CN103290425A - Hydrogen-producing microbial electrolytic cell and biological cathode domestication method - Google Patents
Hydrogen-producing microbial electrolytic cell and biological cathode domestication method Download PDFInfo
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Abstract
A biological cathode domestication method for a biological cathode-type hydrogen-producing microbial electrolytic cell is provided by the invention, and is characterized by comprising: A) culturing an anode electrogenic microbial population under a microbial fuel cell mode; B) domesticating an anode hydrogen-consuming microbial population under a microbial electrolytic cell hydrogen-producing mode; C) carrying out domestication culturing of a cathode hydrogen-producing microbe under a three-electrode mode. On the basis of a further aspect of the invention, a biological cathode-type microbial electrolytic cell (400) is formed by combination of the biological anode obtained by the step A) and the biological cathode obtained by domestication culturing in the step C). The invention also provides the biological cathode-type hydrogen-producing microbial electrolytic cell, and the microbial electrolytic cell comprises the biological anode obtained by the step A) and the biological cathode obtained by domestication culturing in the step C).
Description
Technical field
The invention belongs to the microorganism electrochemical technical field, relate to a kind of product hydrogen microorganism electrolysis cell and biological-cathode acclimation method thereof.
Background technology
Along with expanding economy, people strengthen day by day to the demand of the energy, and Nonrenewable energy resources such as coal, oil, Sweet natural gas can not satisfy the growing needs of people, and the use of these Nonrenewable energy resources is also very serious to the pollution that environment causes simultaneously.Therefore greatly developing renewable energy source, walk sustainable development path, satisfy the low-carbon economy development, has been mandatory policy.Hydrogen has become one of energy carrier that is most widely used with its cleaning, characteristics such as efficient, renewable, causes extensive concern at home and abroad.Present industrialized hydrogen production process is Sweet natural gas or tail gas separating and preparing hydrogen and water electrolysis method hydrogen manufacturing, but cost is higher, and it is bigger to consume energy.Traditional fermentative hydrogen production has cleaning, safety, and advantages such as less energy-consumption, but raw material availability is lower.Microorganism electrolysis cell then is the bioenergy technology of utilizing renewable biomass hydrogen manufacturing that grows up on the microbiological fuel cell basis.Compare the traditional zymotic technology, the microorganism electrolysis cell technology overcomes " fermentation bottleneck ", and energy transformation ratio can reach more than 60%, when handling organic waste water, realizes chemical energy, electric energy, the conversion between the Hydrogen Energy three.
Microorganism electrolysis cell hydrogen manufacturing is to utilize the electrogenesis microorganism at the anodic oxidation organism, produces electronics and proton, electronics and proton under impressed voltage drives, the cathode catalysis hydrogen producing.For reducing the negative electrode overpotential, improve negative electrode hydrogen manufacturing speed, platinum commonly used, precious metals such as palladium are as catalyzer.But these catalyzer costs are than higher, and long-time use easily causes shortcomings such as poisoning of catalyst, and with microorganism as catalyzer, then avoid the deficiency of precious metal, improve the microorganism electrolysis cell economy, for the microorganism electrolysis cell practical application is laid a good foundation.
Summary of the invention
According to an aspect of the present invention, provide a kind of biological-cathode to produce the biological-cathode acclimation method of hydrogen microorganism electrolysis cell, it is characterized in that comprising:
A) under the microbiological fuel cell pattern, cultivate anode electrogenesis microbial population,
B) the domestication anode is bitten the hydrogen microbial population under microorganism electrolysis cell hydrogen manufacturing pattern,
C) domestication is cultivated negative electrode and is produced the hydrogen microorganism under three electrode modes.
According to a further aspect of the present invention, with above-mentioned steps A) in the biological anode and the above-mentioned steps C that obtain) in the domestication biological-cathode combination of cultivating, constitute biological-cathode type microorganism electrolysis cell (400).
According to another aspect of the present invention, provide a kind of product hydrogen biological-cathode type microorganism electrolysis cell, it is characterized in that described product hydrogen biological-cathode type microorganism electrolysis cell comprises:
Above-mentioned steps A) the biological anode that obtains in and
Above-mentioned step C) biological-cathode that domestication is cultivated in.
