CN114735806A - Method for removing azo dye by graphene/polyaniline modified electrode enhanced bioelectrochemistry - Google Patents

Method for removing azo dye by graphene/polyaniline modified electrode enhanced bioelectrochemistry Download PDF

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CN114735806A
CN114735806A CN202210401044.XA CN202210401044A CN114735806A CN 114735806 A CN114735806 A CN 114735806A CN 202210401044 A CN202210401044 A CN 202210401044A CN 114735806 A CN114735806 A CN 114735806A
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electrode
graphene
polyaniline
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cathode
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崔丹
陈艾宏
田梓扬
张启玉
江宏伦
林家兴
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Beijing University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00—Biological treatment of water, waste water, or sewage
    • C02F3/005—Combined electrochemical biological processes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2203/00—Apparatus and plants for the biological treatment of water, waste water or sewage
    • C02F2203/006—Apparatus and plants for the biological treatment of water, waste water or sewage details of construction, e.g. specially adapted seals, modules, connections
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/14—Maintenance of water treatment installations
    • 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

A method for removing azo dyes by graphene/polyaniline modified electrodes through enhanced bioelectrochemistry belongs to the field of sewage treatment. The graphene/polyaniline modified electrode adopts an electrochemical deposition method, graphene oxide is reduced to graphene in situ through cyclic voltammetry scanning, aniline is oxidized to polyaniline, and the polyaniline is modified on the surface of the carbon-based electrode in two steps, so that the electrochemical activity and biocompatibility of the carbon-based electrode are improved. And taking the electrode for modifying the graphene/polyaniline as a cathode of a bioelectrochemical system, and constructing a bipolar chamber bioelectrochemical system for strengthening the decoloration of the azo dye in the water.

Description

Method for removing azo dye by graphene/polyaniline modified electrode enhanced bioelectrochemistry
Technical Field
The invention relates to the field of bioelectrochemistry and the field of wastewater treatment, in particular to a technical method for removing azo dyes by using a graphene/polyaniline modified carbon-based electrode reinforced bioelectrochemical system.
Background
The bioelectrochemical systems (BESs) are a new type of sewage treatment process. The principle is that a system of oxidation or reduction reaction on the surfaces of an anode electrode and a cathode electrode is catalyzed by using a biocatalyst (such as living organisms, organelles, biological enzymes and the like) to promote the conversion between chemical energy and electric energy in substances. The electroactive microorganisms enriched at the BESs anode can oxidize organic matters in the wastewater to generate electrons, and the electrons are transferred to the cathode through an external circuit and can be used for reducing oxidation state substances. Currently, the BESs system has been applied to the removal of organic and inorganic contaminants in wastewater, such as acetate, cellulose, root deposits of rice plants, sulfur, and the like. On the other hand, BESs can reduce nitrate nitrogen and remove refractory pollutants such as nitrobenzene, halogenated organic pollutants and the like at the cathode. Compared with the traditional biological process, BESs have the advantages of rapidness and high efficiency, and can recover electric energy from wastewater treatment.
Azo dyes are among the difficult industrial wastewaters to treat because of their strong oxidizing groups and their bio-toxic intermediates. The traditional anaerobic biological process for degrading azo dyes has low electron utilization rate and more exogenous electron donors. In recent years, many azo dyes have been successfully degraded by a bioelectrochemical system, such as congo red, methyl orange, purple amaranth, reactive brilliant red X-3B, reactive blue 221, orange I, acid orange 7, acid black, reactive red 272, etc., and research shows that the reduction potential of azo bonds of the chromophoric groups of the azo dyes is between-530 mV vs SHE (standard hydrogen electrode) and-180 mV vs SHE, and the cathode potential of BESs can be in the potential range in the power generation mode or the mode of applying smaller voltage, so that the reduction decoloration of the azo dyes can be realized.
