CN110813100A - Composite separation membrane and preparation method thereof - Google Patents
Composite separation membrane and preparation method thereof Download PDFInfo
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- CN110813100A CN110813100A CN201911109219.4A CN201911109219A CN110813100A CN 110813100 A CN110813100 A CN 110813100A CN 201911109219 A CN201911109219 A CN 201911109219A CN 110813100 A CN110813100 A CN 110813100A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/10—Catalysts being present on the surface of the membrane or in the pores
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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Abstract
The invention relates to the technical field of membrane separation, and particularly provides a preparation method of a composite separation membrane, which comprises the following steps: putting the ferromagnetic metal-zinc oxide composite particles into a polymer membrane casting solution to obtain a blended membrane solution; scraping the blended film solution, and adding an external magnetic field to attract the ferromagnetic metal-zinc oxide composite particles to the surface of the blended film solution in the scraping process; then, phase inversion is performed. According to the invention, the ferromagnetic metal-zinc oxide composite particles are reduced on the surface of the blending membrane solution in situ by adding the external magnetic field, so that the flux recovery rate of the composite separation membrane is greatly improved, and the reaction process has the advantages of mild conditions, no energy consumption, high reaction efficiency and obvious popularization advantages.
Description
Technical Field
The invention relates to the technical field of membrane separation, in particular to a composite separation membrane and a preparation method thereof.
Background
The available fresh water resource is continuously atrophied. In addition, water pollution makes the limited water system worse. Pollutants in water body are extremely harmful to human body, and can cause various diseases. The membrane technology is a new technology for cross-discipline practical use, and in recent years, the angle is gradually revealed in the aspect of sewage resource utilization. The membrane separation technology can remove suspended matters, bacteria, toxic metal substances and organic matters in water, thereby greatly improving the water quality. Compared with the traditional separation technology, the membrane technology has the advantages of high efficiency, energy conservation, environmental friendliness, easiness in process control, convenience in operation, easiness in integration with other technologies and the like. Therefore, the membrane method water treatment technology is known as the water treatment technology of the twenty first century. The separation membrane is one of the most ideal methods for treating surface water pollution at present. However, organic matter in water (including polysaccharides, bacteria, etc.) is an important factor in the formation of membrane fouling, which greatly limits the application of membrane technology. Therefore, the film contamination is effectively reduced.
Attracted by membrane technologies, researchers have developed various membrane technologies. Among them, the development of separation membranes having special functionality is currently a hot spot. ZnO is a very good photocatalytic material, and has been widely used in recent years due to its environmental protection property. Research shows that the application of the composite material in the separation membrane is shown to improve the permeability and the antifouling capacity of the membrane. Previous reports also show that the added zinc oxide nanoparticles can provide hydrophilic hydroxyl groups, thereby reducing the adhesion of Bovine Serum Albumin (BSA) to the membrane surface. However, previous studies and other reports have found that ZnO particles agglomerate in the casting solution. In addition, due to density factors, most of the ZnO particles agglomerate inside the film. This not only reduces the antifouling effect of the added ZnO, but also severely hinders the photocatalytic function of the composite film. Based on this, it is an urgent problem to provide a novel composite separation membrane.
Disclosure of Invention
The present invention solves the above-mentioned technical problems in the related art at least to some extent. Therefore, the invention provides the composite separation membrane and the preparation method thereof, which greatly improve the flux recovery rate of the composite separation membrane, have simple operation and low cost, can be recovered and are easy to realize industrial application.
In order to achieve the above object, a first aspect of the present invention provides a method for preparing a composite separation membrane, comprising the steps of:
putting the ferromagnetic metal-zinc oxide composite particles into a polymer membrane casting solution to obtain a blended membrane solution;
scraping the blended film solution, and adding an external magnetic field to attract the ferromagnetic metal-zinc oxide composite particles to the surface of the blended film solution in the scraping process; then, phase inversion is performed.
The second aspect of the present invention provides a composite separation membrane prepared by the above preparation method.
In addition, the preparation method of the composite separation membrane according to the present invention may further have the following additional technical features:
according to one embodiment of the present invention, the method for preparing the ferromagnetic metal-zinc oxide composite particles comprises the steps of:
immersing the ferromagnetic metal particles into a dopamine solution, and sucking out the ferromagnetic metal particles by using a magnet after shaking to obtain dopamine-coated ferromagnetic metal particles; immersing the dopamine coated ferromagnetic metal particles in deionized water containing zinc oxide. The method has strong applicability, can easily realize coating of dopamine, has simple equipment and low cost, and is easy to realize large-scale industrial application.
