CN114653209A - Preparation method and application of magnetic conductive microfiltration membrane - Google Patents
Preparation method and application of magnetic conductive microfiltration membrane Download PDFInfo
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Abstract
The invention relates to a preparation method of a magnetic conductive microfiltration membrane, which comprises the following steps: dissolving polyvinylpyrrolidone and polyvinylidene fluoride in dimethylacetamide, and uniformly stirring to form a mixed solution; adding ammonium persulfate into the mixed solution, adding pyrrole, and stirring uniformly to form a suspension; adding magnetic particles into the suspension, and uniformly stirring to form a membrane casting solution; storing the casting solution to remove bubbles, coating the casting solution on a glass plate, applying an external magnetic field to control the magnetization direction of magnetic particles while coating to obtain a coating with the thickness of 100-300 mu m, standing, and immersing the glass plate with the coating into tap water bath to obtain the magnetic conductive micro-filtration membrane with good filtering performance and stability. The magnetic conductive micro-filtration membrane is used as a filtration membrane and an anode, the sewage treatment effect is good, and the membrane is not easy to be polluted.
Description
Technical Field
The invention relates to the technical field of MBR membrane preparation, in particular to a preparation method and application of a magnetic conductive micro-filtration membrane.
Background
The Microbial Fuel Cell (MFC) can utilize the electroactive microorganisms to oxidize organic matters in the sewage and directly obtain electric energy from the wastewater, and is a clean energy technology and a new sustainable sewage treatment technology. The anode microorganism transfers electrons generated during catabolism of a substrate to the anode in a direct or indirect mode, and the electrons react with hydrogen ions and oxygen near the cathode through an external circuit to generate water, but the wastewater treatment by using the MFC alone is difficult to reach the standard, and the generated electric energy is difficult to be effectively utilized and collected.
Membrane Bioreactor (MBR) is a neotype high-efficient sewage treatment technique that combines together sewage biological treatment and membrane separation, it is effectual to have sewage treatment, area is little, degree of automation is high, mud productivity low grade advantage, nevertheless because granular state or stickness organic matter deposit causes membrane pollution at membrane surface (reversible pollution) or membrane pore (irreversible pollution), influence water quality of water and still can shorten the life of membrane, increase the running cost of MBR, thereby the wide application of membrane bioreactor has been restricted.
At present, the method for slowing down membrane pollution mainly comprises the following steps: a novel membrane material having excellent properties (such as high mechanical strength, good water flux and high surface area) is used; improved process conditions (backwash frequency and solids residence time); optimizing system design (e.g., aeration). However, the above strategies mainly focus on reversible membrane fouling, have little effect on irreversible membrane fouling, and cannot effectively slow down membrane fouling in long-term operation.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method and application of a magnetic conductive microfiltration membrane, aiming at improving the filtration performance of the filtration membrane and reducing membrane pollution.
The technical scheme adopted by the invention is as follows:
in one aspect, the invention provides a preparation method of a magnetic conductive microfiltration membrane, which comprises the following steps:
dissolving polyvinylpyrrolidone and polyvinylidene fluoride in dimethylacetamide, and uniformly stirring to form a mixed solution:
adding ammonium persulfate and pyrrole into the mixed solution, and uniformly stirring to form a suspension;
adding magnetic particles into the suspension, and uniformly stirring to form a membrane casting solution;
storing the casting solution to remove bubbles, coating the casting solution on a glass plate, applying an external magnetic field to control the magnetization direction of the magnetic particles while coating to obtain a coating with the thickness of 100-300 mu m, and standing;
the glass plate with the coating was immersed in a tap water bath, and then the coating was peeled off from the glass plate to obtain a magnetic conductive microfiltration membrane.
The further technical scheme is as follows:
the adding amount of the ammonium persulfate is 10% of the mass of the mixed solution, and the adding amount of the pyrrole is 1% -3% of the mass of the mixed solution.
