CN104538644A - Preparation method and application of sludge carbon plate electrode - Google Patents
Preparation method and application of sludge carbon plate electrode Download PDFInfo
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- CN104538644A CN104538644A CN201410796115.6A CN201410796115A CN104538644A CN 104538644 A CN104538644 A CN 104538644A CN 201410796115 A CN201410796115 A CN 201410796115A CN 104538644 A CN104538644 A CN 104538644A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
- H01M4/8875—Methods for shaping the electrode into free-standing bodies, like sheets, films or grids, e.g. moulding, hot-pressing, casting without support, extrusion without support
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/16—Biochemical fuel cells, i.e. cells in which microorganisms function as catalysts
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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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention discloses a preparation method and application of a sludge carbon plate electrode. The preparation method comprises the steps of uniformly mixing smashed wood flour and dried sludge powder at certain weight ratio, pouring the mixture into a mold, adding with a certain amount of moisture, grinding and shaping; and taking out, drying, and carrying out high-temperature gradient anaerobic carbonization to obtain a sludge carbon plate electrode material. According to the prepared electrode material, waste sludge in a sewage plant and discarded biomass wood flour are used as raw materials, the cost is low, the preparation method is simple and rapid, and the method can provide a new way for the sludge resourced technology. The sludge carbon plate electrode can be applied to a microbial fuel cell, and compared with the traditional graphite electrode, the sludge carbon plate electrode has the power density of the battery, which is improved nearly twice.
Description
Technical field
The preparation method of a kind of mud carbon plate of the present invention electrode and application.
Background technology
Along with the raising of China's urban wastewater treatment rate, the process of a large amount of excess sludge has become the new problem of environment urgently to be resolved hurrily with disposal, and city sewage sludge reclamation process should assess sustainability and the practicality of recycling sludge schemes than 4 aspects from environmental sanitary safety, resource reclaim, resource input output ratio and revenue impact.Municipal sludge is as the large solid waste of China one, and its generation is large, is biomass resource to be utilized.For a long time, owing to being dealt carefully with, cause serious secondary pollution and wasting of resources amplification quantity carbon side by side, make China face the dual-pressure of prevention and cure of pollution and carbon emission reduction.As prepared biological carbon materials, the multi-efficiencies such as waste pollution control and recycling can be realized.And microbiological fuel cell (MFC, microbial fuel cell) be the desirable electrogenesis device utilizing microbe the chemical energy in matrix to be converted into electric energy, there is resource and waste treatment double effects, be of great significance at energy starved tool today.
Summary of the invention
In order to solve above-mentioned Problems existing, the angle that the present invention fully utilizes from waste resource, develop with mud and abandoned biomass for electrode material prepared by raw material, and for microbiological fuel cell technology, this technology is that recycling sludge provides a kind of effective way.
The object of the present invention is to provide a kind of preparation method and application thereof of mud carbon plate electrode.
The technical solution used in the present invention is:
A preparation method for mud carbon plate electrode, comprises the following steps:
1) wood chip is pulverized, sieve;
2) mud is dried, pulverize and sieve, obtain sludge dry powder;
3) wood chip and sludge dry powder are pressed (0 ~ 30): the weight ratio of 100 mixes, and adds the water that weight is wood chip and sludge dry powder total weight 20% ~ 65%, mixing, grinding forming;
4) mixture of upper step grinding forming is taken out oven dry, carbonize under anaerobic condition, obtain electrode material, be i.e. mud carbon plate electrode.
Further, above-mentioned steps 1) described in wood chip sieve into cross 20 ~ 60 mesh sieves.
Further, above-mentioned steps 2) described in mud sieve into cross 60 ~ 120 mesh sieves.
Further, above-mentioned steps 2) described in oven dry for dry to moisture to 5% at 50 ~ 80 DEG C.
Further, above-mentioned steps 4) described in oven dry for dry to moisture to 5% at 50 ~ 80 DEG C.
