CN103413948B - A kind of microorganism electrolysis cell modification biological cathode preparation method and application thereof - Google Patents
A kind of microorganism electrolysis cell modification biological cathode preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a kind of microorganism electrolysis cell modification biological cathode preparation method and application thereof, with MWNT, tourmaline and PANI combination electrode for MEC modification biological negative electrode prepared by base material; First by MWNT and the mixing of tourmaline powder ball milling, add solvent, aniline and ammonium persulfate, stirring reaction under condition of ice bath, washing and drying obtains MWNT/ tourmaline/PANI compound; Compound and binding agent and acetone are mixed with and obtain MWNT/ tourmaline/PANI combination electrode, conventionally biofilm is tamed as MFC anode after natural air drying, then move to MEC negative electrode, finally construct MWNT/ tourmaline/PANI modification biological negative electrode.The multi-functional that the modification biological negative electrode that the present invention prepares has stimulating organism catalytic activity, hydrogen is produced in chemically reinforced biological catalysis, conductivity is high, with low cost, for the scale application realizing the synchronous waste water treatment of MEC and product hydrogen provides technical support.
Description
Technical field
The invention belongs to new forms of energy and new material application technical field, be specifically related to carbon nano-tube/tourmaline/polyaniline-modified biological-cathode application in microorganism electrolysis cell and preparation method thereof.
Background technology
Along with social progress and economic development, the energy crisis in global range and problem of environmental pollution highlight day by day, do not rely on fossil fuel to become the trend in epoch to the energy demand meeting the mankind in continuable, eco-friendly mode.
MEC is the new technology of a kind of biological hydrogen production grown up in recent years, as a kind of biological biodegradable organic that act synergistically with electrochemistry, while chemical energy can be become the new bio process technology of Hydrogen Energy, MEC causes increasing concern.Its basic functional principle is under the effect of additional low-tension supply, and in the electrochemically active microbial degradation aqueous solution adhered to by anode surface, organic substance generates CO
2, H
+and electronics, the electronics of generation is delivered to negative electrode through external circuit; H
+spread by proton membrane or directly arrive negative electrode, obtaining electronics at cathode surface and be reduced into hydrogen.
MEC cathod catalyst is one of technical problem of most critical, and Pt is used widely at MEC because having good catalytic performance, but it is expensive, constrains the industrial application of MEC.For this reason, the cathod catalyst screening of high efficiency low cost is the emphasis studied with preparation.Some alloy electrodes, as Ni-W-P alloy electrode, Ni-Mo alloy copper sheet, Ni-Fe-Mo alloy, Co-Ni alloy etc. have stronger redox catalysis activity, be expected to alternative Pt catalyst (document WaterScienceandTechnology, 2011,63 (3): 440-448; InternationalJournalofHydrogenEnergy, 2011,36:10482-10489), but due to its manufacture method, the limiting factors such as pulp furnish, make its application in MEC be subject to certain restrictions.Metal oxide and sulfide are more potential cathod catalyst (document InternationalJournalofHydrogenEnergy, 2010,35:3227-3233; InternationalJournalofHydrogenEnergy, 2011,36:9439-9445), but this type of poor catalyst stability, its catalytic activity extends along with running time and reduces gradually.Compared with above-mentioned chemical catalyst, with living things catalysis, needed for the biological-cathode of core, applied voltage is low, can realize reducing costs continued biological and produce hydrogen (document EnvironSciTechnol, 2008,42 (2): 629-634; Bioelectrochemistry, 2010,78:39-43).But also exist because poorly conductive, microorganism catalysis performance are low etc. not enough and cause the product hydrogen level of biological-cathode lower.Therefore, above-mentioned precious metals pt negative electrode and base metal negative electrode exist that catalytic stability can differ from and biological-cathode exists the low problem of hydrogen generation efficiency, therefore it is significant to attempt exploitation MEC modification biological negative electrode.
In recent years, carbon nano-tube and mixing nano composite material thereof obtain larger concern owing to having unique structure, electronics and mechanical performance etc.The crystalline mineral of tourmaline to be a kind of boracic be feature, it can have an impact to the activity of water and structure by self there is the far infrared of electric field and transmitting, thus strengthens biological metabolism.Polyaniline obtains a wide range of applications with the characteristic electron of its uniqueness, outstanding environmental stability and the controlled conductivity etc. in protonated and charge transfer process.The present invention utilizes MWNT/ tourmaline/PANI modification biological negative electrode as the cathod catalyst of MEC, and the modification of MWNT, tourmaline and PANI can be utilized to increase electrode specific surface area and then be beneficial to microorganism colonization.Utilize tourmaline to improve microbial activity to the spread effect of microbe, play biocatalytic Activity.And utilize the high conduction performance of carbon nano-tube and polyaniline and Strong oxdiative reducing property etc. synchronously realize chemical catalysis function and accelerate electron transmission etc.In addition, MWNT/ tourmaline/PANI modification biological negative electrode comparatively higher, the price of Pt cathodic stability reduces several times.Therefore, MWNT/ tourmaline/PANI modification biological negative electrode synchronously processes waste water to MEC and production capacity is significant.
