CN108893754A - A kind of device of microorganism electrochemical reduction carbon dioxide - Google Patents
A kind of device of microorganism electrochemical reduction carbon dioxide Download PDFInfo
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- CN108893754A CN108893754A CN201810731819.3A CN201810731819A CN108893754A CN 108893754 A CN108893754 A CN 108893754A CN 201810731819 A CN201810731819 A CN 201810731819A CN 108893754 A CN108893754 A CN 108893754A
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Abstract
The invention discloses a kind of device using microorganism electrochemical reduction carbon dioxide, the problems such as being to solve transmission difficulty and lower microorganism electrochemical cathode material surface area of the prior art solution to carbon dioxide between microorganism.The present invention includes：1) carbon dioxide conversion is organic product by the cathod catalyst that electrochemically reducing carbon dioxide is served as using microorganism；2) porous metals doughnut cathode is used, and external carbon dioxide airbag is connected by gas-guide tube and provides inorganic carbon source for growth of the microorganism on porous metals doughnut cathode.It is larger that specific surface area can be prepared using method of the invention, be conducive to the three-dimensional cathode material that carbon dioxide directly transmits, be conducive to the growth of cathode microbial, electrochemically reducing carbon dioxide installation cost of the present invention is cheap simultaneously, it can use for a long time, capacity usage ratio is high, the large-scale application suitable for carbon dioxide reduction, electrode material preparation and microorganism electrolysis cell.
Description
Technical field
The present invention relates to a kind of devices of electrochemical catalysis reduction carbon dioxide, are suitable for carbon dioxide reduction, electrode material
Material preparation and microorganism electrolysis cell.
Background technique
Currently, global warming and climate change are just causing the concern from world community government and the people.Carbon dioxide row
It puts and is generally acknowledged to have with Global climate change close to linear relationship, thus reduce the carbon dioxide concentration in air, reduce
The use of fossil fuel and develops new energy technology and just becoming modern industry circle and academia makes every effort to solve the problems, such as.Before this
Carbon dioxide recycle and elimination is mainly focused on and is carried out using various porous materials, amino and absorbent lime agent etc.
Carbon dioxide physics and chemisorption storage, however these methods can not change existence form (the carbon oxygen of carbon dioxide completely
Double bond does not fully open), so that it be made to lack possibility (Y.H.Fu, the et for being further converted to high added value organic compound
al.Angewandte Chemie-International Edition,2012,51(14),3364).Use noble metal catalyst
High-temperature catalytic reduction carbon dioxide has equally attracted a lot note that because carbon dioxide conversion can be carbon monoxide, methane by it
Etc. the chemical fuel used that can burn again, but this method equally exists catalyst (palladium, platinum, copper, nickel, iridium, cobalt at high cost
Deng), easily cover the disadvantages of carbon inactivation and energy consumption are high, while institute's conversion product relatively single (single carbon compound) (Z.Y.Hou, et
al.International Journal of Hydrogen Energy,2006,31(5),555)。
To solve the above-mentioned problems, manual simulation's photosynthesis is suggested carry out carbon dioxide conversion, i.e. microorganism electricity
Chemical synthesis.Compared to electrochemically reducing carbon dioxide, there is product to enrich for microorganism electrochemical reduction, electronics utilization efficiency is high
The advantages that, while also because using microorganism as reducing catalyst, relative inexpensiveness.However since carbon dioxide is in water phase
The problems such as middle solubility is lower, and carbon dioxide carbon source needed for microorganism can encounter growth during the growth process is insufficient, microorganism
Growth is restricted to a certain extent, it is difficult to further increase carbon dioxide conversion and organic synthesis yield, this is to using
Certain challenge is proposed for microorganism electrochemical chemical recycling of carbon dioxide.Therefore, it is filled using new electrode materials and electrochemistry
It sets structure and transmits as the task of top priority come efficient, the fine and close growth for promoting microorganism and carbon dioxide to the direct of microorganism.
Summary of the invention
In order to overcome the drawbacks of the prior art, solution is solved to the transmission difficulty of carbon dioxide between microorganism and microorganism electricity
The problems such as chemical cathode material surface area is lower, the present invention propose a kind of microorganism electricity using porous metals doughnut cathode
Chemical system restores the device of carbon dioxide, which can make carbon dioxide gas by porous metals doughnut electrode
It is transmitted directly to avoid the inefficient diffusion of gas up to microorganism end, accelerates microorganism growth and carbon dioxide conversion.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：
A kind of device carbon dioxide reduction being converted into using microorganism electrochemical system organic matter, using double-chamber structure
(proton exchange membrane including anode chamber, cathode chamber and centre), wherein be put into counter electrode material, and with external electrochemistry work
Make station connection forming circuit.
