CN111606526A - Novel method for developing oil-based mud by treating shale gas through double-chamber microbial fuel cell - Google Patents
Novel method for developing oil-based mud by treating shale gas through double-chamber microbial fuel cell Download PDFInfo
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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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/006—Electrochemical treatment, e.g. electro-oxidation or electro-osmosis
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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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/02—Biological treatment
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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
- H01M8/04—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids
- H01M8/04223—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids during start-up or shut-down; Depolarisation or activation, e.g. purging; Means for short-circuiting defective fuel cells
- H01M8/04225—Auxiliary arrangements, e.g. for control of pressure or for circulation of fluids during start-up or shut-down; Depolarisation or activation, e.g. purging; Means for short-circuiting defective fuel cells during start-up
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
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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
A method for treating organic matters in oil-based mud generated by shale gas development by using a double-chamber microbial fuel cell belongs to the technical field of organic wastewater treatment. The invention firstly constructs a double-chamber Microbial Fuel Cell (MFC), anaerobic activated sludge obtained by culturing aerobic activated sludge of a sewage treatment plant is used as anolyte, fresh aerobic sludge is used as catholyte, nutrient solution is added into the anolyte and the catholyte, the MFC is started at the additional rotating speed of 0-200r/min in an anode area of the MFC, after three periods of stabilization, certain nutrient substance is added into a cathode chamber to maintain the growth of microorganisms, and the MFC is prepared by the steps ofThe anaerobic sludge substrate of the anode chamber is replaced by oil-based mud, the MFC is operated at room temperature and constant pressure, the additional rotating speed of the anode area of the MFC is 0-200r/min, organic pollutants in the oil-based mud can be effectively removed, and meanwhile, electric energy can be recycled. The method has the advantages of simple equipment, convenient operation, energy conservation and no secondary pollution. When the stirring speed of the anode region is 100r/min, the maximum power density of the MFC system reaches 10.08W/m2And the internal resistance is minimum, the ohmic polarization loss is minimum, and the COD removal rate can reach 50.4 +/-0.3%.
Description
Technical Field
The invention relates to a method for treating organic matters in oil-based mud generated by shale gas development through a double-chamber microbial fuel cell, belonging to the technical field of organic wastewater treatment.
Background
With the increasing number of complex shale gas wells, the pollution degree caused by the oil-based drilling fluid is higher and higher, and the conventional methods of direct discharge, in-situ burying, in-pit solidification and the like are the main treatment modes of the waste drilling fluid at present. In recent years, the goal of "zero emission" of waste drilling fluids has been addressed in many countries, namely by implementing a harmless "no-landing" treatment of the waste drilling fluids. Therefore, how to overcome the pollution problem of the oil-based mud to fully exert the advantages thereof has become an important issue of environmental protection. At present, the main treatment modes adopted by China for organic mud comprise technologies such as tempering, mechanical stripping, solvent extraction, recharge profile control, ultrasonic treatment and the like, for example, in the 5 th phase of Shanghai environmental science in 2000, the solvent extraction-steam distillation method is used for treating oily sludge (a comparison document 1), after the oily sludge is extracted by adding 3 times of chloroform solvent at room temperature, 0.5mL of water is added into 1g of oily sludge, and distillation is carried out for 45min at the temperature of 400 ℃ and the pressure of 0.2MPa, wherein the deoiling rate can reach more than 80%. However, there are the following problems: (1) the operation process and the flow are complex; (2) the dosage of the extractant is large, the price of the extractant is expensive, and the treatment cost is high. At present, the process for treating the oily sludge by using the solvent extraction method is not widely applied in China.