The addition amount of the magnetic particles is 20-60% of the mass of the pyrrole.
The polyvinylpyrrolidone accounts for 1-10 wt% of the mixed solution, and the polyvinylidene fluoride accounts for 10-20 wt% of the mixed solution.
The magnetic particles are AlNiCo particles, FeCrCo particles, NdFeB particles, Fe-based particles and Fe3O4One or more of particles and Co-based particles.
The external magnetic field is a uniform magnetic field, so that the magnetic particles in the casting solution are magnetized along the same direction.
The external magnetic field direction is vertical to the surface of the glass plate.
On the other hand, the invention provides an application of the magnetic conductive microfiltration membrane prepared by the preparation method of the magnetic conductive microfiltration membrane, which is applied to an MFC-MBR coupling system, and the magnetic conductive microfiltration membrane is used as an MFC anode and an MBR filtration membrane so as to reduce membrane pollution.
The invention has the following beneficial effects:
compared with the traditional PVDF micro-filtration membrane, the magnetic conductive micro-filtration membrane prepared by the preparation method has good filtration performance and stability. The prepared magnetic conductive microfiltration membrane is applied to an MFC-MBR reactor, is used as a filter membrane and an anode, has good sewage treatment effect, and is not easy to be polluted.
The invention has the following specific advantages:
the high-conductivity polypyrrole is used as a conductive material, a conductive path is established in the microfiltration membrane, and the prepared magnetic conductive microfiltration membrane has high conductivity.
The membrane pollution is effectively reduced, on one hand, the dirt on the surface of the membrane is degraded through anode microorganisms, and the reversible pollution is reduced; on the other hand, magnetic particles contained in the magnetic conductive micro-filtration membrane generate a magnetic field parallel to the surface of the membrane on the surface of the membrane and in the membrane pores, and electrons generated by oxidizing organic matters by the anode microorganisms are more distributed to the refractory organic matters on the surface of the reduction membrane and in the membrane pores, so that irreversible pollution is reduced.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a flow chart of the preparation method of the present invention.
FIG. 2 is a schematic view of a casting solution prepared in example 1 of the present invention.
FIG. 3 is a schematic diagram of the operation of preparing a magnetic conductive microfiltration membrane according to embodiment 1 of the invention.
FIG. 4 is an exploded view of a circular membrane module in example 2 of the present invention.
FIG. 5 is a schematic diagram of the electron movement and force applied to the surface (inside the membrane pores) of the magnetic conductive micro-filtration membrane according to the present invention.
In the figure: 1. a beaker; 2. casting membrane liquid; 3. NdFeB particles; 4. a glass rod; 5. a glass plate mold; 6. a permanent magnet; 7. a magnetic conductive microfiltration membrane; 8. a stainless steel sheet frame; 9. a silica gel pad; 10. a stainless steel support frame; 11. holes are reserved.
Detailed Description
The following describes embodiments of the present invention with reference to the drawings.
The application provides a preparation method of a magnetic conductive microfiltration membrane, which comprises the following steps:
dissolving polyvinylpyrrolidone and polyvinylidene fluoride in dimethylacetamide, and uniformly stirring to form a mixed solution;
adding ammonium persulfate into the mixed solution, adding pyrrole, and uniformly stirring to form a suspension;
adding magnetic particles into the suspension, and uniformly stirring to form a membrane casting solution;
storing the casting solution to remove bubbles, coating the casting solution on a glass plate, applying an external magnetic field to control the magnetization direction of the magnetic particles while coating to obtain a coating with the thickness of 100-300 mu m, and standing;
the glass plate with the coating was immersed in a tap water bath to remove residual dimethylacetamide, and then the coating was peeled off from the glass plate to obtain a magnetic conductive microfiltration membrane.