Anode in the anode chamber is to be coated with Pt/C or IrO2/ C catalyst (0.1~0.8mg/cm2) carbon cloth, sun
Pole liquid is buffer, contains 0.3-1.5g/L NH4Cl, 0.3-0.8g/L MgSO4, 0.5-2.5g/L NaCl, 0.01-0.2g/L
CaCl2, 0-0.1g/L KCl, 0.1-0.25g/L KH2PO4, 0-0.35g/L K2HPO4, solvent is water.
It is put into porous metals doughnut cathode in the cathode chamber, and external carbon dioxide airbag is connected by gas-guide tube
(0.2-10L) provides inorganic carbon source for growth of the microorganism on porous metals doughnut cathode.The porous metals are hollow
Fiber cathode outer diameter is 0.8-3mm, and fiber pipe thickness is 0.1-0.5mm, and hole diameter is 0.1-5 μm on fiber tube wall.Yin
Pole liquid contains inorganic carbon source, buffer, microelement and inorganic salts.Catholyte is 0.3-1.5g/L NH4Cl, 0.3-0.8g/L
MgSO4, 0.5-2.5g/L NaCl, 0.01-0.2g/L CaCl2, 0-0.1g/L KCl, 0.1-0.25g/L KH2PO4, 0-
0.35g/L K2HPO4, 1-4g/L NaHCO3, 10ml/L microelement, catholyte pH is 6.5-8.5.Microelement includes
1.5g/L FeCl2·4H2O, 10ml/L 7.7M HCl, 0.006g/L CoCl2·6H2O, 0.036g/L MnCl2·4H2O,
0.024g/L ZnCl2, 0.002g/L H3BO3, 0.19g/L Na2MnO4·2H2O, 0.1g/L NiCl2·6H2O, 0.07g/L
CuCl2·2H2O。
Steps are as follows for porous metals doughnut cathode preparation method：
Step 1：By 1 μm or so of metal powder grain (nickel powder, copper powder or stainless steel particles) and polysulfones, N- crassitude
Ketone is mixed 12~36 hours, and polyvinylpyrrolidone (molecular weight 630000) is added and adjusts solution viscosity, stirs evenly
After vacuumize 12 hours, be compacted solvent under 20psi pressure with nitrogen, finally by Coaxial nozzle squeeze out condensation molding obtain in
Hollow fiber pipe, inside and outside condensing agent are tap water, and agents useful for same is all that analysis is pure.Wherein metal powder grain, polysulfones, N- crassitude
Ketone, polyvinylpyrrolidone mass ratio are 50~60:5~15:25~40:1~5.
Step 2：Hollow fiber conduit is dry, 450-600 DEG C heating 3-6 hours, 800-900 DEG C of logical hydrogen reducing is hollow
Fiber tubing is allowed to metallize.
Step 3：Hollow fiber conduit is cleaned with deionized water and ethyl alcohol, 60-80 DEG C of vacuum drying.
Step 4：Hollow fiber conduit one end is sealed with ethylene oxide, it is as needed that 1-20 root hollow fiber conduit is not close
After sealing end is bundled with conducting wire, rubber gas-guide tube is accessed after conducting wire and fibre pipe contact position coat conducting resinl, it is close with ethylene oxide
Junction is sealed, the cathode construction for the body that can directly ventilate is made.
Above-mentioned apparatus will generate oxygen and hydrogen ion in anode chamber after electrochemical workstation applies certain cathode potential,
Oxygen produces gas collecting bag by anode and collects, and hydrogen ion diffuses to cathode chamber by proton exchange membrane.Carbon dioxide passes through in metal
Hollow fiber pipe is directly enriched in the absorption of the microorganism on cathode, and the hydrogen ion and yin of cathode are diffused in combination with anode chamber
Extremely upper electronics, reduction obtain acetic acid product, and excessive carbon dioxide gas and issuable hydrogen etc. are by cathode gas collection
Bag is collected.