Further, above-mentioned steps 4) described in charing be the charing of high-temperature gradient anaerobism, be specially respectively at 300 DEG C ~ 400 DEG C, 450 DEG C ~ 500 DEG C, 600 DEG C ~ 700 DEG C, in 800 DEG C ~ 900 DEG C these 4 temperature gradients, anaerobism carbonizes 30 ~ 120min successively.
A kind of microbiological fuel cell, this microbiological fuel cell Anodic electrode material is mud carbon plate electrode material prepared by method described above.
The invention has the beneficial effects as follows:
Electrode material prepared by the present invention is with the waste sludge of Sewage Plant and discarded biomass wood chip for raw material, and with low cost and method simple and fast, for sludge resource technology provides new outlet.
Mud carbon plate electrode prepared by the present invention can be applied in microbiological fuel cell, and compared with conventional graphite electrodes, battery maximum power density can improve about 2 times.
The present invention adopts the method for mud and wood chip mixing, and the wood chip of different proportion is mixed with mud, compressing in a mold, is then carried out the charing of anaerobic high temperature gradient, the electrode be finally translated into.Mud carbon plate electrode prepared by the present invention, utilizes " mud " to add the pattern of " abandoned biomass ", in conjunction with the application of microbiological fuel cell, for sludge resource technology and bioenergy provide new application model.
Accompanying drawing explanation
Fig. 1 is the flow chart that embodiment 1 prepares mud carbon plate electrode process;
Fig. 2 is ESEM (SEM) figure of ordinary graphite plate electrode and mud carbon plate electrode of the present invention; A is graphite cake, and B is mud carbon plate;
Under the different anode material of Fig. 3, microbiological fuel cell power density is with the change of current density.
Embodiment
A preparation method for mud carbon plate electrode, comprises the following steps:
1) wood chip is pulverized, sieve;
2) mud is dried, pulverize and sieve, obtain sludge dry powder;
3) wood chip and sludge dry powder are pressed (0 ~ 30): the weight ratio of 100 mixes, and adds the water that weight is wood chip and sludge dry powder total weight 20% ~ 65%, mixing, grinding forming;
5) mixture of upper step grinding forming is taken out oven dry, carbonize under anaerobic condition, obtain electrode material, be i.e. mud carbon plate electrode.
Preferably, above-mentioned steps 1) described in wood chip sieve into cross 20 ~ 60 mesh sieves.
Preferably, above-mentioned steps 2) described in mud sieve into cross 60 ~ 120 mesh sieves.
Preferably, above-mentioned steps 2) described in oven dry for dry to moisture to 5% at 50 ~ 80 DEG C.
Preferably, above-mentioned steps 3) described in wood chip and the sludge dry powder weight ratio of pressing 10:100 mix.
Preferably, above-mentioned steps 3) described in the weight of water be 40% of wood chip and sludge dry powder total weight.
Preferably, above-mentioned steps 4) described in oven dry for dry to moisture to 5% at 50 ~ 80 DEG C.
Further, above-mentioned steps 4) described in charing be the charing of high-temperature gradient anaerobism, be specially respectively at 300 DEG C ~ 400 DEG C, 450 DEG C ~ 500 DEG C, 600 DEG C ~ 700 DEG C, in 800 DEG C ~ 900 DEG C these 4 temperature gradients, anaerobism carbonizes 30 ~ 120min successively.The preferred carbonization time of 4 temperature gradients is 80min.
A kind of microbiological fuel cell, this microbiological fuel cell Anodic electrode material is mud carbon plate electrode material prepared by method described above.
Below in conjunction with specific embodiment, the present invention is further illustrated, but be not limited thereto.
embodiment 1
A preparation method for mud carbon plate electrode, comprises the following steps:
1) wood chip is pulverized, obtain with 40 mesh sieve screenings the wood chip bits meeting size requirements;
2) mud getting Sewage Plant discarded is dried and is polished into powder at 50 ~ 80 DEG C, obtains sludge dry powder with 100 mesh sieve screenings;
3) mixed in the ratio of 0:100,5:100,10:100,20:100 respectively with sludge dry powder by wood chip, mixing is poured in mould, adds the moisture that weight is the two total weight 50%, mixing, grinding forming;
4) mixture of above-mentioned grinding forming is taken out, dry to moisture less than 5% at 50 ~ 80 DEG C, then put into cremator, carry out the charing of high-temperature gradient anaerobism, be specially respectively at 400 DEG C, 500 DEG C, 700 DEG C, in 900 DEG C of these 4 temperature gradients, anaerobism carbonizes 30min successively, obtain electrode material, i.e. mud carbon plate electrode, then it is long × wide × thick to be cut into required specification 2.0 cm × 2.0 cm × 0.5 cm(, the state measurement with after mud carbonization).
