CN108298682B - Novel anaerobic membrane electric biological treatment process for low-strength organic wastewater - Google Patents
Novel anaerobic membrane electric biological treatment process for low-strength organic wastewater Download PDFInfo
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/28—Anaerobic digestion processes
- C02F3/2846—Anaerobic digestion processes using upflow anaerobic sludge blanket [UASB] reactors
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- C02F3/005—Combined electrochemical biological processes
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2303/00—Specific treatment goals
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Abstract
A novel anaerobic membrane electric biological treatment process for low-strength organic wastewater comprises the following steps: loading the acidified carbon nano tube on a glass fiber membrane through vacuum filtration to prepare a microfiltration conductive membrane; the upflow anaerobic sludge bed reactor is used as a main anaerobic biological treatment process, and the membrane bioreactor is horizontally arranged between a suspended sludge zone and a three-phase separation zone to form an anaerobic-membrane integrated biological treatment process; introducing a microfiltration conductive film as an electrode to form a novel anaerobic membrane electric biological treatment process. Parameters for regulating and controlling the reaction device comprise hydraulic retention time, temperature, voltage and the like. The invention can achieve the following effects: the conducting film plays the roles of membrane interception and membrane electrode at the same time, the effluent quality is strengthened, the methane yield is improved, the membrane pollution is synchronously relieved in situ, and the service life of the conducting film is prolonged. The treatment process has the advantages of low investment cost, small occupied area, simple operation, obvious improvement effect and the like, and can be applied to treating low-strength organic wastewater such as municipal domestic sewage and the like.
Description
Technical Field
The invention relates to an anaerobic biological treatment process for urban domestic sewage.
Background
The urban domestic sewage is generally treated by aerobic organisms, and the power consumption is high. The anaerobic biological treatment technology represented by the upflow anaerobic sludge bed reactor has the characteristics of strong impact load resistance, low energy consumption, low excess sludge yield, biogas production (the main components are methane and carbon dioxide), convenient operation and the like, and is applied to treating urban domestic sewage by more and more people.
Theoretically, the anaerobic biological treatment technology is more suitable for treating medium and high-strength organic wastewater, and the chemical oxygen demand of the urban domestic sewage is generally 300-500 mg/L and belongs to low-strength organic wastewater. Therefore, in order to enhance the anaerobic biological treatment effect of the low-strength organic wastewater, it is considered to couple a membrane bioreactor thereto to improve the effluent quality and the methane yield. The membrane bioreactor is horizontally arranged between a suspended sludge area and a three-phase separator in an up-flow anaerobic sludge bed reactor to form an anaerobic-membrane integrated biological treatment process, and organic matters in sewage are further intercepted by utilizing the efficient interception and separation effect of a biological membrane.
However, the anaerobic membrane biological treatment process is not widely applied to the treatment of practical low-strength organic wastewater, and the limitation is mainly caused by the membrane pollution problem of a membrane bioreactor. Along with the continuous pumping and treatment of sewage, a large number of microorganisms can be adsorbed on the surface of a separation membrane of the membrane bioreactor, so that the membrane aperture is reduced, the membrane flux is reduced, and the sewage treatment effect is further influenced. The traditional membrane pollution solution is a physical and chemical method, namely, membrane pollution is relieved by means of hydraulic backwashing or chemical reagent adding and the like, but the process investment cost is increased undoubtedly, the treatment process is complicated, and the added chemical reagent can limit the growth of anaerobic microorganisms, so that the treatment effect of organic matters in wastewater is reduced. In addition, the hydraulic retention time of the anaerobic biological treatment of the urban domestic sewage is generally 1-2 d, and the retention time is long, so that the retention time also becomes a factor for limiting the engineering application of the process. Therefore, the realization of in-situ mitigation of membrane pollution of the anaerobic membrane biological treatment process and the standard treatment of the low-strength organic wastewater within a lower hydraulic retention time are the key for solving the problem of limited application of the low-strength organic wastewater anaerobic membrane biological treatment process at present.
