CN110444768B - Preparation of activated carbon composite cathode and application of coupled microbial fuel cell system in industrial organic acid wastewater treatment - Google Patents

Preparation of activated carbon composite cathode and application of coupled microbial fuel cell system in industrial organic acid wastewater treatment Download PDF

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CN110444768B
CN110444768B CN201910634258.XA CN201910634258A CN110444768B CN 110444768 B CN110444768 B CN 110444768B CN 201910634258 A CN201910634258 A CN 201910634258A CN 110444768 B CN110444768 B CN 110444768B
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柳丽芬
张倩
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Dalian University of Technology
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Abstract

Preparation of active carbon composite cathode and coupling microbial fuel cell system for industrial organic acid wastewater treatment, wherein active carbon particles are used as a substrate, and MnO is loaded by in-situ growth and a sol-gel method2/TiO2/g‑C3N4. Using MnO2/TiO2/g‑C3N4The @ GAC cathode is coupled with the microbial fuel cell to realize the high-efficiency treatment of the high-concentration industrial organic acid wastewater. The electrode has excellent conductivity, high electrochemical performance, high oxygen reduction capacity and high pollution resistance, and can keep high activity and stability after long-term operation. The organic acid wastewater is used as an MFC cathode to treat actual industrial organic acid wastewater, so that the power generation capacity of a system can be improved, the ORR reaction and the removal of pollutants are promoted, the quality of effluent water is improved, and long-term continuous and stable operation is achieved. The system is simple and convenient to operate, high in treatment efficiency and large in volume load, can realize long-term stability of the effluent quality of the device, and is favorable for carrying out amplification experiments.

Description

Preparation of activated carbon composite cathode and application of coupled microbial fuel cell system in industrial organic acid wastewater treatment
Technical Field
The present invention belongs to the field of waste water treating and energy recovering technologyDomain, relates to a high-efficiency MnO2/TiO2/g-C3N4The preparation of the @ GAC electrode and the cathode coupling microbial fuel cell system have obvious effect when treating high-concentration industrial organic acid wastewater. The specific research and development contents are that activated carbon particles are used as a substrate, MnO is loaded by in-situ growth and a sol-gel method2/TiO2/g-C3N4To manufacture a composite electrode. The electrode has good conductivity and electrocatalysis performance, high porosity and large specific surface area, and is beneficial to the attachment and growth of the cathode facultative anaerobe. The method is applied to a Microbial Fuel Cell (MFC) system as a cathode, realizes capacity while treating high-concentration industrial organic acid wastewater, has low system operation cost, good effluent quality and large bearing capacity, and has certain engineering advantages.
Background
In the production process of adipic acid, the produced high-concentration industrial organic acid wastewater contains high-concentration nitrogen and heavy metal Cu pollution, has high COD (chemical oxygen demand) and strong acidity, has pH value of about 1, has serious influence on the environment and is one of industrial wastewater which is difficult to treat.
The microbial fuel cell combines sewage treatment and biological electricity generation, utilizes electricity generation microbes to oxidize organic pollutants and generate electrons simultaneously, and continuously transmits the electrons out to form electric energy, thereby realizing the recycling of energy, and being a typical bioelectrochemical system. Compared with the traditional sewage biological treatment technology and the traditional fuel cell, the microbial fuel cell can degrade organic matters and bottom mud in water and obtain electric energy, has the advantages of simple and convenient operation, low operation requirement, mild condition, recycling, environmental cleanness, friendliness and the like, and has wide research and development potential. But the problems of large internal resistance of the battery, small output power, low coulombic efficiency, poor effluent quality and the like still exist at present.