Summary of the invention
The present invention is directed to the deficiency that existing Pt metal catalyst substitute exists, a kind of MWNT/ tourmaline/PANI modification biological negative electrode application in MEC and preparation method thereof is provided.
For reaching above object, the present invention by the following technical solutions:
A kind of microorganism electrolysis cell modification biological cathode preparation method, with MWNT, tourmaline and PANI combination electrode for MEC modification biological negative electrode prepared by base material; First by MWNT and the mixing of tourmaline powder ball milling, add solvent, aniline and ammonium persulfate, stirring reaction under condition of ice bath, washing and drying obtains MWNT/ tourmaline/PANI compound; Compound and binding agent and acetone are mixed with and obtain MWNT/ tourmaline/PANI combination electrode, conventionally biofilm is tamed as MFC anode after natural air drying, then move to MEC negative electrode, finally construct MWNT/ tourmaline/PANI modification biological negative electrode.
Described preparation method, it specifically comprises the following steps:
(1) purifying of carbon nano-tube;
(2) by carbon nano-tube after purifying and tourmaline powder ball milling mixing in proportion;
(3) in mixture, surfactant, HCl and H is added in proportion
2o, stirs under ice bath;
(4) under ice bath stirring condition, in said mixture, add after decompression distillation, be dissolved in HCl aniline, ammonium persulfate in proportion, and continue ice bath stirring reaction a few hours;
(5) said mixture is washed, centrifugal, suction filtration obtains MWNT/ tourmaline/PANI composite material;
(6) binding agent and solvent is added in proportion to above-mentioned composite material even, and ultrasonic disperse;
(7) ultrasonic mixture is coated in conductive substrates equably, natural air drying obtains MWNT/ tourmaline/PANI combination electrode;
(8) above-mentioned combination electrode is carried out domestication biofilm as MFC anode;
(9) wait taming successfully, MEC negative electrode is moved to.
Described preparation method, the purification process of described carbon nano-tube is: under 50-80 DEG C of condition, ultrasonic 12-24 hour in sulfuric acid/nitric acid mixed liquor (3: 1).
Described preparation method, described tourmaline powder is 325-8000 object schorl powder or dravite powder; Described surfactant is DBSA or kayexalate.
Described preparation method, the mass ratio of described MWNT/ tourmaline/PANI is 24: 3-12: 8-72.
Described preparation method, the amount concentration of the HCl solution mass of described step (3) and (4) is 0.5-1mol/L, and condition of ice bath is 0-5 DEG C; In described step (4), the stirring reaction time is 12-24 hour.
Described preparation method, described binding agent is polytetrafluoroethylene or 5%Nafion solution; Described conductive substrates is carbon cloth, carbon felt or carbon paper.
Described preparation method, the natural air drying time in described step (7) is 24-48 hour.
Described preparation method, taming in described step (9) is successfully voltage stable output in MFC.
The application of microorganism electrolysis cell modification biological negative electrode in microorganism electrolysis cell prepared by described method.
Beneficial effect of the present invention is:
(1) preparation method of the present invention is simple, and easily operate, cost is low, considerably reduces the dependence to precious metals pt catalyst, has the application prospect of wide model in fields such as microorganism electrolysis cell process waste water;
(2) MWNT/ tourmaline/PANI modification biological negative electrode is as the cathod catalyst of MEC, the modification of MWNT, tourmaline and PANI not only can be utilized to increase electrode specific surface area and then be beneficial to microorganism colonization, and tourmaline can be utilized to improve microbial activity to the spread effect of microbe, play biocatalytic Activity.The high conduction performance of carbon nano-tube and polyaniline and Strong oxdiative reducing property etc. can also be utilized synchronously to realize chemical catalysis function and accelerate electron transmission etc.
(3) synchronously process waste water using MWNT/ tourmaline/PANI modification biological negative electrode as the cathod catalyst of MEC and produce hydrogen, can steady in a long-termly run, hydrogen yield is high, reaches 1.61m
3m
-3d
-1, COD clearance reaches 92.3%, for the commercial applications of MEC is had laid a good foundation.