Disclosure of Invention
In order to simultaneously realize in-situ release of membrane pollution of the membrane bioreactor and efficient removal of organic matters within a relatively short hydraulic retention time, the invention provides the following technical scheme: an anaerobic membrane electric biological treatment process device for low-strength organic wastewater, which is characterized in that: the upflow anaerobic sludge bed reactor provided with the heat-insulating layer ii is arranged on the base, and the lower part of the upflow anaerobic sludge bed reactor is provided with a water distributor. The granular sludge area and the suspended sludge area are arranged in the inner cavity of the upflow anaerobic sludge blanket reactor from bottom to top. One end of the water inlet pump is inserted into the water inlet tank through a pipe vi, and the other end of the water inlet pump is connected with the lower bottom of the water distributor through a pipe i and a valve i. At least one pair of carbon rod electrodes is arranged in the granular sludge area, and a titanium wire i is connected with the carbon rod electrodes and penetrates through a through hole i on one side of the lower portion of the upflow anaerobic sludge bed reactor and a connecting wire iii of the wiring port iii of the electrochemical workstation to be connected with a connecting point i. The pipe v and the valve v are connected with the lower part of the other side of the granular sludge area. The pressure gauge ii is connected to the upper part of the suspended sludge zone via a valve iv and a pipe iv. The middle part of the upflow anaerobic sludge blanket reactor is provided with a membrane bioreactor. The middle inside the membrane bioreactor is provided with a conductive film, and gaskets are respectively arranged at the upper side and the lower side of the conductive film. The titanium wire ii is connected with the surface of the conductive film and connected with the connection point ii of the wiring port i of the electrochemical workstation through the through hole ii. The upper part of the upflow anaerobic sludge bed reactor provided with the heat-insulating layer i is a three-phase separation zone, and the three-phase separator and the reference electrode are respectively fixed on the upper cover of the upflow anaerobic sludge bed reactor. And the upper port of the three-phase separator is provided with an air collecting port. The upper part of the reference electrode is connected with the titanium wire iii and a connecting wire i of a wiring port i of the electrochemical workstation is connected with the connecting point iii. The pressure gauge i is connected to the lower part of the three-phase separation zone via a valve iii and a pipe iii. One side of the valve ii is connected with a water outlet at the upper part of the three-phase separation zone through a pipe ii, and the other side is discharged into a water outlet pool through a pipe vii.
The anaerobic membrane biological treatment process for low-strength organic wastewater by using the device comprises the following steps:
1) in a fume hood, firstly, slowly adding 10mL of concentrated nitric acid into a 250mL beaker, then slowly adding 30mL of concentrated sulfuric acid along the wall of the beaker, stirring while adding, and preparing 40mL of mixed acid (the volume ratio is 1:3) for standby.
2) Slowly adding 0.5-1.5g of carbon nano tubes with the particle size range of 40-60nm into the mixed acid in the step 1), and stirring while adding until the carbon nano tubes are completely dissolved in the mixed acid; preferably, 1g of carbon nanotubes is weighed and dissolved in the mixed acid.
3) Slowly pouring the completely mixed solution obtained in the step 2) into a 250mL round-bottom flask, sealing the flask with a preservative film, and then placing the flask in a heating sleeve for stirring and heating, wherein the heating time is 20-30 min, and the temperature is controlled at 60-80 ℃; preferably, the experimental conditions of stirring and heating at the constant temperature of 80 ℃ for 30min are selected to realize the complete acidification of the carbon nano tube. After the heating was stopped, the round-bottom flask was taken out and air-cooled.
4) A1000 mL beaker was used and 800mL of deionized water was placed inside. Slowly pouring the mixed solution in the round-bottom flask cooled in the step 3) into the flask while stirring, repeatedly flushing the round-bottom flask with deionized water, and pouring the flushing liquid into a beaker until the volume of the liquid in the beaker is 1000 mL. And sealing the beaker by using a preservative film, and standing for 10-15 hours. Preferably, the mixture is allowed to stand for 15 hours, and the internal mixture is clearly separated into layers.
5) Pouring out supernatant liquor of the mixed solution layered in the step 4), carrying out suction filtration on the residual solution on a 0.45-micron water film by a vacuum filtration method, repeatedly washing the bottom of the beaker by deionized water, and continuing to carry out suction filtration on the washing liquid until no residual black solid is left at the bottom of the beaker.
6) And (3) scraping the carbon nano tube subjected to surface acidification of the water film in the step 5) by using a medicine spoon, placing the carbon nano tube on the surface of a glass flat plate, and drying at 80 ℃. After drying, the mixture was placed in a beaker and stored at room temperature for further use.
7) And (3) taking 0.03-0.06 g of the carbon nano tube dried and reserved in the step 6), adding the carbon nano tube into 100mL of dimethylformamide while stirring, and performing ultrasonic treatment for 2h to completely dissolve the carbon nano tube to prepare the conductive film material preparation solution. And then loading 10-30 mL of preparation solution onto a glass fiber membrane with the diameter of 40mm by a vacuum filtration method. Preferably, in this step, 0.05g of a preparation solution of the carbon nanotube/(100 mL of dimethylformamide solution) for the conductive film material is used, and vacuum loading is performed with 20mL of the preparation solution/film.
8) Placing the film loaded with the preparation solution in the step 7) into a furnace at 250-300 ℃ for high-temperature sintering for 2-2.5 h to prepare the carbon nanotube-glass fiber conductive film with the diameter of 40 mm; preferably, the temperature-programmed condition is set as: the heating rate is 5 ℃/min, the sintering temperature is 300 ℃, and the sintering time is 2 h.
9) The anaerobic biological treatment device is started by adopting the digested sludge taken from the anaerobic sludge fermentation tank, so that the sludge concentration of the granular sludge area reaches 10-20 g/L.