At present, with the intensive research, the smaller specific surface area and the larger resistance of the electrodes of the BESs system become bottlenecks which restrict the performance and the practical application of the BESs system. The search for novel BESs electrode material with high performance and low cost is an important way for improving the performance of the BESs electrodes. The conductive polymer polyaniline has high chemical activity, high doping level and excellent specific capacitance, and is the most interesting material in the super capacitor. However, the mechanical strength is weak, and the cycling stability is poor, so that the application of the electrode material as a single electrode material is limited. In order to enhance the stability of polyaniline and thus improve its electrochemical properties, inorganic and organic materials can be combined with polyaniline to prepare composite materials. Graphene is a single-atom thick plane composed of SP 2-bonded carbon atoms, has a large specific surface area, and overcomes the limitation of high resistance due to excellent electrical conductivity of carbon materials. The excellent mechanical strength and chemical stability of the polyaniline nano-composite material can make up the defects of polyaniline materials, and can provide a larger surface for the dispersion and deposition of polyaniline particles.
By preparing the graphene/polyaniline composite material, an electrode material with high electrochemical performance and good biocompatibility can be obtained, and the electrode material is applied to a bioelectrochemical system to construct a bipolar chamber bioelectrochemical system with a built-in graphene/polyaniline electrode, so that the internal resistance of a reaction system can be greatly reduced, the treatment efficiency and the electricity generation efficiency of BESs can be further improved, and meanwhile, the good biocompatibility is favorable for forming a biological membrane.
The invention provides a method for modifying a carbon-based electrode by using electrochemical graphene/polyaniline, which is used as a cathode of a bioelectrochemical system, and a biological cathode is constructed by inoculating microorganisms to enhance the decoloring efficiency of azo dyes.
Disclosure of Invention
The invention aims to provide a technical method for removing azo dyes by using a graphene/polyaniline modified electrode reinforced bioelectrochemical system.
In one aspect of the invention, a preparation method of a graphene/polyaniline modified carbon-based electrode is provided, which comprises the following steps:
(1) diluting the graphene oxide solution to 0.3-0.8g/L by using a citric acid buffer solution with pH of 6 as a first-step electrolyte; the buffer solution is citric acid buffer solution.
(2) Diluting aniline solution by 0.1mol/L to 0.1-0.3mol/L with 0.1mol/L protonic acid to serve as second-step electrolyte; the protonic acid is sulfuric acid or hydrochloric acid;
(3) a carbon-based electrode is adopted as a working electrode, and the carbon-based electrode comprises a carbon fiber brush, a carbon felt or a carbon cloth; cleaning and pre-treating with acetone soaking and acid soaking before use.
(4) Constructing a three-electrode system by using the first-step electrolyte as an electrolyte, a platinum mesh as a counter electrode and Ag/AgCl as a reference electrode; scanning for 30-50 circles by adopting a cyclic voltammetry under the conditions that the scanning range is-1.6V-0.6V vs Ag/AgCl and the scanning speed is 50mV/s, and in-situ generated graphene is deposited on the surface of the carbon-based electrode;
(5) taking the electrolyte in the second step as the electrolyte, taking the working electrode obtained in the step (4) as a working electrode, taking a platinum mesh as a counter electrode, and taking Ag/AgCl as a reference electrode to construct a three-electrode system; and (2) adopting a cyclic voltammetry to generate polyaniline in situ to be modified on the surface of the graphene electrode under the conditions of a scanning range of-0.2V-1V vs Ag/AgCl, a scanning speed of 50mV/s and scanning cycles of 10-20 to prepare the graphene/polyaniline modified carbon-based electrode.