Accompanying drawing explanation
Fig. 1 MWNT/ tourmaline/PANI modification biological cathode flow path figure;
Fig. 2 microbiological fuel cell structural representation;
Fig. 3 microorganism electrolysis cell structural representation;
The linear sweep voltammetry curve chart of the different negative electrode of Fig. 4
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
MFC (the microbiological fuel cell used in the present invention, Microbialfuelcell, MFC) structure as shown in Figure 2, comprises MFC anode 1, MFC negative electrode 2, MFC water inlet 3, MFC delivery port 4, MFC reference electrode mouth 5, MFC external resistance 6, MFC data acquisition unit 7 and MFC computer 8.MFC matrix solution is made up of following material: containing glucose 1.0g, ammonium chloride 0.31g, potassium chloride 0.13g, sodium hydrogen phosphate 11.88g, sodium dihydrogen phosphate 2.55g, magnesium sulfate 0.2g and micro-10mL in every premium on currency, COD is 1000mg/L, and pH value is 7.0.
MEC used in the present invention (microorganism electrolysis cell, Microbialelectrolysiscell, MEC) structure as shown in Figure 3, comprise MEC anode 9, MEC negative electrode 10, MEC water inlet 11, MEC delivery port 12, MEC reference electrode mouth 13, gas collection mouth 14, gas sampling mouth 15, gasometric determination pipe 16, water seal equilibration flask 17, D.C. regulated power supply 18, MEC external resistance 19, MEC data acquisition unit 20, MEC computer 21.MEC matrix solution is made up of following material: containing sodium acetate 1.28g, ammonium chloride 0.31g, potassium chloride 0.13g, sodium hydrogen phosphate 11.88g, sodium dihydrogen phosphate 2.55g, magnesium sulfate 0.20g and micro-10mL in every premium on currency, COD is 1000mg/L, and pH value is 7.0.
Embodiment 1
The first step: MWNT/ tourmaline/PANI modified electrode preparation
Unpurified for 2g carbon nano-tube (MWNT) is joined 100mL nitric acid/sulfuric acid mixture liquid (1: 3, v/v) in, stirring reaction 12 hours at 80 DEG C, the black liquor of suction filtration gained, deionized water is washed till neutrality, and after filtering, drying obtains purifying carbon nano-tube.
By carbon nano-tube after 0.2g purifying and the mixing of 0.05g8000 object schorl powder, ball milling 30min under 400r/min condition, the mass ratio obtaining carbon nano-tube and tourmaline is the mixture of 2: 1.1mL surfactant sodium dodecyl base benzene sulfonic acid, dense HCl and 70mLH of 30mL is added in mixture
2o, ultrasonic agitation 3 hours, goes in 0-5 DEG C of ice bath, obtains mixed liquor A; By the aniline 0.6mL preserved under 0-5 DEG C of condition of ice bath after decompression distillation, be dissolved in the HCl solution of 10mL1mol/L, add in above-mentioned mixed liquor A, obtain mixed liquid B; Under stirring, in mixed liquid B, the HCl solution (1.5g ammonium persulfate is dissolved in the HCl solution of 10mL1mol/L) of ammonium persulfate is added with the speed of 20/min, stirring reaction is continued 12 hours under 0-5 DEG C of condition of ice bath, make aniline oxidation polymerization, form ammonium persulfate at MWNT and tourmaline surface; Washing, centrifugal, dry, the mass ratio obtaining MWNT, tourmaline and PANI is the composite material of 24: 6: 72.
0.2g is got by after above-mentioned composite material ball milling, slowly add 0.5mL deionized water and 2.5mL isopropyl alcohol respectively again, the Nafion solution of 4mL5% is got with microsyringe, after being placed in ultrasonic washing instrument ultrasonic agitation 15min, be coated onto as far as possible equably on carbon cloth electrode by the mixture of Nafion and catalyst, the air drying 24 hours i.e. mass ratio of obtained MWNT, tourmaline, PANI is the catalysis electrode of 24: 6: 72.According to the preparation method of above-mentioned catalysis electrode, conventional Pt/C catalyst and binding agent mixing can be obtained Pt/C catalysis electrode.