10) Taking the conductive film obtained in the step 8), placing the conductive film in a membrane bioreactor, connecting the surface of the conductive film with the titanium wire ii, and connecting the conductive film to the outside of the device through the through hole ii. A carbon rod made of conductor material is arranged at the lower part of the upflow anaerobic sludge bed reactor, the surface of the carbon rod is connected with a titanium wire i, and the carbon rod is connected to the outside of the device through a through hole i; preferred conditions are: in order to realize good conductive performance, four carbon rods with the diameter of 10mm and the length of 35mm are selected, and all the carbon rods are connected through titanium wires i.
11) The electrochemical workstation is opened, the titanium wire iii connected to the reference electrode and the connection line i are connected to the connection point iii, the titanium wire ii connected to the conductive membrane and the connection line ii are connected to the connection point ii, and the titanium wire i connected to the carbon rod and the connection line iii are connected to the connection point i. Setting the cathode potential to be 0V, changing the anode potential, and controlling the voltage between the two electrodes to be within the range of 0.8-1.2V; preferably, the control voltage is 1.0V.
12) And opening a water inlet pump and a valve i, and allowing the low-strength organic wastewater to sequentially pass through a pipe vi, a pipe i and a water distributor from a water inlet tank and enter a granular sludge area at the lower part of the upflow anaerobic sludge bed reactor. The hydraulic retention time is controlled to be 4-8 h, and the optimal hydraulic retention time is 6 h; the temperature is controlled to be 25-30 ℃, and the optimal temperature is 30 ℃.
13) Opening a valve iv, and impacting the organic wastewater before interception of the conductive film on a pressure gauge ii through a pipe iv to obtain a pressure number before the film; and opening a valve iii, and impacting the pressure gauge 1 by the treated wastewater of the conductive film through a pipe iii to obtain the pressure number after the film. The difference between the two is the transmembrane pressure difference.
14) Organic wastewater which is subjected to certain anaerobic membrane biological treatment before the conductive membrane passes through the conductive membrane layer under the action of hydraulic impact and enters the upper part of the upflow anaerobic sludge blanket reactor, and water and gas separation is completed in the three-phase separation zone. Opening a valve ii, discharging the effluent reaching the standard through a pipe ii, the valve ii and a pipe vii, and storing in an effluent pool; the generated gas is discharged from the device through the three-phase separator and is effectively collected at the gas collection port.
15) Measuring the volume of the liquid in the water outlet tank in the step 14) every 12-15 h. Preferably, the method comprises the following steps: the pool liquid volume was measured every 15 h.
The anaerobic membrane biological treatment process taking low-strength organic wastewater as a target object is characterized in that: an up-flow anaerobic sludge bed reactor is adopted to realize anaerobic biological treatment of low-strength organic wastewater. The coupling membrane bioreactor forms an anaerobic-membrane integrated biological treatment process, utilizes the high-efficiency separation and interception effect of a biological membrane to intercept organic matters in sewage, realizes the concentration of the organic matters at the lower part of an up-flow anaerobic sludge bed reactor, prolongs the contact time of the organic matters and anaerobic microorganisms, and effectively solves the problem that the effluent quality does not reach the standard under the condition of low hydraulic retention time. The carbon nano tube is a novel high-strength carbon fiber material, has the conductivity of a metal material, and is loaded on the surface of a membrane material after being acidified, filtered, dried and dissolved to prepare the conductive microfiltration membrane with good conductivity. Generally, the surface of an electroactive anaerobic microorganism has negative charges, and according to the principle of opposite attraction of charges, an anode potential is applied to the surface of a conductive microfiltration membrane, so that the surface and the interior of the conductive microfiltration membrane can quickly adsorb certain microorganisms to form an anode biofilm. Its advantages are three aspects: firstly, the adsorbed microorganisms can reduce the porosity of the microfiltration membrane, improve the particle size range of the intercepted organic matters, realize the large-range concentration of the organic matters and be beneficial to the efficient treatment of the organic matters with lower hydraulic retention time; secondly, microorganisms adsorbed on the surface and inside of the conductive film can intensively degrade organic matters in the wastewater, so that the organic matter treatment efficiency is improved; and thirdly, the surface of the conductive film adsorbs the electrically active anaerobic microorganisms, so that the conductivity of the conductive film can be optimized, and the coulomb efficiency is improved. Meanwhile, the electrochemical auxiliary effect can also change the characteristics of the conductive film, and the permeability, the separation performance and the pollution resistance of the conductive film are improved. Therefore, the anaerobic membrane biological treatment process of the low-strength organic wastewater can achieve the following effects: the conductive film simultaneously plays roles of film interception and a film electrode: the organic matters in the wastewater are intercepted, the contact time of the organic matters and anaerobic microorganisms is prolonged, and the organic matter treatment efficiency under low hydraulic retention time is improved; the anode biological film is quickly formed, the conductivity of the conductive film is improved, the effluent quality is enhanced, and the methane yield is improved. The electrochemistry assists in alleviating membrane pollution, improving the permeability and the separation performance of the membrane and prolonging the service life of the conductive membrane. The process technology has the advantages of low investment cost, small occupied area, simple operation, obvious improvement effect and the like, and can be applied to treating low-strength organic wastewater such as municipal domestic sewage and the like.