The step of above-mentioned apparatus reduction carbon dioxide obtains acetic acid is as follows：
(1)：After the completion of microorganism electrochemical system assembles, anolyte and catholyte is added in two Room respectively, and in cathode
Room be inoculated with acetogen, under the conditions of applying certain cathode potential (- 0.4V--1.6V vs.Ag/AgCl), to acetogen into
Row domestication, makes it form microbial film in porous metals doughnut cathode surface.
(2)：Cathode chamber blasts a certain proportion of nitrogen and dioxy by the airbag that porous metals doughnut cathode connects
Change carbon mixed gas (N2:CO2=20~80:80~20) microorganism and electricity, are directly reached by the micropore on doughnut electrode
Pole, catholyte interface, inorganic carbon source needed for enabling microorganism to directly obtain growth and is reduced to acetic acid by catalysis.Two
Carbonoxide reduction temperature is controlled at 25~40 DEG C, is generally reaction time 5~20 days, after replace solution, collect cathode chamber
The acetic acid product of generation.
The acetogen is oval mouse spore bacterium (Sporomusa Ovata) or mixed bacterium (mud after anaerobic acclimation).
Beneficial effect of the present invention：
1, carbon dioxide directly can reach microorganism by the micropore on porous metals doughnut electrode, without relying on
It is spread in solution diffusion or electrode, efficient quick.
2, it can avoid using noble metal catalyst as far as possible using metal hollow fiber electrode, and effectively prevent urging
Agent impregnates in the solution the gradually adverse consequences such as loss and ultimate failure for a long time.
3, it is catalyzed using microorganism and reduces carbon dioxide to cheap, capacity usage ratio is high.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of apparatus of the present invention；Wherein, 1- anode, the anode chamber 2- produce gas collecting bag, and 3- anolyte goes out
Mouthful, 4- anolyte import, 5- proton exchange membrane, 6- carbon dioxide airbag, 7- cathode gas collection of products bag, 8-Ag/AgCl ginseng
Than electrode, 9- metal hollow fiber cathode, 10- catholyte inlet and outlet, the anode chamber 11-, 12- cathode chamber, 13- electrochemical operation
It stands.
Fig. 2A is the scanning electron microscope (SEM) photograph of three-dimensional porous nickel doughnut electrode material in embodiment.
Fig. 2 B is the high resolution scanning electron microscope of three-dimensional porous nickel doughnut electrode material surface pattern in embodiment.
Fig. 2 C is the scanning electron microscope (SEM) photograph of three-dimensional porous nickel doughnut electrode material cross section in embodiment.
Fig. 3 is that electric current, acetic acid content and electron theory are converted into acetic acid amount at any time when microorganism electrochemical system is run
Between variation diagram.
Fig. 4 is scanning electron microscope (SEM) photograph of the acetogen biomembrane on cathode.
Specific embodiment
Further illustrate the present invention with reference to the accompanying drawing and by specific embodiment.
Embodiment 1
The present embodiment provides a kind of microorganism electrochemicals to restore carbon dioxide plant, and structural schematic diagram is referring to Fig. 1, anode 1
It is respectively placed in anode chamber 11 and cathode chamber 12 with metal hollow fiber cathode 9, and is immersed in anolyte and catholyte, pass through matter
Proton exchange 5 separates, and anode is connect by electrochemical workstation 13 with cathode, and applies cathode potential -0.6V vs.Ag/AgCl ginseng
Than electrode 8.Three-dimensional porous nickel hollow cathode be located at cathode chamber outside carbon dioxide airbag 6 connect, in airbag be equipped with nitrogen and
Carbon dioxide, volume ratio 80:20.After applying cathode voltage, the issuable gas O of anode2Gas is produced by anode chamber to receive
Collect bag 2 to collect, and the gases such as hydrogen that cathode chamber generates are collected by cathode gas collection of products bag 7.The addition and receipts of catholyte
Collection is unified in catholyte inlet and outlet 10 and carries out, and the addition of anolyte and taking-up are respectively from anolyte import 4 and anolyte outlet 3
It carries out.Anode material is coated with 0.5mg/cm2IrO2The carbon cloth of/C catalyst.