The polyvinylpyrrolidone accounts for 1-10 wt% of the mixed solution, and the polyvinylidene fluoride accounts for 10-20 wt% of the mixed solution. The stirring process of forming the mixed solution is as follows: stirred at room temperature for 6 h.
The adding amount of the ammonium persulfate is 10% of the mass of the mixed solution, and the adding amount of the pyrrole is 1% -3% of the mass of the mixed solution.
The addition amount of the magnetic particles is 20-60% of the mass of the pyrrole.
The magnetic particles have magnetism, and can be AlNiCo particles, FeCrCo particles, NdFeB particles, Fe-based particles and Fe3O4One or more of particles, Co-based particles, and the like.
And standing the casting solution for 1-3h for storage to remove bubbles.
The external magnetic field is a uniform magnetic field, so that the magnetic particles in the casting solution are magnetized along the same direction.
The external magnetic field direction is vertical to the surface of the glass plate.
The application also provides an application of the magnetic conductive microfiltration membrane obtained by the preparation method of the magnetic conductive microfiltration membrane, which is applied to an MFC-MBR coupling system, and the magnetic conductive microfiltration membrane is used as an MFC anode and an MBR filtration membrane to relieve membrane pollution.
The preparation method of the magnetic conductive micro-filtration membrane comprises the steps of mixing a conductive material and a magnetic material into a casting solution, flatly paving the casting solution on a customized glass plate mold, simultaneously controlling the orientation direction of the magnetic material by an external magnetic field, and preparing the magnetic conductive micro-filtration membrane by a phase inversion method.
The prepared magnetic conductive microfiltration membrane is applied to an MFC-MBR coupling system, and is used as an MFC anode and an MBR filtration membrane, so that the sewage treatment effect is good, and the membrane is not easy to pollute.
The magnetic conductive microfiltration membrane can realize continuous high-quality water outlet as an MBR (membrane bioreactor) filter medium, is used as an MFC (micro-fuel cell) anode to construct a bioelectrochemical system to promote the in-situ degradation of organic matters on the surface and in membrane pores, and is embedded with a magnetic material to generate a magnetic field parallel to the membrane surface so as to change the electron motion direction in the anode membrane, reduce refractory organic matters in the membrane pores and effectively inhibit membrane pollution. Compared with the traditional PVDF micro-filtration membrane, the composite membrane has good filtration performance and stability.
Wherein, pyrrole is used as a conductive raw material, ammonium persulfate is used as an oxidant, polypyrrole is formed after the pyrrole is oxidized, and a conductive path can be established in the interior of the microfiltration membrane, so that the organic microfiltration membrane with high conductivity is prepared.
The magnetic particles can generate a magnetic field parallel to the surface of the membrane on the surface of the membrane and in the membrane hole, and electrons generated by oxidizing organic matters by the anode microorganisms are more distributed on the surface of the reduction membrane and the organic matters which are difficult to degrade in the membrane hole in the application process, so that irreversible pollution is reduced, and the membrane pollution is effectively controlled.
The following specific examples further illustrate the preparation method and specific technical scheme of the application of the magnetic conductive microfiltration membrane.
Example 1
Referring to fig. 1, a method for preparing a magnetic conductive microfiltration membrane comprises the following specific steps:
step 1: dissolving 8 wt% of polyvinylpyrrolidone and 15 wt% of polyvinylidene fluoride in 100ml of dimethylacetamide, and stirring for 6 hours at room temperature to obtain a mixed solution in a beaker 1;
step 2: adding 10% ammonium persulfate serving as an oxidant into the mixed solution, adding 2mL of pyrrole into the solution, and stirring for 6 hours;
and step 3: adding the magnetic NdFeB particles 3 into the mixed solution, and stirring for 6 hours to obtain a suspension as casting solution 2, wherein the addition amount of the magnetic particles is 20% of the mass of pyrrole, and the schematic diagram of the prepared casting solution 2 is shown in FIG. 2;
and 4, step 4: the casting solution 2 was stored for 24 hours to remove air bubbles. Subsequently, as shown in FIG. 3, the casting solution 2 was drained onto a custom-made glass plate mold 5 using a glass rod 4 while controlling the orientation direction of the magnetic particles by applying an external magnetic field using a permanent magnet 6 to obtain a coating having a thickness of 300 μm, and left to stand for 3 hours. In fig. 3, B indicates the direction of the applied external magnetic field, which is a uniform magnetic field.