Drawings
FIG. 1 is a schematic diagram of an anaerobic membrane biological treatment process device for low-strength organic wastewater.
FIG. 2 is a schematic diagram of the change of methane yield in the process of anaerobic membrane biological treatment of low-strength organic wastewater when the Hydraulic Retention Time (HRT) is changed.
FIG. 3 is a diagram showing the change of Chemical Oxygen Demand (COD) of effluent when the Hydraulic Retention Time (HRT) is changed in the anaerobic membrane biological treatment process of low-strength organic wastewater.
FIG. 4 is a schematic diagram of the change of the effluent turbidity of the anaerobic membrane biological treatment process of low-strength organic wastewater when the Hydraulic Retention Time (HRT) is changed.
In fig. 1: 1. connection lines i, 2, connection lines ii, 3, electrochemical stations, 4, connection ports i, 5, connection ports ii, 6, connection ports iii, 7, connection lines ii i, 8, tubes i, 9, water inlet pumps, 10, valves i, 11, connection points i, 12, titanium wires i, 13, through holes i, 14, granular sludge zones, 15, suspended sludge zones, 16, gaskets i, 17, connection points ii, 18, titanium wires ii, 19, through holes ii, 20, insulation layers i, 21, three-phase separators, 22, three-phase separation zones, 23, connection points iii, 24, titanium wires iii, 25, Ag/AgCl reference electrodes, 26, membrane lumens, 27, tubes ii, 28, valves ii, 29, pressure gauges i, 31, tubes iii, 32, membrane bioreactors, 33, valves iii, 34, conductive membranes (working electrodes), 35, valves iv, 36, pressure gauges ii, 38, tubes iv, 39, insulation layers ii, 40. carbon rod (counter electrode), 41, pipe v, 42, valve v, 43, water distributor, 44, base, 45, pipe vi, 46, inlet tank, 47, outlet tank, 48, pipe vii.
Detailed Description
The novel anaerobic membrane electric biological treatment process device for the low-strength organic wastewater is characterized in that: the membrane bioreactor 32 is horizontally arranged and connected between the suspended sludge area 15 and the three-phase separation area 22 of the upflow anaerobic sludge blanket reactor, namely the upflow anaerobic sludge blanket reactor is divided into an upper part and a lower part by taking the membrane bioreactor 32 as a boundary. Wherein, the lower part of the membrane bioreactor 32 is mainly a granular sludge zone 14, the low-strength organic wastewater sequentially passes through a pipe vi-45, a water inlet pump 9, a pipe i-8, a valve i-10 and a water distributor 43, enters the lower part of the up-flow anaerobic sludge bed reactor from a water inlet tank 46, and is subjected to anaerobic biological treatment of the low-strength wastewater under the action of anaerobic microorganisms; and the low hydraulic retention time is set, so that organic matters which are not degraded in time in the wastewater return to the lower part of the upflow anaerobic sludge blanket reactor due to the high-efficiency separation and interception effect of the conductive film 34 in the membrane bioreactor 32, the concentration of the organic matters is realized, the contact time of the organic matters and anaerobic microorganisms is prolonged, and the effluent quality is enhanced. The wastewater after reaching the standard enters the upper part of the upflow anaerobic sludge blanket reactor through the conductive film 34, the separation of water and gas is finished in the three-phase separation zone 22, the effluent is stored in the effluent pool 47 through the pipes ii to 27 and the valves ii to 28, and the generated gas is collected at the gas collection port 26. The application mechanism of the anaerobic membrane electric biological treatment process of the low-strength organic wastewater is as follows:
1. the upflow anaerobic sludge bed reactor is adopted to carry out anaerobic biological treatment on the low-strength organic wastewater, and has the characteristics of low energy consumption, low excess sludge yield, biogas (the main components are methane and carbon dioxide), convenient operation and the like. In order to improve the effluent quality and enhance the organic matter treatment effect, a membrane bioreactor is considered to be coupled with the membrane bioreactor to form an anaerobic-membrane integrated biological treatment process. Under the high-efficiency separation and interception action of the microfiltration membrane, organic matters in the wastewater are effectively intercepted and concentrated, and the contact time of the organic matters and anaerobic microorganisms is prolonged, so that the problem that the effluent quality does not reach the standard under the condition of low hydraulic retention time is effectively solved.