The development trend of treating refractory high-concentration organic wastewater gradually takes biotechnology as the main stream, and although a microorganism and plant restoration method is relatively friendly environment restoration technology, the limitation of climate and environment factors is serious, and the maintenance cost is high. Ecological remediation is a currently favored remediation technology, of which Microbial Fuel Cells (MFCs) are one. The method is a component for converting chemical energy (fuel) into electric energy by means of catalytic reaction of microorganisms, and is an important means for realizing harmless and recycling of wastewater. For example, "Water Research" volume 147 of "Simultaneous removal of organic matter and ironfrom" 2018(comparative document 2), a microbial fuel cell using sulfur as a circulating medium and NaCl as a catholyte, and a multi-batch treatment of the simulated fracturing flow-back fluid, wherein the COD value of the waste liquid is reduced to 200-300 mg/L from 1348 +/-112 m/L, and the power density is 2667 +/-529 mW/m3The feasibility of the oily wastewater as a microbial fuel cell matrix is proved. But the method has the following disadvantages: (1) suspended solids in the wastewater need to be pretreated, and the process is complicated; (2) NaCl in the catholyte has the risk of secondary pollution, and needs to be subjected to desalination treatment after the operation of the battery is finished; (3) compared with actual wastewater, the simulated shale gas flowback wastewater has single component, low organic carbon concentration and low reference value in actual application.
In combination with the fact that no report related to the treatment of oil-based mud by using a microbial fuel cell is seen at present, the invention provides the application of MFC technology to treat petroleum/organic pollutants in the oil-based mud and converts biomass in the mud into electric energy in oxidation-reduction. But mass transfer resistance existing in the anode substrate with higher concentration can affect the diffusion rate of the substrate and microorganisms to the surface of the electrode, thereby affecting the formation and growth of a biological film; secondly, the diffusion of protons to the cathode is influenced by the larger mass transfer resistance, so that the rapid progress of the cathode reaction is hindered, and the internal resistance of the system is increased. Therefore, the influence of the stirring speed on the power generation performance and the pollutant removal efficiency of the MFC is optimized, so that the mud can be fully reduced, harmlessly recycled, and the aerobic sludge almost without cost is used as the catholyte, so that the MFC has a good application prospect.
Disclosure of Invention
The invention aims to provide a novel method for treating oil-based mud by using MFC (microbial fuel cell) technology of electrogenesis bacteria and denitrifying bacteria, which is low in cost and environment-friendly, so that the mud is effectively degraded, and chemical energy of organic matters in the mud can be converted into electric energy. And in order to further optimize the MFC performance, the mass transfer condition of the anode area of the MFC is stirred by applying magnetic force to the anode area, so that the degradation of organic pollutants in the oil-based mud is promoted while the output power of the battery is improved.
The oil-based mud treatment method provided by the invention comprises the following steps:
(1) construction of a two-compartment microbial fuel cell
An H-shaped double-chamber microbial fuel cell device is constructed by selecting organic glass, the schematic diagram of the device is shown in figure 1, and an anode chamber is in a sealed state except a charging opening and a wire guide hole which are reserved on an upper cover of the device; the cathode chamber is in a semi-sealed state and supplies dissolved oxygen for catholyte through a blast aeration device; the anode chamber and the cathode chamber are connected through a flange, the middle part is separated by a Nafion 117 proton exchange membrane, the carbon felt and the carbon cloth are connected by a copper wire to be used as electrode materials of an anode and a cathode and are connected with a 1000 omega load resistor to form an external circuit, and MFC voltage data are collected by a parallel data collector.
(2) Starting of a two-compartment microbial cell
And starting the microbial fuel cell by respectively taking the cultured anaerobic sludge and aerobic sludge as substrates of the anode chamber and the cathode chamber. The reactor adopts an intermittent operation mode, and the additional rotating speed of the anode area of the MFC is 0-200 r/min; after three cycles of operation, the output voltage of the MFC can be kept stable for a long time, the maximum output voltage of each cycle is close, and the starting of the MFC is finished.
(3) Operating a microbial fuel cell based on oil-based mud
Adding certain nutrient substances into the cathode chamber to maintain the growth of microorganisms, replacing the anaerobic sludge substrate of the anode chamber with oil-based mud, operating the MFC at room temperature and constant pressure, collecting anolyte every day to measure the COD concentration of the anolyte at an additional rotating speed of 0-200r/min, and recording the output voltage of the anolyte.
[ the beneficial effects of the above technical solution of the present invention are as follows ]:
firstly, the invention directly realizes the effective degradation of the slurry in the microbial fuel cell without the pretreatment of the slurry, which is superior to that of the comparison document 2; the invention can recover electric energy while removing pollutants in the wastewater, and is superior to the comparison document 1.