According to a further aspect of the present invention, operation mentioned microorganism electrolyzer under the impressed voltage room temperature environment of 0.6-1.0V, and when current density begins to descend, with the solution in new first solution replacing microorganism electrolysis cell, realize microorganism electrolysis cell biological-cathode catalyzing manufacturing of hydrogen
Wherein
Every liter of component of described first solution is: 1g sodium acetate, 0.31g NH
4Cl, 0.52g KCl, 13.44gNaHCO
3, 2.22g NaH
2PO
42H
2O, 9.20g Na
2HPO
412H
2O, the 25ml nutrient salt solution, the vitamin solution of 50ul, surplus is distilled water;
Wherein: every liter of component of described nutritive salt is: 2.3g EDTA, 6.15g MgSO
47H
2O, 0.5gMnSO
4H
2O, 1g NaCl, 0.1g FeSO
47H
2O, 0.076g CaCl
2, 0.1g CoCl
26H
2O, 0.13g ZnCl
2, 0.01g CuSO
45H
2O, 0.01g KAl (SO
4)
212H
2O, 0.01g H
3BO
3, 0.022g (NH
4)
6Mo
7O
244H
2O, 0.024g NiCl
26H
2O, 0.025g Na
2WO
42H
2O.
Description of drawings
Fig. 1 is the synoptic diagram of the structure of the microbiological fuel cell that adopts of one embodiment of the present of invention.
Fig. 2 is according to an embodiment of the invention, be used for the structural representation that the domestication anode is bitten the microorganism electrolysis cell of hydrogen microbial population.
Fig. 3 is the structural representation of the half-cell that domestication cultivation negative electrode product hydrogen Institute of Micro-biology adopts under three electrode modes according to an embodiment of the invention.
Fig. 4 is structural representation according to an embodiment of the invention, that be used for the biological-cathode type microorganism electrolysis cell of realization biological-cathode type microorganism electrolysis cell hydrogen manufacturing.
During Fig. 5 has shown according to one embodiment of present invention microorganism electrolysis cell under impressed voltage 0.8V condition current density with cycle of operation variation relation (wherein current density is based on liquor capacity).
Represented among Fig. 6 that biological-cathode is tamed stage current density variation relation in time in the three electrode mode half-cells in one embodiment of the present of invention.
Fig. 7 has represented the result of cyclic voltammetry (CV) test organisms negative electrode/blank carbon felt in one embodiment of the present of invention.
Fig. 8 has shown the result of biological-cathode performance test in one embodiment of the present of invention, that is: current density/hydrogen-producing speed is with cathode electrode potential variation relation (wherein current density is based on liquor capacity).
Embodiment
Biological-cathode type according to an embodiment of the invention produces the biological-cathode acclimation method of hydrogen microorganism electrolysis cell, may further comprise the steps:
A) under the microbiological fuel cell pattern, cultivate anode electrogenesis microbial population (structure of microbiological fuel cell is shown in the synoptic diagram of Fig. 1),
B) the domestication anode is bitten hydrogen microbial population (structure at microorganism electrolysis cell shows as schematically shown in Figure 2) under microorganism electrolysis cell hydrogen manufacturing pattern,
C) domestication is cultivated negative electrode and is produced hydrogen microorganism (structural representation is as shown in Figure 3) under three electrode modes,
D) with steps A) in the biological anode and the step C that obtain) in the biological-cathode cultivated of domestication be combined into biological-cathode type microorganism electrolysis cell, this biological-cathode type microorganism electrolysis cell of operation under impressed voltage and room temperature environment.
Embodiment 1: cultivate anode electrogenesis microbial population under the microbiological fuel cell pattern
The structure of the microbiological fuel cell that adopts (100) is shown in the synoptic diagram of Fig. 1.Concrete steps:
First solution (composition sees below) is joined microbiological fuel cell (100), and the anode of microbiological fuel cell (100) adopts the carbon felt as base mateiral, and negative electrode adopts the acetylene black carbon film and brushes 0.5mg-Pt/cm
2Catalyzer, in the closed circuit system, insert external resistance R=1000 Ω, batch formula operation, the voltage at continuous monitoring external resistance R two ends;
When in each cycle of operation, the output voltage of microbiological fuel cell (100) (external resistance R both end voltage) constantly descends and when being lower than 100mV, with the solution in fresh first solution replacing microbiological fuel cell (100), repeat a plurality of cycles and change solution, maximum output voltage up to microbiological fuel cell (100) maintains 500～600mV, and biological anode starts and finishes.