Second step: tame biofilm in MWNT/ tourmaline/PANI modified electrode MFC, as shown in Figure 2, adds in MFC reactor biofilm by 60mL anaerobic sludge bacterial strain and 60mL matrix solution with 1: 1 ratio mixing by water inlet 3.With the MWNT/ of above-mentioned preparation tourmaline/PANI modified electrode for anode, conventional Pt/C is negative electrode.In system closed-loop path, access 1000 Ohmic resistances, start to record electricity generation process, when voltage is low, change MFC mesostroma solution and anaerobic sludge bacterial strain mixed liquor; Continue to change until resistance both end voltage is greater than 600mV, and keep stable, show to tame biofilm success (about cultivation, the domestication colonization method of anaerobic sludge bacterial strain, routine techniques is belonged at present in this area, can list of references: the influencing factor of microbiological fuel cell electrogenesis, process engineering journal, 2009,9:526-530).
3rd step: MWNT/ tourmaline/PANI modification biological negative electrode MEC performance test
As shown in Figure 3, by MEC water inlet 11,120mL matrix solution is added in MEC reactor.Take carbon cloth electrode as anode, be MEC negative electrode with the MWNT/ of above-mentioned preparation tourmaline/PANI modified biological negative electrode and Pt/C catalysis electrode respectively, at negative electrode cover plate by MEC and air insulated, make whole microorganism electrolysis cell solution be in anaerobic state.Utilize DC power supply at the additional 0.3-1.0V voltage in electrolytic cell anode and cathode two ends, electrolytic cell is run and produces hydrogen.In system closed-loop path, access 10 Ohmic resistances, start the voltage recording resistance two ends, change MEC mesostroma solution when voltage is low; Under lasting replacing realizes different applied voltage, MEC runs product hydrogen.The performance of different catalysis electrodes in MEC is as shown in table 1.
The performance of the different catalysis electrode of table 1 in MEC
4th step: MWNT/ tourmaline/PANI modified biological electrochemical cathode performance test
The mensuration of cathode performance uses linear sweep voltammetry (LSV), experiment employing three electrode test system, wherein above-mentioned MWNT/ tourmaline/PANI modified biological negative electrode is work electrode, reference electrode is Ag/AgCl electrode, pure platinum plate electrode (2 × 2cm) conduct is to pole, and electrolyte is 50mM phosphate buffer solution, before carrying out electro-chemical test, first logical high pure nitrogen 15min in electrolyte, to remove oxygen wherein.In order to avoid high potential is to the damage of electrode, potential scan scope is at-1.0 ~-0.3V, and sweep speed is 2mV/s, carries out under room temperature condition, and result as shown in Figure 4.As can be seen from Figure 4, the catalytic perfomance of MWNT/ tourmaline/PANI modified biological negative electrode prepared by the present embodiment is better than Pt/C catalysis electrode, and corresponding overpotential is low, and the performance of pure biological-cathode is poor comparatively speaking.
Embodiment 2
Differently from embodiment 1 be to get respectively in the first step carbon nano-tube, 0.1g8000 object schorl powder after 0.2g purifying, 0.6mL aniline and 1.5g ammonium persulfate obtain MWNT, tourmaline, PANI mass ratio be the catalysis electrode of 24: 12: 72.After taming biofilm in MFC, as MEC modification biological negative electrode, carry out MEC and produce hydrogen test, when applied voltage is 0.9V, obtain maximum current density 189Am
-3, COD clearance 91.7%, hydrogen yield 1.53m
3m
3d
-1.This modified biological negative electrode is carried out electrochemical property test, and adopt three electrode test systems, acquired results as shown in Figure 4.
Embodiment 3
Differently from embodiment 1 be to get respectively in the first step carbon nano-tube, 0.15g8000 object schorl powder after 0.6g purifying, 0.2mL aniline and 0.5g ammonium persulfate obtain MWNT, tourmaline, PANI mass ratio be the catalysis electrode of 24: 6: 8.After taming biofilm in MFC, as MEC modification biological negative electrode, carry out MEC and produce hydrogen test, when applied voltage is 0.9V, obtain maximum current density 178Am
-3, COD clearance 91.2%, hydrogen yield 1.34m
3m
3d
-1.This modified biological negative electrode is carried out electrochemical property test, and adopt three electrode test systems, acquired results as shown in Figure 4.
Embodiment 4
Differently from embodiment 1 be to get respectively in the first step carbon nano-tube, 0.3g8000 object schorl powder after 0.6g purifying, 0.2mL aniline and 0.5g ammonium persulfate obtain MWNT, tourmaline, PANI mass ratio be the catalysis electrode of 24: 12: 8.After taming biofilm in MFC, as MEC modification biological negative electrode, carry out MEC and produce hydrogen test, when applied voltage is 0.9V, obtain maximum current density 158Am
-3, COD clearance 90.1%, hydrogen yield 1.20m
3m
3d
-1.This modified biological negative electrode is carried out electrochemical property test, and adopt three electrode test systems, acquired results as shown in Figure 4.