Secondly, the catholyte in the comparison document 2 uses NaCl, while the microbial fuel cell of the invention uses aerobic sludge without cost, thereby reducing the cost, avoiding possible secondary pollution and having better electricity generation effect.
Thirdly, the proper stirring speed can enhance the activity of the electricity-generating microorganisms of the MFC system and the effect of decomposing organic matters, thereby further improving the performance of the MFC.
Description of the drawings:
FIG. 1 is a schematic diagram of a microbial fuel cell sludge treatment apparatus, wherein: 1. an anode chamber, 2. electrogenic bacteria, 3. a magnetic stirrer, 4. a proton exchange membrane, 5. a cathode chamber, 6. oxygen bubbles, 7. a resistance box, and 8. electrons;
FIG. 2 is a graph of voltage versus time at various agitation rates;
FIG. 3 is a plot of polarization at different agitation rates;
FIG. 4 is a graph of power density at various agitation rates.
Detailed Description
The present invention will be further described with reference to the following specific embodiments.
Example 1
A method for processing shale gas to develop oil-based mud by using a double-chamber microbial fuel cell comprises the following specific steps:
(1) construction of a two-compartment microbial fuel cell
Selecting an H-type double-chamber microbial fuel cell made of organic glass as an anode chamber and a cathode chamber of the experimental device, wherein the effective volumes of the H-type double-chamber microbial fuel cell are 800mL, adding 1mol/L HCl and 1mol/L NaOH solution into the anode chamber respectively to soak for 1 hour after each MFC is assembled so as to remove metal ions and other microorganisms which may exist, washing with sterile water for several times until the solution is neutral for later use, and keeping the anode chamber in a sealed state except a charging opening and a wire guide hole reserved on an upper cover of the device; the cathode chamber is in a semi-sealed state, and dissolved oxygen is provided for catholyte through a blast aeration device; the anode chamber and the cathode chamber are connected by a flange with the length of 50mm and the diameter of 30mm, and the effective area of the middle part is 7.07cm2Is separated by a Nafion 117 proton exchange membrane which is boiled with hydrogen peroxide with the concentration of 10 percent, deionized water and 0.5mol/L sulfuric acid before use so as to fully remove impurity oxidation products on the surface of the membrane, a carbon felt with the area of 6cm and × 4cm and a carbon fiber with the area of 0.5mol/LThe carbon cloth is connected by a copper wire and respectively used as an anode and a cathode, before use, 10% hydrogen peroxide is cooked for 3 hours at a constant temperature of 90 ℃, then is cooked for 1 hour by deionized water, and finally the electrode material is cleaned and dried at a constant temperature; the anode is buried at a position 4cm away from the bottom of the container, the cathode is half exposed in the air to ensure full contact with the air, and is connected with a 1000 omega load resistor to form an external circuit, and the voltage data of the MFC is acquired by a parallel data acquisition instrument.
(2) Startup of a two-compartment microbial fuel cell
Preparing 1g/L glucose nutrient solution and cultured anaerobic sludge at a ratio of 1:1 as anolyte, adding 1.6g/L CH3COONa、0.05g/L NH4Cl, 12.5mL/L trace metal liquid and 5mL/L vitamin liquid as nutrient substances, wherein the trace metal liquid is formed by 6.15g/L MgSO4·7H2O, 0.5g/L MnSO4·H2O, 1g/L NaCl and 0.1g/L FeSO4·7H2O, wherein the vitamin solution comprises 2mg/L of biological acid, 2mg/L of folic acid, 10mg/L of vitamin B6, 5mg/L of riboflavin and the like; taking supernatant of aerobic activated sludge as catholyte, and adding 1.0g/LNaHCO3、0.2g/L NH4Cl, 12.5ml/L trace metal liquid and 5ml/L vitamin liquid are taken as nutrient substances, and the microbial fuel cell is started. The reactor adopts an intermittent operation mode, and the additional rotating speed of the anode area of the MFC is 0 (standing). When the output voltage of the MFC drops sharply, indicating that the concentration of nutrients in the MFC has failed to maintain the normal metabolic activity of the microorganisms, the nutrients are re-added according to the original recipe. After 3 cycles, if the output voltage of the MFC can be kept stable for a long time and the maximum output voltage of each cycle is close, the MFC is considered to be successfully started and the growth of the biological membrane on the electrode material is mature.
