CN106024422B - A method of preparing capacitive electrode material using acclimated activated sludge - Google Patents
A method of preparing capacitive electrode material using acclimated activated sludge Download PDFInfo
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- 239000010802 sludge Substances 0.000 title claims abstract description 113
- 239000007772 electrode material Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 41
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 38
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 3
- 239000012298 atmosphere Substances 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 24
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 10
- 239000008363 phosphate buffer Substances 0.000 claims description 10
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 8
- 239000011707 mineral Substances 0.000 claims description 8
- 235000013343 vitamin Nutrition 0.000 claims description 8
- 229940088594 vitamin Drugs 0.000 claims description 8
- 229930003231 vitamin Natural products 0.000 claims description 8
- 239000011782 vitamin Substances 0.000 claims description 8
- 150000003722 vitamin derivatives Chemical class 0.000 claims description 8
- 241000894006 Bacteria Species 0.000 claims description 6
- 238000004939 coking Methods 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 6
- 230000001651 autotrophic effect Effects 0.000 claims description 4
- 241000108664 Nitrobacteria Species 0.000 claims description 3
- 108010027388 phenol 2-monooxygenase Proteins 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 238000004821 distillation Methods 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 244000005700 microbiome Species 0.000 description 6
- 235000010755 mineral Nutrition 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 241000233866 Fungi Species 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical class [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical class [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001546 nitrifying effect Effects 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 229930195143 oxyphenol Natural products 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 150000003233 pyrroles Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/02—Biological treatment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/20—Sludge processing
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Treatment Of Sludge (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Abstract
The invention discloses a kind of methods preparing capacitive electrode material using acclimated activated sludge, include the following steps：(1) nitrification domestication is carried out to activated sludge or phenol is tamed, the activated sludge after being tamed；(2) sludge that step (1) obtains is dried, is ground up, sieved, under atmosphere of inert gases, it is calcined 1.5~4 hours at 700~1000 DEG C, it is acid treated to be washed to neutrality with distillation, it is sieved after dry to obtain the porous sludge carbon material powder of auto-dope, i.e. capacitive electrode material at 55~105 DEG C.The method of the present invention improves the content of nitrogen in sludge carbon material, has better capacitive property.
Description
Technical field
The invention belongs to capacitative materials technical fields, and in particular to a kind of to prepare capacitive character electricity using acclimated activated sludge
The method of pole material.
Background technology
With being on the rise for the energy and problem of environmental pollution, develop new energy or improve energy storage and transform mode by
Gradually cause the interest of researcher.With high power density, the ultracapacitor of long service life and high security is a kind of
Solve the ideal chose of energy conversion and storage problem.Based on charge storage mechanism, ultracapacitor can be divided into electric double layer electricity
Container and pseudocapacitors based on redox reaction.Electrode material for electric double layer capacitor is mainly based on carbon material.Each
In kind pseudocapacitors material, element doping, high molecular polymer, transition metal are high performance ultracapacitor active materials,
Therefore capacitive property can be improved by adding active material into carbon material.
On the other hand, for activated sludge process because it is to water quality and quantity stabilization, energy consumption is few, purifies sewage effect in sewage disposal
It is widely used well, but it will produce a large amount of activated sludge in the process of running.These activated sludge have accumulated a large amount of difficulties
Degradation of organic substances, microorganism, heavy metal and other toxic compounds.If handling using the improper risk that will bring secondary pollution,
Therefore a great problem of activated sludge disposed with worked using sewage plant is become.Activated sludge is mainly by biomass, organic dirt
It contaminates the ingredients such as object and inorganic matter to constitute, rich in organic elements such as C, H, N, O, S.Inorganic matter and der Pilz constitute activated sludge
Skeleton, be the template of attached growth of microorganisms, it is larger that the flocculants such as Fe, Al ingredient and der Pilz so that activated sludge has
Specific surface area and loose pattern.By taking coking wastewater activated sludge as an example, rich in the elements such as oxygen, nitrogen, iron, sulphur, wherein pyridine,
The nitrogen-containing heterocycle compounds such as pyrroles are excellent electro-chemical activity ingredients.Thus, sludge, which has, is used as good capacitive character energy storage
Sludge treatment can be utilized and the preparation of energy storage material is combined by the potentiality of material feedstock.