In addition, the high cost of microbial fuel cell electrodes is also an important factor limiting the further development and application of MFCs. The cathode electrode material has important influence on the treatment effect and the electricity generation performance of the MFC, and the material and the structure of the cathode electrode material can influence the conductivity of the electrode so as to influence the output power of a system and can also influence the cathode oxygen reduction reaction so as to influence the removal effect of pollutants. Generally, a carbon material having high electrical conductivity and being porous and loose is suitable for use as a cathode of MFC. But the catalyst is directly used, and has poor catalytic performance and poor effect. Therefore, the catalyst (such as a semiconductor material and the like) with high activity can be used for modifying the catalyst so as to improve the catalytic performance of the material, accelerate the oxygen reduction reaction and improve the pollutant removal efficiency.
The invention sequentially loads MnO on active carbon particles by in-situ growth, a sol-gel method and an oxygen and nitrogen isolating high-temperature calcination technology2/TiO2/g-C3N4And the catalytic performance of the electrode is improved. The composite electrode developed by the patent has strong conductivity and oxygen reduction capability, can obviously improve the cell potential of the microbial fuel cell, and has good pollution resistance; the high porosity and specific surface area contribute to the entrapment and degradation of contaminants. MnO2/TiO2/g-C3N4The @ GAC cathode coupled microbial fuel cell has good effluent quality when used for treating actual organic acid wastewater, and can stably operate for a long time.
Disclosure of Invention
The invention aims to provide MnO2/TiO2/g-C3N4The @ GAC composite cathode coupled microbial fuel cell and the high-concentration industrial organic acid wastewater treatment application have the advantages that the electrode has good conductivity and electrocatalysis, the cathode oxygen reduction reaction is promoted, the electricity generation is improved, and the problems of poor effluent quality, small electric energy output, low high-concentration industrial organic acid wastewater treatment efficiency, complex process and the like of the traditional microbial fuel cell are solved.
The technical scheme of the invention is as follows:
a preparation method of an active carbon composite cathode comprises the following steps:
(1) soaking the activated carbon particles in 0.05mol/L potassium permanganate solution for more than 3 hours, taking out, washing with deionized water for 3-5 times, and drying at 100 ℃ for 4 hours;
(2) calcining the treated activated carbon particles obtained in the step (1) at 350 ℃ for 3h, heating at the rate of 5 ℃/min, and continuously introducing nitrogen in the period of time without oxygen to prepare MnO2@GAC；
(3) Calcining melamine at 550 ℃ for 4h, heating at the rate of 5 ℃/min to obtain a light yellow solid, grinding the light yellow solid, sieving, uniformly mixing the light yellow solid in 18.5 wt.% hydrochloric acid solution, and uniformly dispersing by ultrasonic; then centrifugally washing the solution by deionized water until Ph is 7, and drying the solution to obtain g-C3N4Standby;
(4) mixing ethanol, pure water, concentrated hydrochloric acid, butyl titanate, and g-C3N4According to the volume ratio of 1700 mL: 30mL of: 1mL of: 100mL of: 1.85g of the mixture is uniformly mixed and kept stand for 48 hours;
(5) MnO prepared in the step (2)2Adding the @ GAC into the mixed solution obtained in the step (4), stirring, and drying at 60-80 ℃ for 4-6 h; placing the dried solid in a tube furnace, calcining for 2-3 h at 400 ℃, heating at the rate of 5 ℃/min, and continuously introducing nitrogen in the period to obtain MnO2/TiO2/g-C3N4@ GAC for use.
The coupled microbial fuel cell system is constructed by adopting an active carbon composite cathode: the microbial fuel cell is of a left-right structure, and the anode chamber and the cathode chamber are separated by a proton exchange membrane; active carbon particles loaded with electrogenesis microorganisms are filled in an anode chamber of the microbial fuel cell, the filling rate is 85% -95%, a carbon rod 1 is used as an anode, and one end of the carbon rod is connected with a lead and then led out; a saturated calomel electrode is used as a reference electrode and is inserted into the anode chamber in parallel with the carbon rod 1, the carbon rod 1 and the saturated calomel electrode are respectively externally connected into a data acquisition system, and the electricity generation condition of the anode is continuously monitored in real time; MnO in step (5) for filling cathode chamber of microbial fuel cell2/TiO2/g-C3N4The method comprises the following steps of @ GAC, installing an aeration head at the bottom of the GAC, controlling aeration quantity, introducing electrons generated by an anode into a cathode chamber by using a carbon rod 2, externally connecting a lead, connecting the lead with the carbon rod 1 and an external resistor in series, and connecting the carbon rod 2 into a data acquisition system; high-concentration organic acid wastewater continuously enters the bottom of the anode chamber through the water inlet flow regulating device, enters the bottom of the cathode chamber from the upper part of the anode chamber through the overflow device, and finally flows out of the treated effluent from the overflow device at the upper part of the cathode chamber.
