CN109022495A - A kind of method of micro-reduction carbon dioxide methane phase - Google Patents
A kind of method of micro-reduction carbon dioxide methane phase Download PDFInfo
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- CN109022495A CN109022495A CN201811057009.0A CN201811057009A CN109022495A CN 109022495 A CN109022495 A CN 109022495A CN 201811057009 A CN201811057009 A CN 201811057009A CN 109022495 A CN109022495 A CN 109022495A
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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
- C12P5/00—Preparation of hydrocarbons or halogenated hydrocarbons
- C12P5/02—Preparation of hydrocarbons or halogenated hydrocarbons acyclic
- C12P5/023—Methane
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
Abstract
The present invention relates to a kind of methods of micro-reduction carbon dioxide methane phase, comprising the following steps: 1) building includes the microorganism electrolysis cell of cathode pool and anode pool, includes working electrode, reference electrode in cathode pool；Anode pool includes to electrode；It is separated between cathode pool and anode pool with proton exchange membrane；2) methanogen culture medium is added in cathode pool and anode pool；3) 1.5~5.0% methanogen bacterium solutions are inoculated in cathode pool；It cultivates at room temperature；4) cathode pool load -0.6v (vs SHE) voltage；5) methane is harvested by cathode pool head space.Compared with prior art, the present invention without chemical catalyst, clean and effective, low cost by CO2Biological reducing is methanol method, and without other by-products, is had broad application prospects.
Description
Technical field
The present invention relates to CO2Resource utilization field more particularly to a kind of promotion microorganism utilize electric energy by CO2It is converted into
The method of methane.
Background technique
Since the industrial revolution, the production activity of the mankind is a significant increase CO in atmosphere2Content.CO2As main
One of greenhouse gases, the growth of content may cause global warming in an atmosphere and weather extreme event increases.How
Reduce CO in atmosphere2Content, or even be translated into high added value chemicals become one the whole world research hot spot.It is common
Method for transformation include chemical conversion and bioconversion.Chemical method generally requires high temperature and pressure and catalyst, in contrast, biological
Conversion can occur under room temperature condition of normal pressure, and reaction condition is mild, has broad application prospects.
Using microorganism by CO2It is converted into the existing extensive research of methane and report.Patent No. CN102925492A's
The patent microorganism that seed sludge is enriched in the cathodic compartment restores CO using electric current2Second can also be produced while methane phase
Acid.But its potential for starting methane phase (- 850mV arrives -950mV, vs Ag/AgCl) is higher, energy consumption is larger；Producing first
By-product acetic acid is generated simultaneously during alkane, the efficiency of methane phase is reduced, increases product separating difficulty.
In this regard, we provide a kind of new biological-cathode, it can be under low potential, by CO2Convert to high efficiency, low cost
For CH4.Utilize nitric acid-high-specific surface area of acetic acid composite fibre film and the good electric conductivity of porosity and carbon nanotube
Working electrode is made.It places it in cathode pool, methane phase sarcine can adhere on the working electrode (s, apply when in cathode
When being powered on gesture, methanogen can will be efficiently quickly by CO2It is converted into methane.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of micro-reductions two
The method of carbonoxide methane phase.
The purpose of the present invention can be achieved through the following technical solutions: a kind of micro-reduction carbon dioxide methane phase
Method, which comprises the following steps:
1) building includes the microorganism electrolysis cell of cathode pool and anode pool, includes electrolyte, working electrode (yin in cathode pool
Pole), reference electrode and methanogen；Anode pool includes electrolyte and platinum to electrode；N117 matter is used between cathode pool and anode pool
Proton exchange separates；
2) methanogen culture medium is added in cathode pool and anode pool；
3) 3ml methanogen bacterium solution, culture are inoculated in cathode pool；
4) cathode pool load -0.6v (vs SHE) voltage；
5) methane is harvested by cathode pool head space.
Working electrode described in step (1) is made of the nitric acid-acetic acid composite fibre film for sticking multi-walled carbon nanotube.
Sticking multi-walled carbon nanotube amount on the nitric acid-acetic acid composite fibre film is 0.1~10mg/cm2, multi-wall carbon nano-tube
Length of tube is 0.5~50 μm；Nitric acid -0.2~2 μm of acetic acid composite fibre membrane pore size.