Every liter of component of described first solution is: 1g sodium acetate, 0.31g NH
4Cl, 0.52g KCl, 13.44gNaHCO
3, 2.22g NaH
2PO
42H
2O, 9.20g Na
2HPO
412H
2O, the 25ml nutrient salt solution, the vitamin solution of 50ul, surplus is distilled water;
Wherein: every liter of component of described nutritive salt is: 2.3g EDTA, 6.15g MgSO
47H
2O, 0.5gMnSO
4H
2O, 1g NaCl, 0.1g FeSO
47H
2O, 0.076g CaCl
2, 0.1g CoCl
26H
2O, 0.13g ZnCl
2, 0.01g CuSO
45H
2O, 0.01g KAl (SO
4)
212H
2O, 0.01g H
3BO
3, 0.022g (NH
4)
6Mo
7O
244H
2O, 0.024g NiCl
26H
2O, 0.025g Na
2WO
42H
2O;
Embodiment 2: the domestication anode is bitten the hydrogen microbial population under the microorganism electrolysis cell hydrogen manufacturing pattern
The electrolyser construction signal of adopting shows as schematically shown in Figure 2.Concrete steps:
B1) the biological anode that starts in the steps A is forwarded to microorganism electrolysis cell (200) (Fig. 2), as the biological anode of electrolyzer (200).The negative electrode of microorganism electrolysis cell (200) adopts carbon cloth as base mateiral, load 0.5mg-Pt/cm
2Catalyzer.After adding first solution, between the biological anode of microorganism electrolysis cell (200) and chemical negative electrode, apply 0.6V voltage, move in following batch formula operation of room temperature environment, and the strength of current of continuous monitoring electrolyzer (200).When in each batch formula cycle, microorganism electrolysis cell (200) current density from the stable platform rapid drawdown to 100-200A/m
3The time, with the solution in new first solution replacing microorganism electrolysis cell (200), repeat a plurality of cycles and change solution, begin to produce hydrogen up to microorganism electrolysis cell (200).When microorganism electrolysis cell (200) can be stable product hydrogen 10 all after dates, the voltage between biological anode and the chemical negative electrode progressively is increased to 0.7V from 0.6V, 0.8V;
B2) collect microorganism electrolysis cell (200) institute aerogenesis body through the anaerobism bag; In entire reaction period, keep being communicated with and not exhaust of collection and confinement of gases anaerobism bag and reactor microorganism electrolysis cell (200);
B3) as shown in Figure 5, microorganism electrolysis cell (200) is under impressed voltage 0.8V condition, and after 10 cycles of operation, the current density of electrolyzer (200) constantly rises, and when running to 40 cycles, current density reaches 500-600A/m
3, and tend towards stability proper extension periodic reaction time this moment.When the current density of microorganism electrolysis cell (200) from platform electric current (500-600A/m
3) drop to 100-200A/m
3The time, continue between the biological anode of microorganism electrolysis cell (200) and chemical negative electrode, to apply the voltage of 0.8V, make microorganism electrolysis cell low current district work 4-6 hour;
Fig. 5 shown microorganism electrolysis cell in the present embodiment (200) under impressed voltage 0.8V condition current density with cycle of operation variation relation (wherein current density is based on liquor capacity).B4) repeating step B2) and B3) 15 batches, finish and bite the biological anode microbial acclimation of hydrogen;
Embodiment 3: domestication is cultivated negative electrode and is produced the hydrogen microorganism under three electrode modes
The structure of the three electrode mode half-cells that adopt shows as schematically shown in Figure 3.Concrete steps:
C1) with step B) in biological anode as negative electrode, the acetylene black carbon film constitutes half-cell (300) as chemical anode.