2. Generally, the surface of an electroactive anaerobic microorganism has a negative charge. The carbon nano tube is loaded on the surface of the microfiltration membrane to prepare the conductive microfiltration membrane with good conductivity, and according to the principle of opposite attraction of charges, an anode potential is applied on the surface of the conductive membrane, so that certain microorganisms are quickly adsorbed on the surface and inside of the conductive membrane, and an anode biological membrane is formed. Its advantages mainly include three: the adsorbed microorganisms reduce the porosity of the microfiltration membrane, expand the particle size range of the intercepted microorganisms, realize large-range concentration of organic matters and facilitate efficient treatment of the organic matters under the condition of lower hydraulic retention time; microorganisms adsorbed on the surface and inside of the conductive film can intensively degrade organic matters in the wastewater, so that the organic matter treatment efficiency is improved; and thirdly, the conductive performance of the conductive film can be optimized by the electroactive microorganisms adsorbed on the surface of the conductive film, so that the coulomb efficiency is improved. Meanwhile, the electrochemical auxiliary effect can also change the characteristics of the conductive film, and the permeability, the separation performance and the pollution resistance of the conductive film are improved.
3. The electrochemical auxiliary action is performed on the coupling treatment process of the upflow anaerobic sludge bed reactor and the membrane bioreactor, namely the anaerobic membrane biological treatment process, and the coupling treatment process has the advantages of low investment cost, small occupied area, simple operation, obvious improvement effect and the like. The conductive film simultaneously plays roles of film interception and a film electrode: the organic matters in the wastewater are intercepted, the contact time of the organic matters and anaerobic microorganisms is prolonged, and the treatment efficiency of the organic matters under the condition of low hydraulic retention time is improved; the method has the advantages of quickly forming an anode biological film by electrically adsorbing electroactive microorganisms, optimizing self-conductivity, strengthening effluent quality and improving methane yield. Meanwhile, the electrochemical auxiliary effect can also change the characteristics of the conductive film, improve the permeability, the separation performance and the pollution resistance of the conductive film and prolong the service life of the conductive film. Therefore, the anaerobic membrane biological treatment process can simultaneously realize membrane bioreactor membrane pollution in-situ relief and efficient removal of organic matters within a short hydraulic retention time, and effectively removes the application limit of the process in the aspect of treatment of low-strength organic wastewater such as municipal domestic sewage.
The invention is further illustrated by the following figures and examples:
as shown in figure 1, the anaerobic membrane biological treatment process device for the low-strength organic wastewater has the following technical characteristics: the upflow anaerobic sludge blanket reactor provided with the heat-insulating layers ii-39 is arranged on a base 44, and the lower part of the upflow anaerobic sludge blanket reactor is provided with a water distributor 43, a granular sludge zone 14 and a suspended sludge zone 15 which are arranged in the inner cavity of the upflow anaerobic sludge blanket reactor from top to bottom. One end of the water inlet pump 9 is inserted into the water inlet tank 46 through a pipe vi-45, and the other end is connected with the lower bottom of the water distributor 43 through a pipe i-8 and a valve i-10. At least one pair of carbon rod electrodes 40 are arranged in the granular sludge area 14, and titanium wires i-12 are connected with the carbon rod electrodes 40 and penetrate through holes i-13 on one side of the lower part of the upflow anaerobic sludge bed reactor to be connected with connecting wires iii-7 of wiring ports iii-6 of the electrochemical workstation 3 to be connected with connecting points i-11. A pipe v-41 and a valve v-42 are connected with the lower part of the other side of the granular sludge zone 14. The pressure gauge ii-36 is connected to the upper part of the suspended sludge zone 15 via a valve iv-35 and a pipe iv-38. The middle part of the upflow anaerobic sludge blanket reactor is provided with a membrane bioreactor 32. The membrane bioreactor 32 is provided with a conductive membrane 34 in the middle, and gaskets 16 are respectively arranged on the upper side and the lower side of the conductive membrane 34. The titanium wires ii-18 are connected to the surface of the conductive film 34 and connected to the connection points ii-17 through connection lines ii-2 passing through the through holes ii-19 and the connection ports i-4 of the electrochemical workstation 3. The upper part of the upflow anaerobic sludge blanket reactor provided with the heat preservation layers i-20 is a three-phase separation zone 22, and a three-phase separator 21 and a reference electrode 25 are respectively fixed on the upper cover of the upflow anaerobic sludge blanket reactor. An air collecting port 26 is arranged at the upper port of the three-phase separator 21; the upper part of the reference electrode 25 is connected with the titanium wire iii-24 and is connected with a connecting wire i-1 of a wiring port i-5 of the electrochemical workstation 3 to a connecting point iii-23; pressure gauge i-29 is connected to the lower part of three-phase separation zone 22 via valve iii-33 and pipe iii-31. Valves ii-28 are connected to the upper outlet of three-phase separation zone 22 via pipes ii-27 on one side and are discharged to outlet tank 47 via pipes vii-48 on the other side.
The anaerobic membrane biological treatment process for low-strength organic wastewater by using the device comprises the following specific operation procedures:
in a fume hood, firstly, slowly adding 10mL of concentrated nitric acid into a 250mL beaker, then slowly adding 30mL of concentrated sulfuric acid along the wall of the beaker, stirring while adding, and preparing 40mL of mixed acid (the volume ratio is 1:3) for standby.