In another aspect of the present invention, there is provided a method for treating wastewater of azo dye using a bioelectrochemical device using a graphene/polyaniline-modified carbon-based electrode as an electrode, the bioelectrochemical device being a bipolar chamber bioelectrochemical device, comprising the steps of:
(1) the cathode is a graphene/polyaniline modified carbon-based electrode, and the anode is an unmodified carbon-based electrode;
(2) the anode is inoculated with microorganisms, and the cathode can be inoculated with or without microorganisms; after the microorganism is inoculated, an electroactive biomembrane is formed on the surface of the electrode; inoculating microorganisms refers to inoculating anaerobic activated sludge of a secondary sedimentation tank on the surface of an electrode;
(3) water is respectively fed into and discharged from an anode chamber and a cathode chamber, the anode chamber is wastewater containing organic pollutants (the wastewater does not contain azo dyes and is easy to degrade, and the easy degradation refers to the azo dyes), and the cathode chamber is wastewater containing the azo dyes;
(4) and a resistor of 5-20 omega is connected between the anode and the cathode.
(5) The anode chamber and the cathode chamber are separated by a diaphragm, and the diaphragm can be a proton exchange membrane or a cation exchange membrane.
(6) A voltage not exceeding 1V is applied between the anode and the cathode.
The step (3) is a sequencing batch or continuous feeding.
Advantageous effects
Compared with the prior art, the invention has the following advantages:
(1) the impedance of the bioelectrochemical device and the electrodes thereof is reduced. According to the invention, the graphene/polyaniline modified carbon-based electrode is utilized, so that the surface area and the electrochemical activity of the electrode in a bioelectrochemical system can be increased, the electron transfer efficiency is enhanced, and the internal resistance and the charge transfer resistance of the bioelectrochemical system are reduced.
(2) The azo dye has high decolorizing efficiency. The invention provides a bioelectrochemical system built by a built-in graphene/polyaniline modified carbon-based electrode, and compared with an anaerobic process, the bioelectrochemical system has the advantages of high decoloring speed and high efficiency.
Drawings
Fig. 1 is a scanning electron microscope image of an unmodified carbon fiber electrode and a graphene/polyaniline modified electrode according to an embodiment of the present invention;
FIG. 2 is a schematic view of a bioelectrochemical system device according to an embodiment of the present invention;
FIG. 3 is a time-varying curve of the output current of the bioelectrochemical system according to the embodiment of the present invention (batch type);
FIG. 4 is a cyclic voltammogram (over a period) of a bioelectrochemical system according to an embodiment of the present invention;
FIG. 5 is an electrochemical impedance diagram of a bioelectrochemical system according to an embodiment of the present invention;
FIG. 6 is a plot of bioelectrochemical dye concentration versus time for an example of the present invention.
Detailed Description
The invention is described in further detail with reference to the accompanying drawings in conjunction with the detailed description.
Example 1
Alizarin Yellow (AYR) was chosen as the characteristic azo dye in this example, and the chemical structure of the dye includes one nitrogen-nitrogen double bond (-N ═ N-) and one nitro (-NO) group2)。
(1) Preparation of graphene/polyaniline electrode
In this example, the graphene/polyaniline electrode is prepared in two steps. Firstly, diluting a graphene oxide aqueous solution to 0.5g/L by using a 0.1mol/L citric acid buffer solution (PH is 6), and performing ultrasonic treatment for 40min to form a stable colloid dispersion solution; and constructing a three-electrode system by using the graphene oxide dispersion solution as an electrolyte, a carbon fiber electrode as a carbon-based electrode, a platinum mesh as a counter electrode and Ag/AgCl as a reference electrode. And reducing the graphene oxide by using a cyclic voltammetry under a continuous stirring condition, wherein the scanning range is-1.6V-0.6V vs Ag/AgCl, the scanning rate is 50mV/s, and the number of scanning cycles is 40. The graphene oxide is continuously reduced and deposited on the surface of the carbon fiber. Then, the aniline solution was diluted to 0.1mol/L with 0.1mol/L sulfuric acid and sonicated for 40min to disperse it uniformly. And (3) constructing a three-electrode system by taking the aniline dispersion solution as electrolyte and taking the electrode modified by the graphene as a working electrode. Aniline is continuously oxidized and reduced by cyclic voltammetry under the condition of continuous stirring, the scanning range is-0.2V-0.8V vs Ag/AgCl, the scanning speed is 50mV/s, and the number of scanning cycles is 15. Fig. 1 shows scanning electron micrographs of an unmodified carbon fiber electrode and a graphene/polyaniline modified electrode. The surface of the unmodified electrode is smooth, and graphene sheets in a corrugated or ripple shape are stacked on the surface of the electrode modified by graphene/polyaniline, so that the electrode is compact and uniform, and the surface area of the electrode is increased. On the graphene lamellar structure, granular polyaniline which is uniformly distributed can be seen, and the improvement of the conductivity of the electrode and the increase of the surface area of the electrode are facilitated.