The preparation method of working electrode is the following steps are included: firstly, be that 0.5~50 μm of multi-wall carbon nano-tube is effective by length
5% hydrogen peroxide dipping shakes 1h, is dissolved in 0.5~20% nafion ethanol solution after dry, is ultrasonically treated 1~60min
Keep multi-walled carbon nanotube evenly dispersed, multi-walled carbon nanotube nafion ethanol solution is made, being then evenly coated in aperture is
On 0.2~2 μm of nitric acid acetic acid composite fibre film, dried in 20~65 DEG C of environment.Make nitric acid-acetic acid composite fibre film
Carbon multi-wall nano tube loaded amount be 0.1~10mg/cm2.Nitric acid-acetic acid composite fibre film of multi-walled carbon nanotube will be loaded with
It is placed in cathode pool, and links to form working electrode with platinum filament.
By pond body, working electrode, reference electrode, electrolytic cell is assembled into electrode etc..In cathode of electrolytic tank pond and anode pool
It is passed through 50mL methanogen and often uses culture medium.
The formula of methanogen culture medium described in step (2) is as follows: 0.35g/L K2HPO4, 0.23g/L KH2PO4,
0.5g/L NH4Cl, 0.5g/L MgSO4·7H2O, 0.25g/L CaCl2, 2.25g/L NaCl, 0.85g/L NaHCO3, 0.5g/
L Na2S·H2O, 10ml/L trace element solution, 1ml/L vitamin solution；Electrolytic cell head space is CO2:N2=1:4's (n/n)
Gaseous mixture；
The trace element solution formula is as follows: 1500mg/L FeCl2·4H2O, 70mg/L ZnCl2, 100mg/L
MnCl2·4H2O, 6mg/L HBO3, 190mg/L CoCl2·6H2O, 2mg/L CuCl2·H2O, 24mg/L NiCl2·6H2O,
36mg/L NaMo4·2H2O, HCl (25%) 10ml/L；
The vitamin solution formula is as follows: 2mg/L biotin, 2mg/L folic acid, 10mg/L vitamin B6, 5mg/L dimension
Raw element B1, 5mg/L vitamin B2, 5mg/L niacin, 5mg/L pantothenic acid, 0.1mg/L vitamin B12, 5mg/L aminobenzoic acid,
5mg/L lipoic acid.
Methanogen described in step (3) is including but not limited to Pasteur's methanogen (Methanosarcina
Barkeri), Bu Shi methanogen (Methanobacterium byrantti) and Heng Shi methanogen
(Methanospirllum hungatei)。
Methanogen described in step (3) is cultivated at room temperature.
1.5~5.0% methanogen bacterium solutions are accessed in cathode pool.To avoid generating other products, which should be by producing
Methane backeria single bacterium composition.Start in cathode application -0.6V potential (vs SHE) and react, in gas chromatograph detection headspace gas
Methane content.
Compared with prior art, working electrode of the present invention is thin by nitric acid-acetic acid composite fibre of loading multi-wall carbon nanotubes
Film composition, the fiber membrane lie in a horizontal plane in cathode bottom of pond portion.It is inoculated with methanogen in cathode pool simultaneously, it can be in lower negative electricity
Utilize microorganism by CO under gesture2It is reduced to methane.The present invention provides a kind of without chemical catalyst, clean and effective, low cost
By CO2Biological reducing is methanol method, and without other by-products, is had broad application prospects.
Detailed description of the invention
Fig. 1 is the structure water body of microorganism electrolysis cell of the present invention
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1:
The embodiment is divided into experimental group A and control group B, C are carried out simultaneously:
Experimental group A is as shown in Figure 1 (embodiment two, three is same).Microorganism electrolysis cell includes cathode pool and anode pool, wherein yin
Reference electrode 2 is equipped in the pond of pole, cathode 4, methanogen 3 and culture medium 5, anode pool is interior to be equipped with to electrode 7, cathode pool and anode
It is equipped with proton exchange membrane 6 between pond, is additionally provided with power supply 1 and is separately connected reference electrode 2, cathode 4 and to electrode 7.In the present embodiment
Middle methanogen 3 is Pasteur's methanogen bacterium solution (Methanosarsina barkeri).Reference electrode 2 is Ag/AgCl electrode,
Cathode 4 is made of the nitric acid-acetic acid composite fibre film for sticking multi-walled carbon nanotube.It is platinum to electrode to electrode 7.