Slowly adding 0.5-1.5g of carbon nano tubes with the particle size range of 40-60nm into the mixed acid while stirring until the carbon nano tubes are completely dissolved in the mixed acid; preferably, 1g of carbon nanotubes is weighed and dissolved in the mixed acid.
Slowly pouring the completely mixed solution into a 250mL round-bottom flask, sealing the flask with a preservative film, placing the flask in a heating jacket, stirring and heating for 20-30 min, and controlling the temperature at 60-80 ℃; preferably, the experimental conditions of stirring and heating at the constant temperature of 80 ℃ for 30min are selected to realize the complete acidification of the carbon nano tube. After the heating was stopped, the round-bottom flask was taken out and air-cooled.
A1000 mL beaker was used and 800mL of deionized water was placed inside. Slowly pouring the cooled mixed solution in the round-bottom flask into the flask while stirring, repeatedly flushing the round-bottom flask with deionized water, and pouring the flushing liquid into a beaker until the volume of the liquid in the beaker is 1000 mL. And sealing the beaker by using a preservative film, and standing for 10-15 hours. Preferably, the mixture is allowed to stand for 15 hours, and the internal mixture is clearly separated into layers.
And pouring out supernatant of the layered mixed solution after standing, carrying out suction filtration on the residual solution on a 0.45 mu m water film by a vacuum filtration method, repeatedly washing the bottom of the beaker by deionized water, and continuing to carry out suction filtration on the washing liquid until no residual black solid exists at the bottom of the beaker.
Scraping the carbon nano tube with the acidified water film surface after the pumping filtration by using a spoon, placing the carbon nano tube on the surface of a glass flat plate, and drying at 80 ℃. After drying, the mixture was placed in a beaker and stored at room temperature for further use.
And (3) adding 0.03-0.06 g of dried carbon nano tube for later use into 100mL of dimethylformamide, stirring while adding, and performing ultrasonic treatment for 2 hours to completely dissolve the carbon nano tube to prepare the conductive film material preparation solution. And then loading 10-30 mL of preparation solution onto a glass fiber membrane with the diameter of 40mm by a vacuum filtration method. Preferably, in this step, 0.05g of a preparation solution of the carbon nanotube/(100 mL of dimethylformamide solution) for the conductive film material is used, and vacuum loading is performed with 20mL of the preparation solution/film.
Placing the film loaded with the preparation solution into a furnace at 250-300 ℃ for high-temperature sintering for 2-2.5 h, and preparing a carbon nanotube-glass fiber conductive film with the diameter of 40 mm; preferably, the temperature-programmed condition is set as: the heating rate is 5 ℃/min, the sintering temperature is 300 ℃, and the sintering time is 2 h.
The anaerobic biological treatment device is started by adopting the digested sludge taken from the anaerobic sludge fermentation tank, so that the sludge concentration of the granular sludge area reaches 10-20 g/L.
And taking the prepared conductive film 34, placing the conductive film in the membrane bioreactor 32, connecting the surface of the conductive film with the titanium wires ii-18, and connecting the conductive film to the outside of the device through the through holes ii-19. A conductor material carbon rod 40 is arranged at the lower part of the upflow anaerobic sludge blanket reactor, the surface of the conductor material carbon rod is connected with a titanium wire i-12 and is connected to the outside of the device through a through hole i-13; preferred conditions are: in order to realize good conductive performance, four carbon rods 40 with the diameter of 10mm and the length of 35mm are selected, and each carbon rod 40 is connected through a titanium wire i-12.
The electrochemical workstation 3 is opened, the titanium wire iii-24 connected to the reference electrode 25 and the connection line i-1 are connected to the connection point iii-23, the titanium wire ii-18 connected to the conductive film 34 and the connection line ii-2 are connected to the connection point ii-17, and the titanium wire i-12 connected to the carbon rod 40 and the connection line iii-7 are connected to the connection point i-11. Setting the cathode potential to be 0V, changing the anode potential, and controlling the voltage between the two electrodes to be within the range of 0.8-1.2V; preferably, the control voltage is 1.0V.
And opening a water inlet pump 9 and a valve i-10, and allowing the low-strength organic wastewater to enter the granular sludge zone 14 at the lower part of the upflow anaerobic sludge blanket reactor from a water inlet tank 46 through a pipe vi-45, a pipe i-8 and a water distributor 43 in sequence. The hydraulic retention time is controlled to be 4-8 h, and the optimal hydraulic retention time is 6 h; the temperature is controlled to be 25-30 ℃, and the optimal temperature is 30 ℃.
Opening the valve iv-35, and impacting the organic wastewater before interception by the conductive film 34 to a pressure gauge ii-36 through a pipe iv-38 to obtain the pressure number before the film; the valve iii-33 is opened and the treated wastewater passing through the conductive membrane 34 impacts the pressure gauge i-29 via the tube iii-31 to obtain the pressure number after the membrane. The difference between the two is the transmembrane pressure difference.