And 5: the glass plate mold 5 with the coating was immersed in a tap water bath for at least 24 hours to remove the residual dimethylacetamide, and the resulting coating was peeled off from the plate to obtain a magnetically conductive microfiltration membrane 7 having good conductivity and filtration properties.
Example 2
Use of a magnetically conductive microfiltration membrane comprising:
as shown in fig. 4, two magnetic conductive microfiltration membranes 7 prepared in example 1 are coated on two sides of a stainless steel support frame 10, a guide plate is left in the stainless steel support frame 10, two waterproof silica gel pads 9 are respectively covered on the membranes, two stainless steel plate frames 8 playing a role in fixing are respectively covered on the two silica gel pads 9, preformed holes 11 are formed in the stainless steel support frame 10, the two waterproof silica gel pads 9 and the two stainless steel plate frames 8, and the stainless steel support frame 10, the two magnetic conductive microfiltration membranes 7, the two silica gel pads 9 and the two stainless steel plate frames 8 are pressed and fixed through the preformed holes 11 by using screws and nuts made of stainless steel, so that a circular membrane module is obtained.
The circular membrane module is arranged in an integrated MFC-MBR reactor, the circular membrane module is used as an MFC anode membrane module, the activated carbon felt is used as an air cathode of the MFC, and the structure of the MFC-MBR reactor further comprises a water inlet peristaltic pump, a water outlet peristaltic pump, an external resistor and an MBR reaction tank (the circular membrane module is also an MBR filter membrane). The external resistance is a constant value resistance or a variable resistor of 10 omega-10000 omega. In the embodiment, a 500 ohm external resistor is selected, and the cathode, the anode and the external resistor are respectively connected through titanium wires.
The volume of the MBR reaction tank is 4.5L, the COD of the inlet water is 500mg/L, the suspended solid content of the mixed liquid is 7566mg/L, and the effective filtration area of the magnetic conductive microfiltration membrane is 52cm2And a water outlet peristaltic pump is used for pumping membrane outlet water and controlling the membrane flux to be 1.5mL/min respectively, and a pressure gauge is connected between the anode membrane component and the water outlet peristaltic pump.
And (3) in the starting stage of the reactor, an external circuit is disconnected, the water outlet peristaltic pump is closed, water overflows, the potential difference between the two electrodes is monitored, when the potential difference reaches more than 400mV, the anode is proved to have the enrichment of electrochemically active microorganisms, the external circuit is connected, a resistor is inserted, and the water outlet peristaltic pump is opened.
During operation, granular or viscous organic matters blocking membrane pores in MBR membrane pollution are utilized by the electrochemical active microorganisms enriched on the magnetic conductive membrane material, and reversible pollution is favorably reduced. Namely, the anode membrane component decomposes dirt on the surface of the membrane through microbial oxidation, mainly complex organic matters such as protein, polysaccharide and the like, and once the decomposition rate is about equal to or higher than the growth rate of the dirt, the dirt is not accumulated or even lightened, so that the MBR can stably run. In the process, part of electrons generated by the electrochemical microorganisms are conducted to the surface of the anode membrane, the electrons are transmitted to the cathode through the titanium wire to generate electric energy, part of the electrons are received by the organic matters which are difficult to degrade, reduction reaction is carried out to break bonds, and the NdFeB particles generate a magnetic field parallel to the surface of the membrane to be beneficial to the electrons to degrade the organic matters on the surface of the membrane (in membrane pores). That is, electrons generated by the oxidation of organic matters by anode microorganisms are transferred to the outside of cells, and after the electrons are transferred to the outside of the cells, two utilization modes are provided, wherein one part is directly conducted to a cathode by an anode to be subjected to the electricity generation of MFC-MBR, and the other part is distributed to reduce the dirt on the surface of an anode membrane and even on a membrane pore.