C2) add second solution (composition sees below) at half-cell, with the working electrode electromotive force constant at-1.1V(with respect to saturated calomel electrode), a side of chemical anode feeds hydrogen, moves under the room temperature environment.When being reduced to 80A/m under half-cell (300) current density in each cycle
3The time, with the solution in new second solution replacing half-cell (300), repeat a plurality of cycles and change solution, obtain stable electric current up to half-cell (300).As shown in Figure 6, biological-cathode in half-cell (300) initial 0-25 hour, current density has slow downtrending, when electric current drops to 80A/m
3When following, change second solution of half-cell (300), continuous service half-cell (300), when about 180 hours of operation, current density reached 100A/m
3, current density tends towards stability, and continues to produce hydrogen under this pattern, namely finishes the domestication cultivation that biological-cathode produces the hydrogen microorganism.
Represented in the three electrode mode half-cells of embodiment 3 biological-cathode domestication stage current density variation relation in time among Fig. 6; Wherein, solid line represents the variation relation of biological-cathode, and dotted line represents the variation relation that blank negative electrode is the blank carbon felt of lifeless matter catalyzer; Current density is based on cloudy liquor capacity; Solution is changed in the arrow representative.
Every liter of component of described second solution is: 0.31g NH
4Cl, 0.52g KCl, 13.44g NaHCO
3, 2.22g NaH
2PO
42H
2O, 9.20g Na
2HPO
412H
2O, the 25ml nutrient salt solution, the vitamin solution of 50ul, surplus is distilled water;
Wherein: every liter of component of described nutritive salt is: 2.3g EDTA, 6.15g MgSO
47H
2O, 0.5gMnSO
4H
2O, 1g NaCl, 0.1g FeSO
47H
2O, 0.076g CaCl
2, 0.1g CoCl
26H
2O, 0.13g ZnCl
2, 0.01g CuSO
45H
2O, 0.01g KAl (SO
4)
212H
2O, 0.01g H
3BO
3, 0.022g (NH
4)
6Mo
7O
244H
2O, 0.024g NiCl
26H
2O, 0.025g Na
2WO
42H
2O;
Fig. 7 has represented the result of the biological-cathode/blank carbon felt of cyclic voltammetry (CV) test half-cell (300) in the present embodiment.Among Fig. 7, real point represents the test result of biological-cathode, and imaginary point represents the test result that blank negative electrode is the blank carbon felt of lifeless matter catalyzer; Sweep speed and be 50mV/s, current density is based on liquor capacity.
By the blank carbon felt under cyclic voltammetry (CV) test organisms negative electrode and the equal conditions, as shown in Figure 7, further the biological-cathode electrocatalysis characteristic is tested, draw contain biological catalyst in identical scanning area biological-cathode electrochemical double layer area obviously greater than the electrochemical double layer area of the negative electrode of blank carbon felt, and can produce bigger current density, the biology catalytic activity of cathode microbial is better as can be seen, biocatalysis has taken place produced the hydrogen effect.In addition, from Fig. 7, can draw, when electromotive force be lower than-1.3V(is with respect to saturated calomel reference electrode) time, blank negative electrode (being the blank carbon felt of lifeless matter catalyzer) self can produce current density 100A/m
3, the liberation of hydrogen effect can take place, so the electrode potential of biological-cathode should be chosen in the potential range of the catalytic hydrogen evolution of avoiding carbon felt self.
Fig. 8 has shown biological-cathode electrocatalysis characteristic test result in the present embodiment, that is: current density/hydrogen-producing speed is with cathode electrode potential variation relation (wherein current density is based on liquor capacity).
As shown in Figure 8, by the control cathode electromotive force, the hydrogen performance is produced in biological-cathode catalysis to be characterized, reduction along with cathode electrode potential, biological-cathode (comparing with blank carbon felt) current density and hydrogen-producing speed all have remarkable increase, illustrate that low cathode electrode potential is conducive to biocatalysis and produces hydrogen, cathode electrode potential-1.1～-1.3V(is with respect to saturated calomel electrode) between the scope, biological-cathode catalyzing manufacturing of hydrogen better performances.