Application of coupled microbial fuel cell system: before the industrial organic acid wastewater enters the reactor, adjusting the pH to 5-6, domesticating microorganisms in an anode chamber of the reactor through the diluted industrial organic acid wastewater in the early stage of the operation of the reactor, and gradually increasing the water inlet concentration when the power generation and effluent quality of a system are stable; the operation mode is continuous operation, and the hydraulic retention time is 8-12 h.
The invention has the beneficial effects that: the invention prepares MnO by using cheap and easily available materials2/TiO2/g-C3N4The @ GAC composite electrode has excellent conductivity, high electrochemical performance, high oxygen reduction capacity and high pollution resistance, and can keep high activity and stability after long-term operation. The MnO2/TiO2/g-C3N4The @ GAC composite cathode coupled microbial fuel cell is used for actual organic acid wastewater treatment, can improve the electricity generation capacity of a system, promotes oxygen reduction reaction and pollutant elimination, effectively improves effluent water quality, and can effectively intercept thalli and particulate matters, so that the number of negative-pole facultative anaerobes is increased, the whole biomass conversion is increased, the volume load is large, and the treatment efficiency is high. The system has simple structure and convenient operation, is suitable for continuous treatment of high-concentration organic acid wastewater, and can realize the long-term stability of the effluent quality of the device.
Drawings
FIG. 1 shows MnO in the present invention2/TiO2/g-C3N4Graph of CV for the @ GAC electrode.
Fig. 2 is a diagram of the effluent COD removal performance of the activated carbon substrate composite electrode microbial fuel cell system.
In the figure: the abscissa represents time in units d; the ordinate represents the effluent concentration and the removal efficiency in mg/L and percent; the dots represent the COD effluent concentration and the triangles represent the COD removal efficiency.
FIG. 3 shows effluent NH of an active carbon substrate composite electrode microbial fuel cell system4 +-N removal performance map.
In the figure: the abscissa represents time in units d; the ordinate represents the effluent concentration and the removal efficiency in mg/L and percent; dots represent NH4 +N effluent concentration, triangle for NH4 +-N removal efficiency.
FIG. 4 shows effluent NO of activated carbon substrate composite electrode microbial fuel cell system3 --N removal performance map.
In the figure: the abscissa represents time in units d; the ordinate represents the effluent concentration and the removal efficiency in mg/L and percent; dots indicating NO3 -N effluent concentration, triangle for NO3 --N removal efficiency.
Fig. 5 is a potential diagram of an activated carbon substrate composite electrode microbial fuel cell system.
In the figure: the abscissa represents time in units d; the ordinate represents voltage, in units V; circles represent cell potential, positive triangles represent anode potential, and diamonds represent cathode potential.
Detailed Description
The following detailed description of the embodiments of the invention is provided in connection with the accompanying drawings and the appended claims.