FIG. 5 is a schematic diagram of the electron movement and stress on the surface (inside the membrane pores) of the magnetic conductive micro-filtration membrane according to this embodiment. Fig. 5 (a) and (b) are schematic diagrams of the movement of electrons on the surface of the membrane (in the membrane pores) and the force exerted by the electrons on the surface of the membrane (in the membrane pores), respectively. The NdFeB particles can generate a magnetic field B parallel to the surface of the membrane on the surface of the membrane and in the membrane holes, electrons moving towards the surface of the membrane are subjected to Lorentz force F parallel to the surface of the membrane, the electrons are promoted to be deflected to the direction parallel to the surface of the membrane, more electrons are distributed to refractory organic matters on the surface of the reduction membrane and in the membrane holes, and therefore irreversible pollution is reduced.
The average COD removal rate of effluent of the MFC-MBR reactor is 85%, the membrane-spanning pressure difference reaches 35kPa, the time is 50 days, and the effective working time is far longer than that of the MBR using the traditional PVDF membrane.
The magnetic conductive microfiltration membrane of the embodiment is applied to an MFC-MBR coupling system, not only plays a role in filtering, but also serves as an MFC anode, and can achieve the effects of good effluent quality, energy consumption reduction and membrane pollution reduction.
Those of ordinary skill in the art will understand that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of a magnetic conductive microfiltration membrane is characterized by comprising the following steps:
dissolving polyvinylpyrrolidone and polyvinylidene fluoride in dimethylacetamide, and uniformly stirring to form a mixed solution;
adding ammonium persulfate and pyrrole into the mixed solution, and uniformly stirring to form a suspension;
adding magnetic particles into the suspension, and uniformly stirring to form a membrane casting solution;
storing the casting solution to remove bubbles, coating the casting solution on a glass plate, applying an external magnetic field to control the magnetization direction of the magnetic particles while coating to obtain a coating with the thickness of 100-300 mu m, and standing;
the glass plate with the coating was immersed in a tap water bath, and then the coating was peeled off from the glass plate to obtain a magnetic conductive microfiltration membrane.
2. The method for preparing a magnetic conductive microfiltration membrane according to claim 1, wherein the addition amount of the ammonium persulfate is 10% by mass of the mixed solution, and the addition amount of the pyrrole is 1% to 3% by mass of the mixed solution.
3. The method for preparing a magnetic conductive microfiltration membrane according to claim 1 wherein the amount of the magnetic particles added is 20-60% of the mass of the pyrrole.
4. The method for preparing a magnetic conductive microfiltration membrane according to claim 1, wherein polyvinylpyrrolidone accounts for 1 wt% -10 wt% of the mixed solution, and polyvinylidene fluoride accounts for 10 wt% -20 wt% of the mixed solution.
5. The method for preparing a magnetic conductive microfiltration membrane according to claim 1 wherein the magnetic particles are AlNiCo particles, FeCrCo particles, NdFeB particles, Fe-based particles, Fe3O4One or more of particles and Co-based particles.
6. The method for preparing a magnetic conductive microfiltration membrane according to claim 1 wherein the external magnetic field is a uniform magnetic field, so that magnetic particles in the membrane casting solution are magnetized in the same direction.
7. The method according to claim 1, wherein the external magnetic field is directed perpendicular to the surface of the glass sheet.
8. Use of the magnetically conductive microfiltration membrane according to claim 1 as an MFC anode and an MBR filtration membrane for reducing membrane fouling in an MFC-MBR coupled system.
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