.
6. method according to claim 1, it is characterised in that in step (2), concentration of the graphene oxide in water is
0.1~1mg/ml.
7. method according to claim 1, it is characterised in that the current potential described in step (3) is relative to Ag/AgCl electrodes
It is -0.85~-1.2V.
8. method according to claim 1, it is characterised in that in step (1)~(3), the formula of described PETC solution
It is as follows：NH4Cl 0.5~2g/L, KCl 0.1~0.3g/L, MgSO47H2O 0.5~1g/L of 0.1~0.3g/L, NaCl,
KH2PO4 0.1~0.3g/L, CaCl20.01~0.03g/L, NaHCO30.5~2g/L, pH=6.5~7.5, solvent is water.
9. method according to claim 1, it is characterised in that in step (1) and (2), the hydrogen and carbon dioxide
The volume ratio of hydrogen and carbon dioxide is 60~80 in mixed gas:40~20.
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| CN113231095A (en) * | 2021-05-08 | 2021-08-10 | 南京工业大学 | Carbon nitride heterojunction photocatalyst and preparation method and application thereof |
| CN113881716A (en) * | 2021-10-27 | 2022-01-04 | 江南大学 | Method for promoting carbon chain extension microbial electrosynthesis of organic acid |
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| CN113231095A (en) * | 2021-05-08 | 2021-08-10 | 南京工业大学 | Carbon nitride heterojunction photocatalyst and preparation method and application thereof |
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