Invention content
In order to overcome the disadvantages mentioned above and deficiency of the prior art, domestication activity is utilized the purpose of the present invention is to provide a kind of
The method that sludge prepares capacitive electrode material improves the content and specific surface area of nitrogen in sludge carbon material by domestication,
With better capacitive property.
The purpose of the present invention is achieved through the following technical solutions：
A method of capacitive electrode material being prepared using acclimated activated sludge, is included the following steps：
(1) nitrification domestication is carried out to activated sludge or phenol is tamed, the activated sludge after being tamed；
The nitrification domestication, specially：
Activated sludge is passed through air that flow is 1~3L/min into acting charitably in the nitrification domestication liquid of pH=7.0~8.0
Oxygen nitrification domestication culture, MLSS is in 3~6g/L for control, obtains the autotrophic type active pollution index using nitrobacteria as dominant bacteria；
The nitrification domestication liquid includes ammonia nitrogen；
The phenol domestication, specially：
Activated sludge is passed through air that flow is 1~3L/min into acting charitably in the phenol domestication liquid of pH=7.0~8.0
Oxy phenol domestication culture；MLSS is controlled in 3~6g/L；The heterotroph activated sludge that Phenol hydroxylase gene is dominant bacteria is obtained to wad a quilt with cotton
Body；The phenol domestication liquid includes phenol；
(2) sludge that step (1) obtains is dried, is ground up, sieved, under atmosphere of inert gases, in 700~1000
It is calcined 1.5~4 hours at DEG C, it is acid treated to be washed to neutrality with distillation, it is sieved after dry to obtain at 55~105 DEG C and mix certainly
Miscellaneous porous sludge carbon material powder, i.e. capacitive electrode material.
The nitrification domestication liquid includes phosphate buffer, mineral solution, vitamin solution, inorganic carbon source and ammonia nitrogen；Institute
It includes phosphate buffer, mineral solution, vitamin solution, nitrogen source and phenol to state phenol domestication liquid.
A concentration of 200~500mg/L of ammonia nitrogen in the nitrification domestication liquid.
A concentration of 500~1000mg/L of phenol in the phenol domestication liquid.
The aerobic nitrification domestication culture is by the way of gradient concentration culture；The aerobic phenol domestication culture is using ladder
Spend the mode of concentration culture.
The aerobic nitrification domestication culture is by the way of gradient concentration culture：Successively ammonia nitrogen concentration be 50,100,
150,200 it, 250,300,400, is tamed in the nitrification domestication liquid of 500mg/L.
The aerobic phenol domestication culture is by the way of gradient concentration culture, specially：Successively phenol concentration be 50,
100,200 it, 300,400,600,800, is tamed in the phenol domestication liquid of 1000mg/L.
The activated sludge is the activated sludge rich in oxygen element, nitrogen, ferro element.
The activated sludge is coking wastewater activated sludge.
The porous sludge carbon material powder of auto-dope includes that N doping porous carbon, Fe2O3 doping porous carbon and surface are rich in
Oxygen functional group porous carbon.
The principle of the present invention is：
The present invention is by taming activated sludge, during taming culture, the type of the microorganism in sludge
It is developed to the specific function type of selectivity, adapts to the micro organism quantity of specific environment, the micro- of specific nutrition substance cannot be utilized
It is biological then gradually dead, superseded.Microorganism in final activated sludge can form a large amount of and relatively stablize single dominant group.It is logical
Specific domestication culture is crossed, the nitrogen element content in sludge is further enriched with and is improved, and carbon-nitrogen ratio tends towards stability, in addition living
Property sludge in abundant carbon, oxygen, ferro element so that the carbon material prepared by acclimated activated sludge should have stronger conductive energy
Power, electro-chemical activity and the controllability for stablizing preparation.
Compared with prior art, the present invention has the following advantages and beneficial effect：
(1) present invention improves nitrogen member in sludge carbon material by carrying out nitrification domestication or phenol domestication to activated sludge
The content of element has better capacitive property.
(2) method that capacitive electrode material is prepared based on activated sludge of the invention, simple process and low cost, raw material
It derives from a wealth of sources.
(3) capacitive character sludge carbon material powder prepared by the present invention has pattern loose porous and specific surface area height, ratio
The good characteristic of heavy and light, cyclical stability.