Example 1: MnO2/TiO2/g-C3N4Preparation of @ GAC electrode
(1)MnO2Preparation of @ GAC: soaking 100g of activated carbon particles in 300mL of potassium permanganate solution with the concentration of 0.05mol/L for 3h, taking out, washing with deionized water for a plurality of times, drying at 100 ℃, calcining the obtained activated carbon particles at 350 ℃ for 3h, heating at the rate of 5 ℃/min, continuously isolating oxygen and introducing nitrogen during the heating, washing and drying to obtain MnO2@ GAC for standby;
(2) calcining melamine at 550 ℃ for 4h, heating at the rate of 5 ℃/min to obtain a light yellow solid, grinding the light yellow solid, screening, uniformly mixing the light yellow solid in 18.5% hydrochloric acid solution, and carrying out ultrasonic treatment for 6 h. Then centrifugally washing the solution by deionized water until Ph is 7, and drying the solution to obtain g-C3N4Powder is reserved; adding 680mL ethanol into 1000mL beaker, adding 12mL pure water and 0.4mL concentrated hydrochloric acid under magnetic stirring, mixing, slowly adding 40mL butyl titanate, and stirring while adding 0.74 g-C3N4Then, continuously stirring for 1h, standing for 48h, and repeatedly stirring and standing in the period; then MnO is added2@ GAC was added to the above solution, stirred and dried at 80 ℃. Placing the dried solid inCalcining in a tube furnace at 400 ℃ for 2h, and continuously introducing nitrogen during the calcining to obtain MnO2/TiO2/g-C3N4@ GAC electrode. As can be seen from the CV diagram of the electrode in potassium ferricyanide solution of FIG. 1, MnO was successfully prepared in comparison with pure activated carbon particles2/TiO2/g-C3N4The @ GAC composite electrode has good redox activity.
Example 2: MnO2/TiO2/g-C3N4Treatment of organic acid wastewater by virtue of @ GAC cathode coupled microbial fuel cell
(1) Construction of a coupling system: the anode chamber of the microbial fuel cell is designed to be 5 multiplied by 15cm in size, activated carbon particles loaded with electrogenesis microbes are filled in the anode chamber, the filling rate is about 90 percent, the carbon rod 1 is used as the anode and has the size of phi 5 multiplied by 100mm, and one end of the carbon rod is connected with a lead and then is led out; the saturated calomel electrode is used as a reference electrode and is inserted into the anode chamber in parallel with the carbon rod, and the carbon rod and the saturated calomel electrode are respectively externally connected into a data acquisition system to continuously monitor the electricity generation condition of the anode in real time. The anode chamber and the cathode chamber are connected by a proton exchange membrane, the cathode chamber is 5 multiplied by 4 multiplied by 15cm in size and is filled with prepared MnO2/TiO2/g-C3N4@ GAC, about 80g, the filling rate is about 80%, the bottom is installed with the aeration head and is controlled the aeration rate, the electron that produces the positive pole with carbon-point 2 is leading-in cathode chamber to external conductor links to each other with data acquisition system, 1000 omega external resistance of series connection between carbon-point 2 and positive pole carbon-point 1. The wastewater continuously enters the bottom of the anode chamber through the water inlet flow regulating device and enters the bottom of the cathode chamber from the upper part of the anode chamber through the overflow device, and finally the treated effluent flows out of the overflow device 3cm away from the top of the cathode chamber.
(2)MnO2/TiO2/g-C3N4The @ GAC cathode coupled microbial fuel cell is used for industrial organic acid wastewater treatment: the actual industrial organic acid wastewater is taken as inlet water (COD is about 8000mg/L), the inlet water concentration is from low to high, and the pH value needs to be adjusted to 5-6 before entering a reactor. The COD of the inlet water in the initial stage of the operation of the reactor is about 2000mg/L, and the inlet water of the reactor is sequentially increased to 40%, 60%, 80% and 100% of the raw water after the quality of the outlet water, the anode potential and the battery potential are stable. Inverse directionThe hydraulic retention time of the reactor in the early stage of operation is 8h, and when the inlet water is raw water, the hydraulic retention time is prolonged to 12 h. Taking the overflow effluent every 24h to test COD and NH4 +-N、NO3 -Indexes such as-N, as shown in figures 2-4, when the system is used for treating high-concentration organic acid wastewater, the COD removal rate is more than 96%, and NH4 +The removal rate of-N is more than 99 percent, NO3 -The removal rate of-N is more than 94 percent, which shows that the system can stably and effectively purify high-concentration industrial organic acid wastewater. Fig. 5 is a diagram of the power generation performance of the system, which illustrates that the system can improve the power generation of the system while realizing the high-efficiency treatment of wastewater.