In the present embodiment preparation process, Making programme is shown in Fig. 1, and before experiment, mud wood chip mixture color is ashen, and after charing, mud carbon color becomes black.
The SEM of mud carbon plate electrode (in its raw material, wood chip and sludge dry powder weight ratio are 10:100) prepared by the present embodiment schemes as shown in Figure 2 B, and the SEM of existing ordinary graphite plate schemes as shown in Figure 2 A.
embodiment 2
A preparation method for mud carbon plate electrode, comprises the following steps:
1) wood chip is pulverized, obtain with 20 mesh sieve screenings the wood chip bits meeting size requirements;
2) mud getting Sewage Plant discarded is dried and is polished into powder at 50 ~ 80 DEG C, obtains sludge dry powder with 80 mesh sieve screenings;
3) mixed in the ratio of 2:100,4:100,6:100,8:100 respectively with sludge dry powder by wood chip, mixing is poured in mould, adds the moisture that weight is the two total weight 65%, mixing, grinding forming;
4) mixture of above-mentioned grinding forming is taken out, dry at 50 ~ 80 DEG C to moisture less than 5%, put into cremator again, carry out the charing of high-temperature gradient anaerobism, be specially respectively at 400 DEG C, 500 DEG C, 700 DEG C, in 850 DEG C of these 4 temperature gradients, anaerobism carbonizes 50min successively, obtains electrode material, i.e. mud carbon plate electrode.
embodiment 3
1) wood chip is pulverized, obtain with 60 mesh sieve screenings the wood chip bits meeting size requirements;
2) mud getting Sewage Plant discarded is dried and is polished into powder at 50 ~ 80 DEG C, obtains sludge dry powder with 120 mesh sieve screenings;
3) mixed in the ratio of 5:100,10:100,15:100,30:100 respectively with sludge dry powder by wood chip, mixing is poured in mould, adds the moisture that weight is the two total weight 40%, mixing, grinding forming;
4) mixture of above-mentioned grinding forming is taken out, dry at 50 ~ 80 DEG C to moisture less than 5%, put into retort again, carry out the charing of high-temperature gradient anaerobism, be specially respectively at 300 DEG C, 500 DEG C, 700 DEG C, in 800 DEG C of these 4 temperature gradients, anaerobism carbonizes 90min successively, obtains electrode material, i.e. mud carbon plate electrode.
embodiment 4
1) wood chip is pulverized, obtain with 40 mesh sieve screenings the wood chip bits meeting size requirements;
2) mud getting Sewage Plant discarded is dried and is polished into powder at 70 DEG C, obtains sludge dry powder with 100 mesh sieve screenings;
3) mixed with the ratio of sludge dry powder in 10:100 by wood chip, mixing is poured in mould, adds the moisture that weight is the two total weight 40%, mixing, grinding forming;
4) mixture of above-mentioned grinding forming is taken out, dry at 80 DEG C to moisture less than 5%, put into cremator again, carry out the charing of high-temperature gradient anaerobism, be specially respectively at 350 DEG C, 500 DEG C, 650 DEG C, in 900 DEG C of these 4 temperature gradients, anaerobism carbonizes 80min successively, obtains electrode material, i.e. mud carbon plate electrode.