The formula of culture medium 5 is as follows: 0.35g/L K2HPO4, 0.23g/L KH2PO4, 0.5g/L NH4Cl, 0.5g/L
MgSO4·7H2O, 0.25g/L CaCl2, 2.25g/L NaCl, 0.85g/L NaHCO3, 0.5g/L Na2S·H2O, 10ml/L are micro-
Secondary element solution, 1ml/L vitamin solution；Electrolytic cell head space is CO2:N2The gaseous mixture of=1:4 (n/n)；The microelement
Solution formula is as follows: 1500mg/L FeCl2·4H2O, 70mg/L ZnCl2, 100mg/L MnCl2·4H2O, 6mg/L HBO3,
190mg/L CoCl2·6H2O, 2mg/L CuCl2·H2O, 24mg/L NiCl2·6H2O, NiCl2mg/L NaMo4·2H2O,
HCl (25%) 10ml/L；The vitamin solution formula is as follows: 2mg/L biotin, 2mg/L folic acid, 10mg/L vitamin
B6, 5mg/L vitamin B1, 5mg/L vitamin B2, 5mg/L niacin, 5mg/L pantothenic acid, 0.1mg/L vitamin B12, 5mg/L amino
Benzoic acid, 5mg/L lipoic acid.
CO is restored using above-mentioned apparatus2It is as follows for the method for methane:
Pasteur's methanogen bacterium solution (Methanosarsina barkeri) of 1.5mL (1.5%) is accessed in cathode pool,
Head space is full of CO2And N2Gaseous mixture (1:4).Working electrode (i.e. cathode 4) is mixed using nitric acid-acetic acid of attachment multi-walled carbon nanotube
Condensating fiber film is made.Firstly, being that effective 5% hydrogen peroxide dipping of 50 μm of multi-wall carbon nano-tubes shakes 1h by length, dissolved after dry
In 15% nafion ethanol solution.Ultrasonic treatment 20min keeps multi-walled carbon nanotube evenly dispersed, and multi-walled carbon nanotube is made
Nafion ethanol solution.Then being evenly coated in aperture is on 1.5 μm of nitric acid acetic acid composite fibre films, in 55 DEG C of environment
Middle drying.Make the carbon multi-wall nano tube loaded amount 8mg/cm of nitric acid-acetic acid composite fibre film2.Working electrode is horizontal positioned,
The potential of working electrode is adjusted to -0.6V (vs SHE) to react.
Control group B accesses production Pasteur's methanogen bacterium solution (Methanosarsina of 1.5mL (1.5%) in cathode pool
Barkeri), head space is full of CO2And N2Gaseous mixture (1:4).Working electrode is using traditional carbon cloth electrode, by the potential of working electrode
- 0.6V (vs SHE) is adjusted to be reacted.
Control group C accesses 1.5mL (1.5%) Pasteur's methanogen bacterium solution (Methanosarsina in cathode pool
Barkeri), working electrode is not placed, applying electrical potential is not applied.Head space is full of CO2And N2Gaseous mixture (1:4).
The headspace gas ingredient of three groups of experiments uses gas chromatograph for determination after 78 hours.It as a result is that A group is 8.453 μ
Mol, B group are 6.371 μm of ol.C group methane production is 3.379 μm of ol.It can be seen that under the same conditions, the present invention is significantly
Improve the yield of methane.It is with a wide range of applications.
Embodiment 2:
The embodiment is divided into experimental group A and control group B, C are carried out simultaneously:
Experimental group A is as shown in Figure 1.The Bu Shi methanogen bacterium solution of 5mL (5.0%) is accessed in cathode pool
(Methanobacterium byrantti), head space are full of CO2And N2Gaseous mixture (1:4).Working electrode is using attachment multi wall carbon
The nitric acid of nanotube-acetic acid composite fibre film is made.Firstly, being the effective 5% dioxygen water logging of 10 μm of multi-wall carbon nano-tubes by length
Bubble concussion 1h, is dissolved in 2% nafion ethanol solution after dry.Ultrasonic treatment 1h keeps multi-walled carbon nanotube evenly dispersed,
Multi-walled carbon nanotube nafion ethanol solution is made.Then being evenly coated in aperture is 2 μm of nitric acid acetic acid composite fibre films
On, it is dried in 37 DEG C of environment.Make the carbon multi-wall nano tube loaded amount 4.5mg/cm of nitric acid-acetic acid composite fibre film2。
The potential of working electrode is adjusted to -0.6V (vs SHE) to react.