The present embodiment provides a kind of preparation method of three-dimensional porous nickel doughnut electrode material, in the three-dimensional porous nickel
Hollow fiber electrode, outer diameter 1.5mm, fiber pipe thickness are 0.3mm, and hole diameter is about 1.2 μ on doughnut tube wall
m。
Based on the preparation method of above-mentioned three-dimensional porous nickel doughnut electrode material, its step are as follows：
Step 1：Nickel powder particle, polysulfones and N-Methyl pyrrolidone by 1 μm or so are 56 in mass ratio:12:30 carry out
It is mixed 18 hours, mixture is with mass ratio 49:1, which adds the polyvinylpyrrolidone that molecular weight is 630000, adjusts solution
Viscosity vacuumizes 12 hours after mixing evenly, is compacted solvent under 20psi pressure with nitrogen, squeezes out finally by Coaxial nozzle
Condensation molding obtains doughnut tubing, and inside and outside condensing agent is tap water, and agents useful for same is all that analysis is pure；
Step 2：Diamond heating macromolecule chemical combination into 560 DEG C of removal tubing will be put into after the drying of doughnut tubing
Object, heating time are 6 hours.Then in 810 DEG C of logical hydrogen reducing nickel doughnut tubing, it is allowed to metallize.
Step 3：After porous nickel hollow fiber conduit deionized water and ethyl alcohol are cleaned, 60 DEG C are dried in vacuo to get institute is arrived
Three-dimensional porous nickel hollow cathode material is stated, as shown in Fig. 2A~Fig. 2 C.
Step 4：Three-dimensional porous nickel hollow tube one end is sealed with ethylene oxide, more nickel hollow tube unsealing ends are with leading
After line binding, rubber gas-guide tube is accessed, is sealed the joint with ethylene oxide, the cathode material for the body that can directly ventilate, such as Fig. 1 is made
It is shown.
Domestication and bio-film colonization of the acetogen Sporomusa Ovata on cathode then carry out under hydrogen promotion,
The production acetic acid that 125ml anolyte and 125ml contain 10v/v% is separately added into microorganism electrochemical device anode chamber and cathode chamber
The catholyte of bacterium inoculation liquid, in the cathodic compartment by gas volume than 40:50:10 are passed through H2/N2/CO2, apply cathode potential -0.6V
Vs.Ag/AgCl, each periodic duty 7-8 days then show to tame successfully until acetic acid content is basically unchanged.
Anolyte ingredient used is：0.5g/L NH4Cl, 0.25g/L MgSO4, 2.25g/L NaCl, 0.1g/L CaCl2,
0.23g/L KH2PO4, 0.35g/L K2HPO4, solvent is water.
Catholyte is 0.5g/L NH4Cl, 0.25g/L MgSO4, 2.25g/L NaCl, 0.1g/L CaCl2,0.23g/L
KH2PO4, 0.35g/L K2HPO4, 1g/L NaHCO3, 10ml/L microelement, catholyte pH is 6.5-8.5.Microelement includes
1.5g/L FeCl2·4H2O, 10ml/L 7.7M HCl, 0.006g/L CoCl2·6H2O, 0.036g/L MnCl2·4H2O,
0.024g/L ZnCl2,0.002g/L H3BO3, 0.19g/L Na2MnO4·2H2O, 0.1g/L NiCl2·6H2O, 0.07g/L
CuCl2·2H2O。
After acetogen is tamed successfully, fresh anolyte and catholyte are replaced, and pass through the titanium dioxide outside cathode chamber
It is 80 that carbon airbag, which constantly blasts volume ratio,:20 nitrogen/carbon dioxide gas mixture provides inorganic carbon source for acetogen, and
Apply cathode potential -0.6V vs.Ag/AgCl.Acetic acid concentration is continuously increased in catholyte, reaches 1.46 ± 0.04mM, and acetic acid produces
Rate reaches 144.9 ± 4.2mM/d/m2, coulombic efficiency has also exceeded 75%, as shown in figure 3, being much higher than same cathode potential and yin
Acetic acid producing rate (30 ± 7mM/m of carbon cloth biological-cathode of carbon material biological-cathode under atomic biotic factor2/ day, graphite rod biology
Cathode 76mM/m2/day).Meanwhile SEM figure (such as Fig. 4) shows that Sporomusa ovata bacterium is uniformly distributed in porous-metal nickel
On doughnut cathode, the good biocompatibility of cathode is shown.It can be seen that compared with two-dimentional biological-cathode, the present apparatus
In carbon dioxide gas directly transmitted by porous-metal nickel doughnut electrode greatly improve microorganism electrochemical system
Restore the rate that carbon dioxide produces acetic acid.