embodiment 5
1) wood chip is pulverized, obtain with 40 mesh sieve screenings the wood chip bits meeting size requirements;
2) mud getting Sewage Plant discarded is dried and is polished into powder at 80 DEG C, obtains sludge dry powder with 100 mesh sieve screenings;
3) mixed with the ratio of sludge dry powder in 10:100 by wood chip, mixing is poured in mould, adds the moisture that weight is the two total weight 20%, mixing, grinding forming;
4) mixture of above-mentioned grinding forming is taken out, dry at 80 DEG C to moisture less than 5%, put into cremator again, carry out the charing of high-temperature gradient anaerobism, be specially respectively at 300 DEG C, 450 DEG C, 600 DEG C, in 800 DEG C of these 4 temperature gradients, anaerobism carbonizes 120min successively, obtains electrode material, i.e. mud carbon plate electrode.
embodiment 6 microbiological fuel cell
the structure of microbiological fuel cell (MFC)
1) microbe single chamber air cathode fuel cell is built according to the conventional method: using polymethyl methacrylate as battery raw material (rectangle), MFC inside be one long be 4.0, the cylinder of diameter 3.0 cm, negative and positive the two poles of the earth length is organic square glass sealing of 6.0 cm.
2) cathode sheets is made according to the conventional method: negative electrode carbon cloth side uniform application 0.5 mg/cm
2pt catalyst (20% Pt/C), after natural air drying.
3) the mud carbon plate electrode material that prepared by Example 1 is cut into required specification as anode material.
4) treat that above preparation is ready, assembled battery anode, insert the ready anode material of step 3), by inside for the one side that negative electrode diaphragm will scribble catalyst layer, do not have the face of catalyst to expose in atmosphere, such cathode catalysis better effects if, with plug seal cell top end opening, and with titanium silk as wire connected battery the two poles of the earth, inner dischargeable capacity is 28 ml.
The MFC that the present embodiment builds except anode material is different with the MFC of routine, other all identical.
the operation of microbiological fuel cell (MFC)
MFC operation method conveniently, inoculates 5.0 ml anaerobic sludges (GuangZhou, China Lie De sewage treatment plant) and 23 ml sodium acetate (1000mgL by above-mentioned mounted MFC
-1) substrate solution, startup optimization.Sodium acetate substrate solution becomes to be grouped into: NaH
2pO
42H
2o (2.77 gL
-1), Na
2hPO
412H
2o (11.40 gL
-1), NH
4cl (0.31 gL
-1), KCl (0.13 gL
-1), vitamin solution (12.5 mLL
-1) and mineral solution (12.5 mLL
-1).
MFC is cultivated in the insulating box of 30 ± 1 DEG C, electrogenesis voltage adopts 16 channel signal collectors, be stored in computer every 2 minutes automatic data collections, after battery reaches the stabilization sub stage, change battery extrernal resistance 50 to 5000 Ω, under each external resistance, battery all runs a complete cycle, then obtain corresponding voltage, draw power density and polarization curve.
Fig. 3 be under different anode material microbiological fuel cell power density with the change of current density, in embodiment 1, weight ratio is that the performance curve of the mud carbon plate electrode prepared of the wood chip of 10:100 and mud as the microbiological fuel cell of anode is as the circle point curve in Fig. 3, square curve is under the same terms, the performance curve of the microbiological fuel cell adopting conventional anode material graphite cake to prepare.Therefrom can find out, compared with conventional flat electrodes (graphite cake), sludge organism carbon electrode material of the present invention makes the maximum current density value of microorganism electrode improve about 1.5 times, and battery maximum power density increases about 2 times.Visible sludge organism carbon electrode material of the present invention is better than the graphite cake commonly used, and brings better electricity generation performance to microbiological fuel cell.
For those skilled in the art's easy understand; the foregoing is only the preferred embodiment of patent of the present invention; not in order to limit the present invention, any amendment done within all the spirit and principles in the present invention, equivalent to replace and improvement etc., within the protection range all dropping on application claims.
Claims (7)
1. a preparation method for mud carbon plate electrode, is characterized in that: comprise the following steps:
1) wood chip is pulverized, sieve;
2) mud is dried, pulverize and sieve, obtain sludge dry powder;
3) wood chip and sludge dry powder are pressed (0 ~ 30): the weight ratio of 100 mixes, and adds the water that weight is wood chip and sludge dry powder total weight 20% ~ 65%, mixing, grinding forming;
4) mixture of upper step grinding forming is taken out oven dry, carbonize under anaerobic condition, obtain electrode material, be i.e. mud carbon plate electrode.