Control group B accesses the production Bu Shi methanogen bacterium solution (Methanobacterium of 5mL (5.0%) in cathode pool
Byrantti), head space is full of CO2And N2Gaseous mixture (1:4).Working electrode is using traditional carbon cloth electrode, by the potential of working electrode
- 0.6V (vs SHE) is adjusted to be reacted.
Control group C accesses 5mL (5.0%) in cathode pool and produces Bu Shi methanogen bacterium solution (Methanobacterium
Byrantti), working electrode is not placed, applying electrical potential is not applied.Head space is full of CO2And N2Gaseous mixture (1:4).
The headspace gas ingredient of three groups of experiments uses gas chromatograph for determination after 78 hours.It as a result is that A group is 7.471 μ
Mol, B group are 5.643 μm of ol.C group methane production is 1.808 μm of ol.It can be seen that under the same conditions, the present invention is significantly
Improve the yield of methane.It is with a wide range of applications.
Embodiment 3:
The embodiment is divided into experimental group A and control group B, C are carried out simultaneously:
Experimental group A is as shown in the figure.The Heng Shi methanogen bacterium solution of 3mL (3.0%) is accessed in cathode pool
(Methanospirllum hungatei), head space are full of CO2And N2Gaseous mixture (1:4).Working electrode is received using attachment multi wall carbon
The nitric acid of mitron-acetic acid composite fibre film is made.Firstly, being that effective 5% hydrogen peroxide dipping of 2 μm of multi-wall carbon nano-tubes shakes by length
1h is swung, is dissolved in 20% nafion ethanol solution after dry.Ultrasonic treatment 5min keeps multi-walled carbon nanotube evenly dispersed, makes
At multi-walled carbon nanotube nafion ethanol solution.Then being evenly coated in aperture is 0.44 μm of nitric acid acetic acid composite fibre film
On, it is dried in 37 DEG C of environment.Make the carbon multi-wall nano tube loaded amount 6.8mg/cm of nitric acid-acetic acid composite fibre film2。
The potential of working electrode is adjusted to -0.6V (vs SHE) to react.
Control group B accesses the production Heng Shi methanogen bacterium solution (Methanospirllum of 3mL (3.0%) in cathode pool
Hungatei), head space is full of CO2And N2Gaseous mixture (1:4).Working electrode is using traditional carbon cloth electrode, by the potential of working electrode
- 0.6V (vs SHE) is adjusted to be reacted.
Control group C accesses 3mL (3.0%) in cathode pool and produces Heng Shi methanogen bacterium solution (Methanospirllum
Hungatei), working electrode is not placed, applying electrical potential is not applied.Head space is full of CO2And N2Gaseous mixture (1:4).
The headspace gas ingredient of three groups of experiments uses gas chromatograph for determination after 78 hours.It as a result is that A group is 6.845 μ
Mol, B group are 5.331 μm of ol.C group methane production is 1.664 μm of ol.It can be seen that under the same conditions, the present invention is significantly
Improve the yield of methane.It is with a wide range of applications.
Claims (8)
1. a kind of method of micro-reduction carbon dioxide methane phase, which comprises the following steps:
1) building includes the microorganism electrolysis cell of cathode pool and anode pool, includes working electrode, reference electrode in cathode pool；Anode
Pond includes to electrode；It is separated between cathode pool and anode pool with proton exchange membrane；
2) methanogen culture medium is added in cathode pool and anode pool；
3) 1.5~5.0% methanogen bacterium solutions, culture are inoculated in cathode pool；
4) cathode pool load -0.6v (vs SHE) voltage；
5) methane is harvested by cathode pool head space.
2. a kind of method of micro-reduction carbon dioxide methane phase according to claim 1, which is characterized in that step
(1) proton exchange membrane described in is N117 proton exchange membrane.
3. a kind of method of micro-reduction carbon dioxide methane phase according to claim 1, which is characterized in that step
(1) working electrode described in is made of the nitric acid-acetic acid composite fibre film for sticking multi-walled carbon nanotube.