Embodiment 4: realize the hydrogen manufacturing of biological-cathode type microorganism electrolysis cell
The structure of biological-cathode type microorganism electrolysis cell shows as schematically shown in Figure 4.Concrete steps:
With biological anode and the step C that obtains in the steps A) in the biological-cathode cultivated of domestication be combined into biological-cathode type microorganism electrolysis cell (400), under the impressed voltage of 0.6-1.0V and room temperature environment, move microorganism electrolysis cell (400), when current density begins to descend, with the solution in new first solution replacing microorganism electrolysis cell (400), realize microorganism electrolysis cell (400) biological-cathode catalyzing manufacturing of hydrogen, hydrogen-producing speed is as shown in the table:
Wherein, hydrogen-producing speed Q
H2=V
H2/ (V
LT); V
H2Collect the volume of hydrogen for collecting bag; V
LThe volume of reactor solution in the biological-cathode type microorganism electrolysis cell (400); The reaction times of T one-period.
Claims (10)
1. biological-cathode acclimation method that produces the hydrogen microorganism electrolysis cell is characterized in that comprising:
A) under the microbiological fuel cell pattern, cultivate anode electrogenesis microbial population,
B) the domestication anode is bitten the hydrogen microbial population under microorganism electrolysis cell hydrogen manufacturing pattern,
C) domestication is cultivated negative electrode and is produced the hydrogen microorganism under three electrode modes.
2. according to the method for claim 1, it is characterized in that described steps A) comprising:
First solution is joined microbiological fuel cell (100), and described microbiological fuel cell (100) comprises biological anode and chemical negative electrode,
In the closed circuit system, insert external resistance (R), batch formula operation, the voltage at continuous monitoring external resistance (R) two ends,
When in each cycle of operation, the output voltage of microbiological fuel cell (100) is that the voltage at external resistance (R) two ends constantly drops to when being lower than 100mV, with the solution in fresh first solution replacing microbiological fuel cell (100), repeat a plurality of cycles, maximum output voltage up to microbiological fuel cell (100) can maintain 500～600mV, and biological anode starts and finishes.
3. according to the method for claim 2, it is characterized in that
The described biological anode of microbiological fuel cell (100) adopts the carbon felt as base mateiral, and described chemical negative electrode adopts the acetylene black carbon film and brushes 0.5mg-Pt/cm
2Catalyzer.
4. according to the method for claim 2 or 3, it is characterized in that
Every liter of component of described first solution is: 1g sodium acetate, 0.31g NH
4Cl, 0.52g KCl, 13.44gNaHCO
3, 2.22g NaH
2PO
42H
2O, 9.20g Na
2HPO
412H
2O, the 25ml nutrient salt solution, the vitamin solution of 50ul, surplus is distilled water;
Wherein: every liter of component of described nutritive salt is: 2.3g EDTA, 6.15g MgSO
47H
2O, 0.5gMnSO
4H
2O, 1g NaCl, 0.1g FeSO
47H
2O, 0.076g CaCl
2, 0.1g CoCl
26H
2O, 0.13g ZnCl
2, 0.01g CuSO
45H
2O, 0.01g KAl (SO
4)
212H
2O, 0.01g H
3BO
3, 0.022g (NH
4)
6Mo
7O
244H
2O, 0.024g NiCl
26H
2O, 0.025g Na
2WO
42H
2O.
5. according to the method for claim 1, it is characterized in that described step B) comprising:
B1）
With steps A) in the biological anode that starts be forwarded to microorganism electrolysis cell (200), as the biological anode of microorganism electrolysis cell (200), wherein said microorganism electrolysis cell (200) has chemical negative electrode,
After adding first solution, between the biological anode of microorganism electrolysis cell (200) and chemical negative electrode, apply 0.6V voltage, move in following batch formula of room temperature environment, and the strength of current of continuous monitoring electrolyzer (200),
In each batch formula cycle, when microorganism electrolysis cell (200) current density begins from the stable platform rapid drawdown to 100-200A/m
3The time, the solution with in fresh first solution replacing microorganism electrolysis cell (200) repeats a plurality of cycles, begins to produce hydrogen up to microorganism electrolysis cell (200),
When microorganism electrolysis cell (200) can be stable product hydrogen 5-10 week after date, the impressed voltage of microorganism electrolysis cell (200) progressively is increased to 0.7V from 0.6V, 0.8V.