(2) Construction of a bioelectrochemical System
The bioelectrochemical system constructed in this embodiment mainly consists of an anode chamber and a cathode chamber, and the anode chamber and the cathode chamber are separated by a proton exchange membrane, as shown in fig. 2. In the example, the reaction device is made of organic glass, the volumes of the two chambers are both 100ml, the inside of the rectangular appearance is cylindrical, the anode is an unmodified carbon fiber electrode, the cathode is a prepared graphene/polyaniline carbon fiber electrode, and Ag/AgCl is selected as a reference electrode; both the anode and the cathode are inoculated with activated sludge; the device is externally applied with 0.7V constant voltage, and the circuit is externally connected with a 10 omega resistor; the anode and cathode chambers are fed with water intermittently, the anolyte takes 2g/L sodium acetate as carbon source, and the catholyte contains 30mg/L azo dye. Fig. 3 is a current periodic variation diagram of a device, and the peak current of a bioelectrochemical system using a graphene/polyaniline modified electrode as a cathode is 1.2 times that of a control device (using an unmodified electrode as a cathode).
(3) Degradation of azo dye alizarin yellow
The degradation process of alizarin yellow in the cathode conforms to the first-order reaction kinetics law, namely C (t) ═ C0e (-kt), wherein (C)0The initial concentration of alizarin yellow, k is a kinetic constant, and t is the reaction time), and the larger the value of the kinetic constant k of the reaction is, the faster the dye is degraded. The alizarin yellow decolorization rate constant of the bioelectrochemical system with the built-in graphene/polyaniline carbon fiber electrode is obtained by fitting according to an equation and is 0.18 which is greater than 0.16 of the unmodified carbon fiber electrode, and the decolorization rate is high. The decolorization rate of a bioelectrochemical system of the graphene/polyaniline carbon fiber electrode reaches 94% within 24h, and the decolorization rate of alizarin yellow of the bioelectrochemical system of the unmodified carbon fiber electrode is 81% within 24 h.
(4) Impedance change of bioelectrochemical system
By using an electrochemical workstation, an impedance result of the bioelectrochemical system is obtained through alternating current impedance scanning, as shown in fig. 5, Rs represents ohmic internal resistance, Rct represents charge transfer resistance, Wo represents diffusion internal resistance, and the Rs resistance value of the electrochemical system with the built-in graphene/polyaniline electrode is 87 ohms smaller than that of an unmodified electrode.