(4) element that capacitative materials prepared by the present invention are adulterated derives from activated sludge.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) figure of capacitive character sludge carbon material powder prepared by embodiment 1.
Fig. 2 is that capacitive character sludge carbon material powder x-ray photoelectron prepared by embodiment 1 can (XPS) spectrogram.
Fig. 3 is the nitrogen adsorption desorption test chart that embodiment 1 prepares capacitive character sludge carbon material powder.
Fig. 4 is the graph of pore diameter distribution of capacitive character sludge carbon material powder prepared by embodiment 1.
Fig. 5 is capacitive character sludge carbon material powder CV scanning curve figures prepared by embodiment 1.
Fig. 6 is capacitive character sludge carbon material powder GCD curve graphs prepared by embodiment 1.
Fig. 7 is capacitive character sludge carbon material powder cyclical stability test chart prepared by embodiment 1
Fig. 8 is capacitive character sludge carbon material powder CV scanning curve figures prepared by embodiment 2.
Fig. 9 is capacitive character sludge carbon material powder GCD curve graphs prepared by embodiment 2.
Figure 10 is capacitive character sludge carbon material powder CV scanning curve figures prepared by comparative example.
Figure 11 is capacitive character sludge carbon material powder GCD curve graphs prepared by comparative example.
Figure 12 is embodiment 1, embodiment 2, the capacitive character sludge carbon material powder GCD curve comparison figures of comparative example preparation.
Figure 13 (a)~(c) is respectively the scanning electron microscope (SEM) of sludge in embodiment 1, embodiment 2, comparative example
Figure.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, embodiments of the present invention are not limited thereto.
Embodiment 1
10 grams are taken (to be somebody's turn to do by the nitrification domestication autotrophic type activated sludge of splendid steel coking wastewater project aerobic tank sludge acclimatization culture
The mass percent of carbon is 23.04% in sludge, and the mass percent of nitrogen is 6.39%, the quality percentage of oxygen element
Than 28.56%) to be dried 6 hours at 60 DEG C, grinding, sieving with 100 mesh sieve after taking-up, then under nitrogen atmosphere, with per minute
10 degrees Celsius of heating rate is calcined 2 hours at 800 DEG C, during the carbon dust of gained is washed to after HCl treatment with distillation
Property, it crosses 300 mesh after dry at 60 DEG C and sieves to obtain the porous sludge carbon material powder of auto-dope, i.e. capacitive electrode material.
The nitrification domestication, specially：
Activated sludge is passed through the air that flow is 1~3L/min and carries out aerobic domestication culture, control in nitrifying domestication liquid
MLSS obtains the autotrophic type active pollution index using nitrobacteria as dominant bacteria in 3~6g/L.
The nitrification domestication liquid (is equivalent to comprising 0.1mol/L pH=8.0 phosphate buffers, 1.91g/L ammonium chlorides
500mg/L ammonia nitrogens), 3g/L sodium bicarbonates, 10mL mineral solutions and 10mL vitamin solutions is added in every liter of phosphate buffer
The formula of 0.1mol/L pH=8.0 phosphate buffers is as shown in table 1.
Table 1
Mineral solution formula is as shown in table 2.
Table 2
Vitamin solution formula is as shown in table 3 below.
Table 3
Fig. 1 is the Scanning Electron microscope imaging figure of capacitive character sludge carbon material powder prepared by the present embodiment.It can see
Go out, which has loose porous structure.
Fig. 2 is the full spectrogram of x-ray photoelectron spectroscopy of capacitive character sludge carbon material powder prepared by the present embodiment.It can see
Go out, in addition to carbon, rich in elements such as nitrogen, oxygen, sulphur.After measured, the doping of nitrogen content 2.6%, nitrogen helps
In improving material electrochemical activity, material capacitive property is improved.
Fig. 3 is the nitrogen adsorption desorption test chart of capacitive character sludge carbon material powder prepared by the present embodiment.It after measured, can be with
Learn that its specific surface area is 609.4m2/g。
Fig. 4 is the graph of pore diameter distribution of capacitive character sludge carbon material powder prepared by the present embodiment.After measured, main bore dia
Concentrate on 12.13nm or so.