(3) Operation of a two-compartment microbial fuel cell
Adding 1.0g/L NaHCO into the cathode chamber3、0.2g/L NH4Cl nutrient substances maintain the growth of microorganisms, the anaerobic sludge substrate of the anode chamber is replaced by oil-based mud, the MFC is operated at room temperature and constant pressure, the additional rotating speed of the anode area of the MFC is 0 (standing), and the anolyte is collected every day to measure the COD concentration of the anolyteAnd recording the output voltage and calculating to obtain the power density.
Example 2
A method for processing shale gas to develop oil-based mud by using a double-chamber microbial fuel cell comprises the following specific steps:
(1) construction of a two-compartment microbial fuel cell
The same procedure as in step (1) of example 1.
(2) Startup of a two-compartment microbial fuel cell
Preparing 1g/L glucose nutrient solution and cultured anaerobic sludge at a ratio of 1:1 as anolyte, adding 1.6g/L CH3COONa，0.05g/L NH4Cl, 12.5mL/L trace metal liquid and 5mL/L vitamin liquid as nutrient substances, wherein the trace metal liquid is formed by 6.15g/L MgSO4·7H2O, 0.5g/L MnSO4·H2O, 1g/L NaCl and 0.1g/L FeSO4·7H2O, wherein the vitamin solution comprises 2mg/L of biological acid, 2mg/L of folic acid, 10mg/L of vitamin B6, 5mg/L of riboflavin and the like; taking supernatant of aerobic activated sludge as catholyte, and adding 1.0g/L NaHCO30.2g/L of NH4And Cl, 12.5ml/L of trace metal liquid and 5ml/L of vitamin liquid are taken as nutrient substances, and the microbial fuel cell is started. The reactor adopts an intermittent operation mode, and the additional rotating speed of the anode area of the MFC is 100 r/min. When the output voltage of the MFC drops sharply, indicating that the concentration of nutrients in the MFC has failed to maintain the normal metabolic activity of the microorganisms, the nutrients are re-added according to the original recipe. After 3 cycles, if the output voltage of the MFC can be kept stable for a long time and the maximum output voltage of each cycle is close, the MFC is considered to be successfully started and the growth of the biological membrane on the electrode material is mature.
(3) Operation of a two-compartment microbial fuel cell
Adding 1.0g/L NaHCO into the cathode chamber3、0.2g/L NH4Cl nutrient substances maintain the growth of microorganisms, the anaerobic sludge substrate of the anode chamber is replaced by oil-based mud, the MFC is operated at room temperature and constant pressure, the additional rotating speed of the anode area of the MFC is 100r/min, the anolyte is collected every day to measure the COD concentration, the output voltage is recorded, andand calculating to obtain the power density.
Example 3
A method for processing shale gas to develop oil-based mud by using a double-chamber microbial fuel cell comprises the following specific steps:
(1) construction of a two-compartment microbial fuel cell
The same as in (1) in example 1.
(2) Startup of a two-compartment microbial fuel cell
Preparing 1g/L glucose nutrient solution and cultured anaerobic sludge at a ratio of 1:1 as anolyte, adding 1.6g/L CH3COONa、0.05g/L NH4Cl, 12.5mL/L trace metal liquid and 5mL/L vitamin liquid as nutrient substances, wherein the trace metal liquid is formed by 6.15g/L MgSO4·7H2O, 0.5g/L MnSO4·H2O, 1g/L NaCl and 0.1g/L FeSO4·7H2O, wherein the vitamin solution comprises 2mg/L of biological acid, 2mg/L of folic acid, 10mg/L of vitamin B6, 5mg/L of riboflavin and the like; taking the supernatant of the aerobic activated sludge as catholyte, and adding 1.0g/L NaHCO3、0.2g/L NH4Cl, 12.5ml/L trace metal liquid and 5ml/L vitamin liquid are taken as nutrient substances, and the microbial fuel cell is started. The reactor adopts an intermittent operation mode, and the additional rotating speed of the anode area of the MFC is 200 r/min. When the output voltage of the MFC drops sharply, indicating that the concentration of nutrients in the MFC has failed to maintain the normal metabolic activity of the microorganisms, the nutrients are re-added according to the original recipe. After 3 cycles, if the output voltage of the MFC can be kept stable for a long time and the maximum output voltage of each cycle is close, the MFC is considered to be successfully started and the growth of the biological membrane on the electrode material is mature.