4. a kind of method of micro-reduction carbon dioxide methane phase according to claim 3, which is characterized in that described
Sticking multi-walled carbon nanotube amount on nitric acid-acetic acid composite fibre film is 0.1~10mg/cm2, multi-wall carbon nano-tube length of tube
It is 0.5~50 μm；
Nitric acid -0.2~2 μm of acetic acid composite fibre membrane pore size.
5. a kind of method of micro-reduction carbon dioxide methane phase according to claim 1, which is characterized in that step
(2) formula of the methanogen culture medium described in is as follows: 0.35g/L K2HPO4, 0.23g/L KH2PO4, 0.5g/L NH4Cl,
0.5g/L MgSO4·7H2O, 0.25g/L CaCl2, 2.25g/L NaCl, 0.85g/L NaHCO3, 0.5g/L Na2S·H2O,
10ml/L trace element solution, 1ml/L vitamin solution；Electrolytic cell head space is CO2:N2The gaseous mixture of=1:4 (n/n).
6. a kind of method of micro-reduction carbon dioxide methane phase according to claim 5, which is characterized in that described
Trace element solution formula is as follows: 1500mg/L FeCl2·4H2O, 70mg/L ZnCl2, 100mg/L MnCl2·4H2O, 6mg/
L HBO3, 190mg/L CoCl2·6H2O, 2mg/L CuCl2·H2O, 24mg/L NiCl2·6H2O, 36mg/L NaMo4·
2H2O, HCl (25%) 10ml/L；
The vitamin solution formula is as follows: 2mg/L biotin, 2mg/L folic acid, 10mg/L vitamin B6, 5mg/L vitamin
B1, 5mg/L vitamin B2, 5mg/L niacin, 5mg/L pantothenic acid, 0.1mg/L vitamin B12, 5mg/L aminobenzoic acid, 5mg/L
Lipoic acid.
7. a kind of method of micro-reduction carbon dioxide methane phase according to claim 1, which is characterized in that step
(3) methanogen described in is that including but not limited to Pasteur's methanogen (Methanosarcina barkeri), Bu Shi produces first
Alkane bacterium (Methanobacterium byrantti) and Heng Shi methanogen (Methanospirllum hungatei).
8. a kind of method of micro-reduction carbon dioxide methane phase according to claim 1, which is characterized in that step
(3) methanogen described in is cultivated at room temperature.
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Cited By (5)
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| CN109666703A (en) * | 2019-01-21 | 2019-04-23 | 福建农林大学 | A kind of method of optical drive sarcina methanica reduction carbon dioxide methane phase |
| CN110284150A (en) * | 2019-07-26 | 2019-09-27 | 华东理工大学 | A method of promoting microorganism electrochemical chemical recycling of carbon dioxide methane phase |
| CN113564628A (en) * | 2021-08-13 | 2021-10-29 | 中国科学技术大学 | Metal-free molecular catalyst and preparation method and application thereof |
| DE102020123184A1 (en) | 2020-09-04 | 2022-03-10 | Electrochaea GmbH | Process for the production of a synthetic product, e.g., methane, using methanogenic microorganisms in a microbial electrolytic cell (MEC) by employing a separate nutrient supply strategy |
| CN114699908A (en) * | 2022-01-20 | 2022-07-05 | 中国环境科学研究院 | Activated sludge coupled device and method for fixing carbon dioxide by driving microorganisms with electric energy |
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| CN110284150A (en) * | 2019-07-26 | 2019-09-27 | 华东理工大学 | A method of promoting microorganism electrochemical chemical recycling of carbon dioxide methane phase |
| DE102020123184A1 (en) | 2020-09-04 | 2022-03-10 | Electrochaea GmbH | Process for the production of a synthetic product, e.g., methane, using methanogenic microorganisms in a microbial electrolytic cell (MEC) by employing a separate nutrient supply strategy |
| CN113564628A (en) * | 2021-08-13 | 2021-10-29 | 中国科学技术大学 | Metal-free molecular catalyst and preparation method and application thereof |
| CN114699908A (en) * | 2022-01-20 | 2022-07-05 | 中国环境科学研究院 | Activated sludge coupled device and method for fixing carbon dioxide by driving microorganisms with electric energy |
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