The organic wastewater treated by a certain anaerobic membrane biological treatment before the conductive membrane 34 passes through the conductive membrane layer under the action of hydraulic impact, enters the upper part of the upflow anaerobic sludge blanket reactor, and is separated from water and gas in the three-phase separation zone 22. Opening valves ii-28, discharging effluent reaching the standard through the devices ii-27, ii-28 and vii-48, and storing in a water outlet pool 47; the generated gas is discharged from the device through the three-phase separator 21 and is effectively collected at the gas collection port 26.
And measuring the volume of the liquid in the water pool 47 every 12-15 h. Preferably, the method comprises the following steps: every 15h, the liquid volume of the sump 47 was measured out.
As shown in fig. 2, the methane yield was always maintained at a higher level in the anaerobic membrane electro-biological treatment process using the low-strength organic wastewater as compared to the conventional anaerobic biological treatment process as the hydraulic retention time was changed. When the hydraulic retention time is 6 hours, the methane yield of the anaerobic membrane biological treatment process is improved most obviously, which is about 4 times of that of the common anaerobic biological treatment process.
As shown in FIG. 3, the concentration of the chemical oxygen demand of the effluent is always maintained at a lower level (less than 35mg/L) in the anaerobic membrane electro-biological treatment process using the low-strength organic wastewater as compared with the conventional anaerobic biological treatment process, as the hydraulic retention time is changed. When the hydraulic retention time is 6 hours, the effluent chemical oxygen demand of the anaerobic membrane biological treatment process has the lowest value, which is about 23 mg/L.
As shown in FIG. 4, the turbidity of the effluent was always maintained at a lower level (below 22NTU) in the anaerobic membrane electro-biological treatment process using the low strength organic wastewater as compared to the conventional anaerobic biological treatment process as the hydraulic retention time was varied. At a hydraulic retention time of 6 hours, the effluent turbidity of the anaerobic membrane biological treatment process has the lowest value, about 15 NTU.
Claims (4)
1. An anaerobic membrane electric biological treatment process device for low-strength organic wastewater, which is characterized in that: the upflow anaerobic sludge blanket reactor provided with the heat-insulating layer ii (39) is arranged on a base (44), the lower part of the upflow anaerobic sludge blanket reactor is provided with a water distributor (43), and the granular sludge zone (14) and the suspended sludge zone (15) are arranged in the inner cavity of the upflow anaerobic sludge blanket reactor from bottom to top; one end of the water inlet pump (9) is inserted into the water inlet pool (46) through a pipe vi (45), and the other end of the water inlet pump is connected with the lower bottom of the water distributor (43) through a pipe i (8) and a valve i (10); at least one pair of carbon rod electrodes (40) is arranged in the granular sludge area (14); a titanium wire i (12) is connected with the carbon rod electrode (40) and penetrates through a through hole i (13) on one side of the lower part of the upflow anaerobic sludge blanket reactor to be connected with a connecting wire iii (7) of a wire connecting port iii (6) of the electrochemical workstation (3) to be connected with a connecting point i (11); a pipe v (41) and a valve v (42) are connected with the lower part of the other side of the granular sludge area (14); pressure gauge ii (36)）Connected to the upper part of the suspended sludge zone (15) via a valve iv (35) and a pipe iv (38); the middle part of the up-flow anaerobic sludge bed reactor is provided with a membrane bioreactor (32); the membrane bioreactor (32)A conductive film (34) is arranged in the middle of the inner part, and gaskets (16) are respectively arranged on the upper side and the lower side of the conductive film (34); a titanium wire ii (18) is connected with the surface of the conductive film (34) and passes through the through hole ii (19) to be connected with a connecting line ii (2) of a wiring port i (4) of the electrochemical workstation (3) to be connected with a connecting point ii (17); the upper part of the upflow anaerobic sludge blanket reactor provided with the heat-insulating layer i (20) is a three-phase separation zone (22),whileThe three-phase separator (21) and the reference electrode (25) are respectively fixed on the upper cover of the upflow anaerobic sludge bed reactor; an air collecting port (26) is arranged at the upper port of the three-phase separator (21); the upper part of the reference electrode (25) is connected with the titanium wire iii (24) and is connected with a connecting line i (1) of a wiring port i (5) of the electrochemical workstation (3) to a connecting point iii (23); the pressure gauge i (29) is connected with the lower part of the three-phase separation zone (22) through a valve iii (33) and a pipe iii (31); valve ii (28) is connected on one side to the water outlet in the upper part of the three-phase separation zone (22) via pipe ii (27) and on the other side to the effluent tank (47) via pipe vii (48).
2. The anaerobic membrane electro-biological treatment process device of low-strength organic wastewater according to claim 1, characterized in that: the carbon rod electrodes (40) are counter electrodes, and the number of the carbon rod electrodes is 2.
3. The anaerobic membrane electro-biological treatment process device of low-strength organic wastewater according to claim 1, characterized in that: the conductive film (34) is a working electrode.