Should be understood that, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection range that all should belong to claims of the present invention.
Claims (9)
1. a microorganism electrolysis cell modification biological cathode preparation method, is characterized in that: with carbon nano-tube, tourmaline and polyaniline composite electrode for microorganism electrolysis cell modification biological negative electrode prepared by base material; First by carbon nano-tube and the mixing of tourmaline powder ball milling, add solvent, aniline and ammonium persulfate, stirring reaction under condition of ice bath, washing and drying obtains carbon nano-tube/tourmaline/Polyaniline; Compound and binding agent and acetone are mixed with and obtain carbon nano-tube/tourmaline/polyaniline composite electrode, conventionally biofilm is tamed as anode of microbial fuel cell after natural air drying, then move to microorganism electrolysis cell negative electrode, finally construct carbon nano-tube/tourmaline/polyaniline-modified biological-cathode.
2. preparation method as claimed in claim 1, is characterized in that: it specifically comprises the following steps:
(1) purifying of carbon nano-tube;
(2) by carbon nano-tube after purifying and tourmaline powder ball milling mixing in proportion;
(3) in mixture, add surfactant, hydrochloric acid and water in proportion, stir under ice bath;
(4) under ice bath stirring condition, in said mixture, add after decompression distillation, be dissolved in hydrochloric acid aniline, ammonium persulfate in proportion, and continue ice bath stirring reaction a few hours;
(5) said mixture is washed, centrifugal, suction filtration obtains carbon nano-tube/tourmaline/polyaniline composite material;
(6) binding agent and solvent is added in proportion to above-mentioned composite material even, and ultrasonic disperse;
(7) mixture after ultrasonic disperse is coated in conductive substrates equably, natural air drying obtains carbon nano-tube/tourmaline/polyaniline composite electrode;
(8) above-mentioned combination electrode is placed in anode of microbial fuel cell and carries out domestication biofilm;
(9) after voltage stable output in microbiological fuel cell, microorganism electrolysis cell negative electrode is moved to.
3. preparation method as claimed in claim 2, is characterized in that: the purification process of described carbon nano-tube is: under 50-80 DEG C of condition, and ultrasonic 12-24 hour in the mixed liquor of sulfuric acid and nitric acid, wherein the volume ratio of sulfuric acid and nitric acid is 3: 1.
4. preparation method as claimed in claim 2, is characterized in that: described tourmaline powder is 325-8000 object schorl powder or dravite powder; Described surfactant is DBSA or kayexalate.
5. preparation method as claimed in claim 2, it is characterized in that: in described combination electrode, the mass ratio of carbon nano-tube, tourmaline, polyaniline is 24: (3-12): (8-72).
6. preparation method as claimed in claim 2, is characterized in that: the hydrochloric acid solution substance withdrawl syndrome of described step (3) and (4) is 0.5-1mol/L, and condition of ice bath is 0-5 DEG C; In described step (4), the stirring reaction time is 12-24 hour.
7. preparation method as claimed in claim 2, is characterized in that: described binding agent is polytetrafluoroethylene or 5%Nafion solution; Described conductive substrates is carbon cloth, carbon felt or carbon paper.
8. preparation method as claimed in claim 2, is characterized in that: the natural air drying time in described step (7) is 24-48 hour.
9. the application of microorganism electrolysis cell modification biological negative electrode in microorganism electrolysis cell prepared by the method as described in as arbitrary in claim 1-8.
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| CN103715433A (en) * | 2013-12-12 | 2014-04-09 | 大连理工大学 | Preparation method and application of tourmaline-polyaniline combined electrode |
| CN106946362B (en) * | 2017-04-11 | 2018-04-20 | 哈尔滨工业大学 | The preparation method of magnetic mesoporous carbon material modified anode, the magnetic microbe electro-chemical systems of pulse electromagnetic field auxiliary |
| CN109065896B (en) * | 2018-08-15 | 2022-01-28 | 山东建筑大学 | Preparation method of mesoporous silica/polypyrrole nano material modified microbial fuel cell anode |
| CN110534760B (en) * | 2019-08-30 | 2022-01-07 | 哈尔滨工业大学 | Tourmaline/manganese dioxide composite cathode for deposition type microbial fuel cell and preparation method thereof |
| CN113764682B (en) * | 2021-09-11 | 2023-04-25 | 东莞理工学院 | SMFC manganous oxide/tourmaline composite cathode and preparation method thereof |
| CN115029292B (en) * | 2022-07-12 | 2023-08-25 | 重庆大学 | Electrolytic high-efficiency hydrogen-producing biological cathode and domestication method thereof |
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