Using the capacitive character porous carbon materials prepared by the present embodiment as electrode material for super capacitor, using three-electrode system
Electrochemical workstation detect its capacitive property.Wherein working electrode is the glass carbon electricity for loading the carbon dust prepared by the present embodiment
Pole, reference electrode are saturated calomel electrode (SCE), are platinum filament to electrode, and electrolyte is 1mol/L H2SO4Solution.CV scanning knots
Fruit is as shown in figure 5, be scanning speed of the capacitive character sludge carbon material prepared by the present embodiment in 10,20,50,100,200mV/s
CV curve graphs under rate.GCD Dependence Results are as shown in fig. 6, the capacitive character sludge carbon material respectively prepared by the present embodiment exists
1,2,3,5,10, the charge and discharge charging and discharging curve under 15A/g difference current densities, under the current density of 1A/g, the ratio of material
Capacitance is 889F/g.Cyclical stability is as shown in fig. 7, close in electric current for the capacitive character sludge carbon material prepared by the present embodiment
Degree is the curve of the circle of charge and discharge 10000 cycle gained under the conditions of 20A/g, and after cycle 10000 is enclosed, capacitance is not substantially reduced.
Embodiment 2
10 grams are taken (to be somebody's turn to do by the phenol domestication heterotroph activated sludge of splendid steel coking wastewater project aerobic tank sludge acclimatization culture
The mass percent of carbon is 24.06% in sludge, and the mass percent of nitrogen is 4.72%, the quality percentage of oxygen element
Than 29.16%) to be dried 6 hours at 60 DEG C, grinding, sieving with 100 mesh sieve after taking-up, then under nitrogen atmosphere, with per minute 5
Degree Celsius heating rate, calcined 2 hours at 800 DEG C, neutrality be washed to distillation after HCl treatment, it is dry at 60 DEG C
300 mesh are crossed afterwards to sieve to obtain the porous sludge carbon material powder of auto-dope, i.e. capacitive electrode material.
The phenol of the present embodiment is tamed, specially：
Activated sludge is passed through the air that flow is 1~3L/min and carries out aerobic domestication culture in phenol domestication liquid；Control
MLSS is in 3~6g/L；Obtain the heterotroph active pollution index that Phenol hydroxylase gene is dominant bacteria.
The phenol domestication liquid includes 0.1mol/L pH=7.0 phosphate buffers, 800mg/L phenol, 0.2g/L chlorinations
10mL mineral solutions and 10mL vitamin solutions are added in every liter of phosphate buffer for ammonium.Mineral solution and vitamin solution
Formula and embodiment 1 it is same.
The formula of 0.1mol/L pH=7.0 phosphate buffers is as shown in table 4 below.
Table 4
Subsequent experimental condition is same as Example 1, and CV scanning results are as shown in figure 8, for the capacitance prepared by the present embodiment
Sweep speed under CV curve of the property sludge carbon material in 10mV/s；GCD curves are as shown in figure 9, for the capacitive character prepared by the present embodiment
Sludge carbon material is 1A/g constant current charge-discharge curve graphs in current density, and specific capacitance value is 578F/g.
Comparative example
This comparative example is used prepares sludge carbon material without the activated sludge of domestication, specific as follows：
Taking 10 grams of splendid steel coking wastewater project aerobic tank activated sludge, (mass percent of carbon is in the sludge
21.62%, the mass percent of the nitrogen is 4.01%, and the mass percent of oxygen element is 32.13%) dry at 60 DEG C
It 6 hours, grinds, sieves with 100 mesh sieve after taking-up, then under nitrogen atmosphere, with 5 degrees Celsius of heating rate per minute, in 800 DEG C
Lower calcining 2 hours, neutrality is washed to after HCl treatment with distillation, it is dry at 60 DEG C after 300 mesh of mistake sieve to obtain auto-dope it is more
Hole sludge carbon material powder, i.e. capacitive electrode material.
Subsequent experimental condition is same as Example 1, CV scanning results such as Figure 10, the capacitive character sludge prepared by the present embodiment
The GCD Dependence Results such as Figure 11 of carbon material under conditions of current density is 1A/g, specific capacitance value are 146F/g.Embodiment 1, reality
Apply example 2, capacitive character sludge carbon material powder GCD curve comparison figures such as Figure 12 prepared by comparative example.