4. An anaerobic membrane electro-biological treatment process for low strength organic wastewater using the apparatus of claim 1, comprising the following steps:
1) in a fume hood, firstly, slowly adding 10mL of concentrated nitric acid into a 250mL beaker, then slowly adding 30mL of concentrated sulfuric acid along the wall of the beaker, stirring while adding, and preparing 40mL of mixed acid for later use;
2) slowly adding 0.5-1.5g of carbon nano tubes with the particle size range of 40-60nm into the mixed acid while stirring until the carbon nano tubes are completely dissolved in the mixed acid;
3) slowly pouring the completely mixed solution into a 250mL round-bottom flask, sealing the flask with a preservative film, placing the flask in a heating jacket, stirring and heating for 20-30 min, and controlling the temperature at 60-80 ℃; after the heating is stopped, taking out the round-bottom flask, and cooling the round-bottom flask by air;
4) adopting a 1000mL beaker, and placing 800mL deionized water in the beaker; slowly pouring the cooled mixed solution in the round-bottom flask into the flask while stirring, repeatedly flushing the round-bottom flask with deionized water, and pouring the flushing liquid into a beaker until the volume of the liquid in the beaker is 1000 mL; sealing the beaker by using a preservative film, and standing for 10-15 h; layering of internal mixed liquor can be obviously observed;
5) pouring out supernatant of the layered mixed solution after standing, carrying out suction filtration on the residual solution on a 0.45-micron water film by a vacuum filtration method, repeatedly washing the bottom of the beaker by deionized water, and continuing to carry out suction filtration on the washing liquid until no residual black solid exists at the bottom of the beaker;
6) scraping the carbon nano tube subjected to surface acidification of the water film after the suction filtration by using a spoon, placing the carbon nano tube on the surface of a glass flat plate, and drying at 80 ℃; after drying, placing the mixture in a beaker, and storing the mixture at room temperature for later use;
7) adding 0.03-0.06 g of dried carbon nano tube for later use into 100mL of dimethylformamide, stirring while adding, and performing ultrasonic treatment for 2h to completely dissolve the carbon nano tube to prepare a conductive film material preparation solution; then loading 10-30 mL of preparation solution onto a glass fiber membrane with the diameter of 40mm by a vacuum filtration method;
8) placing the film loaded with the preparation solution into a furnace at 250-300 ℃ for high-temperature sintering for 2-2.5 h, and preparing a carbon nanotube-glass fiber conductive film with the diameter of 40 mm;
9) starting an up-flow anaerobic sludge bed reactor by adopting digested sludge taken from an anaerobic sludge fermentation tank to enable the sludge concentration of a granular sludge zone (14) to reach 10-20 g/L;
10) taking the prepared conductive film (34) to be placed in a membrane bioreactor (32), connecting the surface of the conductive film with a titanium wire ii (18), and connecting the conductive film to the outside of the device through a through hole ii (19); a carbon rod electrode (40) is arranged at the lower part of the upflow anaerobic sludge blanket reactor, the surface of the carbon rod electrode is connected with a titanium wire i (12), and the carbon rod electrode is connected to the outside of the device through a through hole i (13);
11) opening the electrochemical workstation (3), connecting the titanium wire iii (24) connected with the reference electrode (25) and the connecting line i (1) to the connecting point iii (23), connecting the titanium wire ii (18) connected with the conductive film (34) and the connecting line ii (2) to the connecting point ii (17), and connecting the titanium wire i (12) connected with the carbon rod electrode (40) and the connecting line iii (7) to the connecting point i (11); setting the cathode potential to be 0V, changing the anode potential, and controlling the voltage between the two electrodes to be within the range of 0.8-1.2V;
12) opening a water inlet pump (9) and a valve i (10), and allowing the low-strength organic wastewater to enter a granular sludge area (14) at the lower part of the upflow anaerobic sludge bed reactor from a water inlet tank (46) through a pipe vi (45), a pipe i (8) and a water distributor (43) in sequence; the hydraulic retention time is controlled to be 4-8 h; controlling the temperature to be 25-30 ℃;
13) opening a valve iv (35), impacting the organic wastewater before interception by the conductive film (34) on a pressure gauge ii (36) through a pipe iv (38) to obtain a pressure number before membrane; opening a valve iii (33), and impacting the treated wastewater through the conductive film (34) to a pressure gauge i (29) through a pipe iii (31) to obtain a pressure number after the film; the difference between the two is the transmembrane pressure difference;
14) organic wastewater subjected to certain anaerobic membrane biological treatment before the conductive membrane (34) passes through the conductive membrane layer under the action of hydraulic impact, enters the upper part of the upflow anaerobic sludge blanket reactor, and is separated into water and gas in the three-phase separation zone (22); opening a valve ii (28), discharging the effluent reaching the standard through a pipe ii (27), the valve ii (28) and a pipe vii (48), and storing in an effluent pool (47); the generated gas is discharged from the device through a three-phase separator (21) and is effectively collected at a gas collecting port (26);
15) measuring the volume of the liquid in the water pool (47) every 12-15 h.
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