Claims (3)

1. The preparation method of the active carbon composite cathode is characterized by comprising the following steps:
(1) soaking the activated carbon particles in 0.05mol/L potassium permanganate solution for more than 3 hours, taking out, washing with deionized water for 3-5 times, and drying at 100 ℃ for 4 hours;
(2) calcining the treated activated carbon particles obtained in the step (1) at 350 ℃ for 3h, heating at the rate of 5 ℃/min, and continuously introducing nitrogen in the period of time without oxygen to prepare MnO2@GAC；
(3) Calcining melamine at 550 ℃ for 4h, heating at the rate of 5 ℃/min to obtain a light yellow solid, grinding the light yellow solid, sieving, uniformly mixing the light yellow solid in 18.5 wt.% hydrochloric acid solution, and uniformly dispersing by ultrasonic; then centrifugally washing the solution by deionized water until Ph is 7, and drying the solution to obtain g-C3N4Standby;
(4) mixing ethanol, pure water, concentrated hydrochloric acid, butyl titanate, and g-C3N4According to the volume ratio of 1700 mL: 30mL of: 1mL of: 100mL of: 1.85g of the mixture is uniformly mixed and kept stand for 48 hours;
(5) MnO prepared in the step (2)2Adding the @ GAC into the mixed solution obtained in the step (4), stirring, and drying at 60-80 ℃ for 4-6 h; placing the dried solid in a tube furnace, calcining for 2-3 h at 400 ℃, heating at the rate of 5 ℃/min, and continuously introducing nitrogen in the period to obtain MnO2/TiO2/g-C3N4@ GAC for use.
2. A coupled microbial fuel cell system is constructed by adopting the activated carbon composite cathode prepared in the claim 1, and is characterized in that the microbial fuel cell is of a left-right structure, and an anode chamber and a cathode chamber are separated by adopting a proton exchange membrane; active carbon particles loaded with electrogenesis microorganisms are filled in an anode chamber of the microbial fuel cell, the filling rate is 85% -95%, a carbon rod 1 is used as an anode, and one end of the carbon rod is connected with a lead and then led out; a saturated calomel electrode is used as a reference electrode and is inserted into the anode chamber in parallel with the carbon rod 1, the carbon rod 1 and the saturated calomel electrode are respectively externally connected into a data acquisition system, and the electricity generation condition of the anode is continuously monitored in real time; MnO in step (5) for filling cathode chamber of microbial fuel cell2/TiO2/g-C3N4The method comprises the following steps of @ GAC, installing an aeration head at the bottom of the GAC, controlling aeration quantity, introducing electrons generated by an anode into a cathode chamber by using a carbon rod 2, externally connecting a lead, connecting the lead with the carbon rod 1 and an external resistor in series, and connecting the carbon rod 2 into a data acquisition system; high-concentration organic acid wastewater continuously enters the bottom of the anode chamber through the water inlet flow regulating device, enters the bottom of the cathode chamber from the upper part of the anode chamber through the overflow device, and finally flows out of the treated effluent from the overflow device at the upper part of the cathode chamber.
3. The application of the activated carbon composite cathode to construction of a coupled microbial fuel cell system is characterized in that before industrial organic acid wastewater enters a reactor, the pH is adjusted to 5-6, microorganisms in an anode chamber of the reactor are acclimated by the diluted industrial organic acid wastewater in the early stage of operation of the reactor, and when the power generation and effluent quality of the system are stable, the influent concentration is gradually increased; the operation mode is continuous operation, and the hydraulic retention time is 8-12 h.
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