The present invention has following advantage：
1. three-dimensional porous metallic fiber electrode aperture is uniform, divide after being conducive to carbon dioxide conversion city organic matter with microorganism
From；
2. three-dimensional porous metallic fiber electrode ensure that carbon dioxide gas is directly transferred to microorganism end, dioxy is accelerated
Change carbon rate of reduction, while without carrying out basification to carbon dioxide, effectively reducing cost；
3. three-dimensional porous metallic fiber electrode can form conductive fiber in conjunction with current hollow ceramic tunica fibrosa packaging technology
Membrane module is conducive on a large scale restore carbon dioxide.
The above is only a preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (3)
1. a kind of device using microorganism electrochemical reduction carbon dioxide, the proton including anode chamber, cathode chamber and centre
Exchange membrane is put into counter electrode material in anode chamber, cathode chamber, and connect forming circuit with external electrochemical workstation, special
Sign is：
Anode in the anode chamber is to be coated with Pt/C or IrO2The carbon cloth of/C catalyst, catalyst loadings are 0.1~0.8mg/
cm2, anolyte is buffer, and anolyte ingredient is 0.3~1.5g/L NH4Cl, 0.3~0.8g/L MgSO4, 0.5~2.5g/L
NaCl, 0.01~0.2g/L CaCl2, 0~0.1g/L KCl, 0.1~0.25g/L KH2PO4, 0~0.35g/L K2HPO4, molten
Agent is water；
Porous metals doughnut cathode is put into the cathode chamber, and it is micro- for connecting external carbon dioxide airbag by gas-guide tube
Growth of the biology on cathode provides inorganic carbon source；The cathode outer diameter be 0.8~3mm, fiber pipe thickness be 0.1~
0.5mm, the bore dia on fiber tube wall are 0.1~5 μm；There is 0.3~1.5g/L NH in catholyte4Cl, 0.3~0.8g/L
MgSO4, 0.5~2.5g/L NaCl, 0.01~0.2g/L CaCl2, 0~0.1g/L KCl, 0.1~0.25g/L KH2PO4、0
~0.35g/L K2HPO4, 1~4g/L NaHCO3, 10ml/L microelement, catholyte pH be 6.5~8.5；Microelement includes
1.5g/L FeCl2·4H2O、10ml/L 7.7M HCl、0.006g/L CoCl2·6H2O、0.036g/L MnCl2·4H2O、
0.024g/L ZnCl2、0.002g/L H3BO3、0.19g/L Na2MnO4·2H2O、0.1g/L NiCl2·6H2O、0.07g/L
CuCl2·2H2O。
2. the device according to claim 1 using microorganism electrochemical reduction carbon dioxide, it is characterised in that described more
Mesoporous metal doughnut cathode preparation method is as follows：
Step 1：1 μm of metal powder grain and polysulfones, N-Methyl pyrrolidone are mixed 12~36 hours, molecular weight is added
It for 630000 polyvinylpyrrolidone, vacuumizes after mixing evenly 12 hours, is compacted solvent under 20psi pressure with nitrogen,
Condensation molding is squeezed out finally by Coaxial nozzle and obtains hollow fiber conduit, and inside and outside condensing agent is tap water, and agents useful for same is all point
It analyses pure；Wherein metal powder grain, polysulfones, N-Methyl pyrrolidone, polyvinylpyrrolidone mass ratio are 50~60:5~15:25~
40:1~5；
Step 2：Hollow fiber conduit is dry, and 450~600 DEG C are heated 3~6 hours, 800~900 DEG C of logical hollow fibres of hydrogen reducing
Tubing is tieed up, is allowed to metallize；
Step 3：Hollow fiber conduit is cleaned with deionized water and ethyl alcohol, 60~80 DEG C of vacuum drying；
Step 4：Hollow fiber conduit one end is sealed with ethylene oxide, 1~20 hollow fiber conduit unsealing end is tied with conducting wire
After tying up, rubber gas-guide tube is accessed after conducting wire and fibre pipe contact position coat conducting resinl, is sealed the joint, is made with ethylene oxide
Can directly be ventilated the cathode construction of body.
3. the device according to claim 2 using microorganism electrochemical reduction carbon dioxide, it is characterised in that the step
Metal powder grain in rapid one is nickel powder, copper powder or stainless steel particles.
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