6. according to the method for claim 5, it is characterized in that described step B) further comprise:
B2) collect microorganism electrolysis cell (200) institute aerogenesis body through the anaerobism bag; In entire reaction period, keep collecting the anaerobism bag of gas and being communicated with and not exhaust of microorganism electrolysis cell (200);
B3) under the impressed voltage of microorganism electrolysis cell (200) at 0.8V, current density drops to 100-200A/m from the platform electric current
3The time, continue to apply at microorganism electrolysis cell (200) voltage of 0.8V, make microorganism electrolysis cell (200) low current district work 4-6 hour;
B4) repeating step B2) and B3) 10-20 batch, finish and bite the biological anode microbial acclimation of hydrogen;
Wherein, the chemical negative electrode of microorganism electrolysis cell (200) adopts carbon cloth as base mateiral, load 0.5mg-Pt/cm
2Catalyzer.
7. according to the method for claim 1, it is characterized in that described step C) comprising:
C1) with step B) in biological anode be forwarded to half-cell (300), anode is chemical anode,
C2) in half-cell (300), add second solution, with the working electrode electromotive force constant with respect to described reference electrode-1.1～-1.3V, chemical anode feeds hydrogen, moves half-cell (300) under the room temperature environment,
The current density of half-cell in each cycle (300) drops to and is lower than 80A/m
3The time, the solution with in fresh second solution replacing half-cell (300) repeats a plurality of cycles, reaches 100A/m up to current density
3And tend towards stability, and under this pattern, continue to produce hydrogen, namely finish the domestication cultivation that biological-cathode produces the hydrogen microorganism.
Every liter of component of described second solution is: 0.31g NH
4Cl, 0.52g KCl, 13.44g NaHCO
3, 2.22g NaH
2PO
42H
2O, 9.20g Na
2HPO
412H
2O, the 25ml nutrient salt solution, the vitamin solution of 50ul, surplus is distilled water;
Wherein: every liter of component of described nutritive salt is: 2.3g EDTA, 6.15g MgSO
47H
2O, 0.5gMnSO
4H
2O, 1g NaCl, 0.1g FeSO
47H
2O, 0.076g CaCl
2, 0.1g CoCl
26H
2O, 0.13g ZnCl
2, 0.01g CuSO
45H
2O, 0.01g KAl (SO
4)
212H
2O, 0.01g H
3BO
3, 0.022g (NH
4)
6Mo
7O
244H
2O, 0.024g NiCl
26H
2O, 0.025g Na
2WO
42H
2O.
8. according to the method for claim 7, it is characterized in that
Described chemical anode is the acetylene black carbon film and brushes 0.5mg-Pt/cm
2Catalyzer, described reference electrode is saturated calomel electrode.
9. a biological-cathode type produces hydrogen microorganism electrolysis cell (400), it is characterized in that described biological-cathode type produces hydrogen microorganism electrolysis cell (400) and comprising:
As the described steps A of one of claim 1-8) in the biological anode that obtains and
The described step C of one of claim 1-8) biological-cathode that domestication is cultivated in.
10. the biological-cathode type according to claim 9 produces hydrogen microorganism electrolysis cell (400), it is characterized in that:
Operation described microorganism electrolysis cell (400) under the impressed voltage of 0.6-1.0V and room temperature environment,
When the current density of microorganism electrolysis cell (400) begins to descend, with the solution in fresh first solution replacing microorganism electrolysis cell (400), realize microorganism electrolysis cell (400) biological-cathode catalyzing manufacturing of hydrogen,
Wherein
Every liter of component of described first solution is: 1g sodium acetate, 0.31g NH
4Cl, 0.52g KCl, 13.44gNaHCO
3, 2.22g NaH
2PO
42H
2O, 9.20g Na
2HPO
412H
2O, the 25ml nutrient salt solution, the vitamin solution of 50ul, surplus is distilled water;
Wherein: every liter of component of described nutritive salt is: 2.3g EDTA, 6.15g MgSO
47H
2O, 0.5gMnSO
4H
2O, 1g NaCl, 0.1g FeSO
47H
2O, 0.076g CaCl
2, 0.1g CoCl
26H
2O, 0.13g ZnCl
2, 0.01g CuSO
45H
2O, 0.01g KAl (SO
4)
212H
2O, 0.01g H
3BO
3, 0.022g (NH
4)
6Mo
7O
244H
2O, 0.024g NiCl
26H
2O, 0.025g Na
2WO
42H
2O.
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