The results show that the bioelectrochemical system with the built-in graphene/polyaniline electrode can reduce the internal resistance of the electrochemical system and improve the decoloring efficiency of azo dyes.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (4)

1. A preparation method of a graphene/polyaniline modified carbon-based electrode is characterized by comprising the following steps:
(1) diluting the graphene oxide solution to 0.3-0.8g/L by using a citric acid buffer solution with pH of 6 as a first-step electrolyte; the buffer solution is citric acid buffer solution;
(2) diluting aniline solution by 0.1mol/L to 0.1-0.3mol/L with 0.1mol/L protonic acid to serve as second-step electrolyte; the protonic acid is sulfuric acid or hydrochloric acid;
(3) a carbon-based electrode is adopted as a working electrode, and the carbon-based electrode comprises a carbon fiber brush, a carbon felt or a carbon cloth; cleaning and pretreating by using acetone soaking and acid soaking before use;
(4) constructing a three-electrode system by taking the first-step electrolyte as an electrolyte, a platinum mesh as a counter electrode and Ag/AgCl as a reference electrode; adopting cyclic voltammetry to scan 30-50 circles under the conditions of a scanning range of-1.6V-0.6 Vvs Ag/AgCl and a scanning rate of 50mV/s, and depositing the in-situ generated graphene on the surface of the carbon-based electrode;
(5) taking the electrolyte obtained in the second step as the electrolyte, taking the working electrode obtained in the step (4) as a working electrode, taking a platinum mesh as a counter electrode and taking Ag/AgCl as a reference electrode, and constructing a three-electrode system; and (2) adopting a cyclic voltammetry to generate polyaniline in situ to be modified on the surface of the graphene electrode under the conditions of a scanning range of-0.2V-1V vs Ag/AgCl, a scanning speed of 50mV/s and scanning cycles of 10-20 to prepare the graphene/polyaniline modified carbon-based electrode.
2. The graphene/polyaniline modified carbon-based electrode prepared by the method of claim 1.
3. A method for treating wastewater of azo dyes by using the bioelectrochemical device which uses the graphene/polyaniline-modified carbon-based electrode prepared by the method of claim 1 as an electrode, comprising the following steps of:
(1) the cathode is a graphene/polyaniline modified carbon-based electrode, and the anode is an unmodified carbon-based electrode;
(2) the anode is inoculated with microorganisms, and the cathode can be inoculated with or without microorganisms; after the microorganism is inoculated, an electroactive biomembrane is formed on the surface of the electrode; inoculating microorganisms refers to inoculating anaerobic activated sludge of a secondary sedimentation tank on the surface of an electrode;
(3) water is respectively fed into and discharged from the anode chamber and the cathode chamber, the anode chamber is wastewater containing organic pollutants, and the cathode is wastewater containing azo dyes; the wastewater containing the organic pollutants is easily degradable organic pollutants without containing azo dyes, wherein the easy degradation refers to the condition of the azo dyes;
(4) a resistor of 5-20 omega is connected between the anode and the cathode;
(5) the anode chamber and the cathode chamber are separated by a diaphragm, and the diaphragm can be a proton exchange membrane or a cation exchange membrane;
(6) a voltage not exceeding 1V is applied between the anode and the cathode.
4. A method according to claim 3, wherein said step (3) is a batch or continuous feed.
CN202210401044.XA 2022-04-14 2022-04-14 Method for removing azo dye by graphene/polyaniline modified electrode enhanced bioelectrochemistry Pending CN114735806A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102760888A (en) * 2012-07-16 2012-10-31 北京工业大学 Preparation and application of graphene/substrate electrode and polyaniline-graphene/substrate electrode
CN111430730A (en) * 2020-03-31 2020-07-17 北京工业大学 Preparation method of graphene modified carbon-based electrode and microbial electrochemical sewage treatment synchronous electricity generation device constructed by using same
CN112830567A (en) * 2021-01-07 2021-05-25 南开大学 Application of induced polyaniline loaded graphene modified electrode reactor and Congo red removing method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102760888A (en) * 2012-07-16 2012-10-31 北京工业大学 Preparation and application of graphene/substrate electrode and polyaniline-graphene/substrate electrode
CN111430730A (en) * 2020-03-31 2020-07-17 北京工业大学 Preparation method of graphene modified carbon-based electrode and microbial electrochemical sewage treatment synchronous electricity generation device constructed by using same
CN112830567A (en) * 2021-01-07 2021-05-25 南开大学 Application of induced polyaniline loaded graphene modified electrode reactor and Congo red removing method

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