(3) Operation of a two-compartment microbial fuel cell
Adding 1.0g/LNaHCO into the cathode chamber3，0.2g/LNH4And Cl nutrient substances maintain the growth of microorganisms, the anaerobic sludge substrate of the anode chamber is replaced by oil-based mud, the MFC is operated at room temperature and constant pressure, the additional rotating speed of the anode area of the MFC is 200r/min, the anolyte is collected every day to measure the COD concentration, the output voltage is recorded, and the power density is calculated.
Results of the experiment
Example 2 is a suitable method for processing shale gas to develop oil-based mud using a two-compartment microbial fuel cell.
The MFC system is started and operated under different conditions, the output voltage curve of the MFC system along with the change of time is shown in figure 2, and the output voltage of the battery is the maximum under the condition that the stirring speed is 100r/min, which indicates that the condition is the proper rotating speed of the electricity generating microorganisms of the battery, at the moment, the activity of the electricity generating microorganisms is the strongest, and the reaction of oxidizing and decomposing organic matters is the most violent. Tests show that when the stirring speed is 0, 100r/min and 200r/min, the final removal rates of COD of the anolyte in the MFC system are 44.1 +/-0.2%, 50.4 +/-0.3% and 41.3 +/-0.5% respectively, which indicates that proper stirring can improve the degradation efficiency of COD in the anolyte, probably because the suspended microorganisms in the anolyte can be fully mixed with the anolyte by stirring, and the microorganisms are favorable for decomposing organic matters.
When the stirring rate was increased from 0 to 100r/min, the internal resistance calculated from FIG. 3 decreased from 740. omega. to 601. omega. and FIG. 4 shows that the maximum power density of MFC was increased from 9.13W/m2Increased to 10.08W/m2The results show that the proper stirring speed can accelerate the transfer speed of anode ions, reduce ohmic loss of the anode and reduce activation loss and mass transfer loss.
Claims (3)
1. A method for processing shale gas to develop oil-based mud by using a two-chamber microbial fuel cell is characterized by comprising the following steps:
(1) construction of a two-compartment microbial fuel cell
An H-shaped double-chamber microbial fuel cell device is constructed by selecting organic glass, and an anode chamber is in a sealed state except for a reserved charging opening and a wire hole on an upper cover of the device; the cathode chamber is in a semi-sealed state and supplies dissolved oxygen for catholyte through a blast aeration device; the anode chamber and the cathode chamber are connected through a flange, the middle part is separated by a Nafion 117 proton exchange membrane, the carbon felt and the carbon cloth are respectively used as anode and cathode materials through copper wires and are connected with a 1000 omega load resistor to form an external circuit, and MFC voltage data are collected by a parallel data collector.
(2) Startup of a two-compartment microbial fuel cell
And starting the microbial fuel cell by respectively taking the cultured anaerobic sludge and aerobic sludge as substrates of the anode chamber and the cathode chamber. The reactor adopts an intermittent operation mode, and the additional rotating speed of the anode area of the MFC is 0-200 r/min; after three cycles of operation, the output voltage of the MFC can be kept stable for a long time, the maximum output voltage of each cycle is close, and the starting of the MFC is finished.
(3) Operating a microbial fuel cell based on oil-based mud
Adding certain nutrient substances into the cathode chamber to maintain the growth of microorganisms, replacing the anaerobic sludge substrate of the anode chamber with oil-based mud, operating the MFC at room temperature and constant pressure, collecting anolyte every day to measure the COD concentration of the anolyte at an additional rotating speed of 0-200r/min, and recording the output voltage of the anolyte.
2. The method for processing shale gas to develop oil-based mud by using the dual-chamber microbial fuel cell as claimed in claim 1, wherein in the step 2 and the step 3, a magnetic stirrer is arranged at the bottom of the anode chamber to stir and mix the anolyte.
3. The method for processing shale gas to develop oil-based mud according to claim 1, wherein step 3 can achieve both effective removal of organic pollutants in the mud and recovery of electrical energy.
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