Figure 13 (a)~(c) is the scanning electron microscope diagram of sludge in embodiment 1, embodiment 2, this comparative example, can be seen
It is sparse to microorganism growth fraction in non-acclimation sludge 13 (a), denser, structure is grown in acclimation sludge 13 (b), 13 (c)
It is compact.
Table 1 is sludge and sludge carbon organic element content in embodiment 1, embodiment 2 and this comparative example, it can be seen that through from
The sludge and non-acclimation sludge of the type of supporting or heterotroph domestication, and the sludge carbon material accordingly prepared are compared, and have higher nitrogen member
Cellulose content and carbon-nitrogen ratio, nitrogen doped with the raising conducive to capacitive property.
Table 5
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by the embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of method preparing capacitive electrode material using acclimated activated sludge, which is characterized in that include the following steps：
(1) nitrification domestication is carried out to activated sludge or phenol is tamed, the activated sludge after being tamed；
The nitrification domestication, specially：
Activated sludge is passed through the air that flow is 1~3L/min and carries out aerobic nitre in the nitrification domestication liquid of pH=7.0~8.0
Change domestication culture, MLSS is in 3~6g/L for control, obtains the autotrophic type active pollution index using nitrobacteria as dominant bacteria；It is described
It includes ammonia nitrogen to nitrify domestication liquid；
The phenol domestication, specially：
Activated sludge is passed through the air that flow is 1~3L/min and carries out aerobic benzene in the phenol domestication liquid of pH=7.0~8.0
Phenol domestication culture, MLSS is in 3~6g/L for control；Obtain the heterotroph active pollution index that Phenol hydroxylase gene is dominant bacteria；Institute
It includes phenol to state phenol domestication liquid；
(2) sludge that step (1) obtains is dried, is ground up, sieved, under atmosphere of inert gases, at 700~1000 DEG C
Calcining 1.5~4 hours, it is acid treated to be washed to neutrality with distilling, it is sieved after dry to obtain auto-dope at 55~105 DEG C more
Hole sludge carbon material powder, i.e. capacitive electrode material.
2. the method according to claim 1 for preparing capacitive electrode material using acclimated activated sludge, which is characterized in that
The nitrification domestication liquid includes phosphate buffer, mineral solution, vitamin solution, inorganic carbon source and ammonia nitrogen；The phenol is tamed and dociled
It includes phosphate buffer, mineral solution, vitamin solution, nitrogen source and phenol to change liquid.
3. the method according to claim 1 for preparing capacitive electrode material using acclimated activated sludge, which is characterized in that
A concentration of 200~500mg/L of ammonia nitrogen in the nitrification domestication liquid.
4. the method according to claim 1 for preparing capacitive electrode material using acclimated activated sludge, which is characterized in that
A concentration of 500~1000mg/L of phenol in the phenol domestication liquid.
5. the method according to claim 1 for preparing capacitive electrode material using acclimated activated sludge, which is characterized in that
The aerobic nitrification domestication culture is by the way of gradient concentration culture；The aerobic phenol domestication culture is trained using gradient concentration
Foster mode.
6. the method according to claim 5 for preparing capacitive electrode material using acclimated activated sludge, which is characterized in that
The aerobic nitrification domestication culture is by the way of gradient concentration culture：Successively ammonia nitrogen concentration be 50,100,150,200,
250,300 it, 400, is tamed in the nitrification domestication liquid of 500mg/L.
7. the method according to claim 5 for preparing capacitive electrode material using acclimated activated sludge, which is characterized in that
The aerobic phenol domestication culture is by the way of gradient concentration culture, specially：Successively phenol concentration be 50,100,200,
300,400 it, 600,800, is tamed in the phenol domestication liquid of 1000mg/L.
8. the method according to claim 1 for preparing capacitive electrode material using acclimated activated sludge, which is characterized in that
The activated sludge is the activated sludge rich in oxygen element, nitrogen, ferro element.
9. the method according to claim 1 for preparing capacitive electrode material using acclimated activated sludge, which is characterized in that
The activated sludge is coking wastewater activated sludge.
10. the method according to claim 1 for preparing capacitive electrode material using acclimated activated sludge, feature exist
In the porous sludge carbon material powder of auto-dope includes that N doping porous carbon, Fe2O3 doping porous carbon and surface are rich in oxygen official
Porous carbon can be rolled into a ball.
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