2. the preparation method of a kind of mud carbon plate electrode according to claim 1, is characterized in that: wood chip described in step 1) sieves as crossing 20 ~ 60 mesh sieves.
3. the preparation method of a kind of mud carbon plate electrode according to claim 1, is characterized in that: step 2) described in mud sieve into cross 60 ~ 120 mesh sieves.
4. the preparation method of a kind of mud carbon plate electrode according to claim 1, is characterized in that: step 2) described in oven dry for dry to moisture to 5% at 50 ~ 80 DEG C.
5. the preparation method of a kind of mud carbon plate electrode according to claim 1, is characterized in that: the oven dry described in step 4) for dry to moisture to 5% at 50 ~ 80 DEG C.
6. the preparation method of a kind of mud carbon plate electrode according to claim 1, it is characterized in that: charing described in step 4) is the charing of high-temperature gradient anaerobism, be specially respectively at 300 DEG C ~ 400 DEG C, 450 DEG C ~ 500 DEG C, 600 DEG C ~ 700 DEG C, in 800 DEG C ~ 900 DEG C these 4 temperature gradients, anaerobism carbonizes 30 ~ 120min successively.
7. a microbiological fuel cell, is characterized in that: this microbiological fuel cell Anodic electrode material is mud carbon plate electrode material prepared by the arbitrary described method of claim 1 ~ 6.
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Cited By (6)
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| CN105140528A (en) * | 2015-07-31 | 2015-12-09 | 华南理工大学 | Self-doped microbial fuel cell cathode material and preparation method thereof |
| CN106745676A (en) * | 2016-11-25 | 2017-05-31 | 浙江工商大学 | A kind of ecological many negative electrode urine processing devices and method |
| CN106920972A (en) * | 2017-04-11 | 2017-07-04 | 大连理工大学 | The preparation method and microbiological fuel cell of the novel composite anode of a kind of N doping charcoal based on sludge and porous volcanic rock |
| CN106920966A (en) * | 2017-04-12 | 2017-07-04 | 同济大学 | A kind of carbon-based lithium ion cell negative electrode material and its preparation using sludge as precursor |
| CN107240687A (en) * | 2017-06-12 | 2017-10-10 | 黎烈武 | Energy storage material and its methods and applications prepared by a kind of utilization activated sludge |
| CN107732258A (en) * | 2017-10-27 | 2018-02-23 | 江苏理工学院 | A kind of nano-sheet Pt/ charings scrap wood material and preparation method thereof |
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| CN105140528A (en) * | 2015-07-31 | 2015-12-09 | 华南理工大学 | Self-doped microbial fuel cell cathode material and preparation method thereof |
| CN106745676A (en) * | 2016-11-25 | 2017-05-31 | 浙江工商大学 | A kind of ecological many negative electrode urine processing devices and method |
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| CN106920972B (en) * | 2017-04-11 | 2019-04-16 | 大连理工大学 | The preparation method and microbiological fuel cell of the novel composite anode of a kind of N doping charcoal based on sludge and porous volcanic rock |
| CN106920966A (en) * | 2017-04-12 | 2017-07-04 | 同济大学 | A kind of carbon-based lithium ion cell negative electrode material and its preparation using sludge as precursor |
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| CN107240687A (en) * | 2017-06-12 | 2017-10-10 | 黎烈武 | Energy storage material and its methods and applications prepared by a kind of utilization activated sludge |
| WO2018227535A1 (en) * | 2017-06-12 | 2018-12-20 | 黎烈武 | Energy storage material prepared by using active sludge and method therefor and applications thereof |
| CN107240687B (en) * | 2017-06-12 | 2020-08-18 | 黎烈龙 | Energy storage material prepared from activated sludge and method and application thereof |
| CN107732258A (en) * | 2017-10-27 | 2018-02-23 | 江苏理工学院 | A kind of nano-sheet Pt/ charings scrap wood material and preparation method thereof |
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