According to an embodiment of the present invention, the oscillation time is: the shaking temperature is 30-35 ℃ for 20-24 h.
According to one embodiment of the present invention, the ferromagnetic metal particles are selected from nickel particles or iron particles, and the polymer is selected from any one of polyvinylidene fluoride, polysulfone, polyethylene or polypropylene, preferably, the ferromagnetic metal particles are selected from nickel particles, and the polymer is selected from polyvinylidene fluoride.
According to one embodiment of the present invention, the method for preparing the nickel particles comprises the steps of: sequentially pouring nickel sulfate hexahydrate, sodium pyrophosphate decahydrate, ammonia water and dimethylamino borane into deionized water to obtain a dissolved solution; silver nitrate was poured into the dissolution.
According to an embodiment of the present invention, the method for preparing nickel particles further comprises the steps of: fully reacting at 25-30 ℃ for 20-25min to obtain solid nickel precipitate, taking out the solid nickel precipitate, drying and fully grinding.
According to an embodiment of the present invention, the scraping comprises scraping with a 200-: the blended film solution was poured onto the surface of a glass plate, and preferably, a 20 μm doctor blade was used for the film scraping.
According to one embodiment of the invention, the preparation conditions of the blended membrane solution comprise that the temperature is controlled to be 80-85 ℃, and the stirring is carried out for 12-13 h; the adding of the external magnetic field comprises: placing a magnet right above the glass plate, and staying for 30-35s, preferably, the preparation conditions of the blended membrane solution comprise that the temperature is controlled to be 80 ℃, and stirring is carried out for 12 h; the adding of the external magnetic field comprises: a magnet was placed directly above the glass plate and left for 30 seconds.
According to an embodiment of the invention, the flux recovery rate of the composite separation membrane prepared by the preparation method is 83% -100%.
Compared with the prior art, the invention has the following beneficial effects:
the ferromagnetic metal-zinc oxide composite particles are reduced on the surface of the blending membrane solution in situ by adding an external magnetic field, so that the flux recovery rate of the composite separation membrane is greatly improved, and the reaction process has mild conditions, does not need energy consumption, has high reaction efficiency and has obvious popularization advantages. Specifically, after humic acid is filtered for three times, flux recovery rate of 100% is achieved through photocatalytic cleaning; after filtering the sodium alginate for three times, the flux recovery rate of 100 percent is achieved through photocatalytic cleaning; after filtering bovine serum albumin for three times, the flux recovery rate reaches 83% through photocatalytic cleaning; after the yeast is filtered for the third time, the flux recovery rate of 83 percent is achieved through photocatalytic cleaning. And the composite separation membrane is easy to recover, excellent in flux recovery effect, energy-saving, efficient and environment-friendly.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a process diagram of an experimental method for preparing a PVDF-Ni-ZnO composite separation membrane according to the invention;
FIG. 2 is a Scanning Electron Microscope (SEM) image of particles before and after compounding in accordance with the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) image of the surface of the film before and after the present invention is compounded;
FIG. 4 is the flux recovery of the PVDF-Ni-ZnO composite separation membrane of the present invention in four contaminants;
FIG. 5 is a magnetic verification diagram of the PVDF-Ni-ZnO composite separation membrane and zinc oxide particles of the invention.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
It is to be understood that the terminology used herein is for the purpose of describing particular example embodiments only, and is not intended to be limiting. As used herein, the singular forms "a", "an" and "the" may be intended to include the plural forms as well, unless the context clearly indicates otherwise. The terms "comprising," "including," and "having" are inclusive and therefore specify the presence of stated features, elements, and/or components, but do not preclude the presence or addition of one or more other features, elements, components, and/or groups thereof.
In the description of the present invention, unless otherwise explicitly specified or limited, the terms "disposed" and "connected" are to be construed broadly, e.g., as meaning a fixed connection, a detachable connection, or an integral connection; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first", "second", may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
For convenience of description, spatially relative terms, such as "bottom," "front," "upper," "oblique," "lower," "top," "inner," "horizontal," "outer," and the like, may be used herein to describe one element or feature's relationship to another element or feature as illustrated in the figures. This spatially relative relationship is intended to encompass different orientations of the mechanism in use or operation in addition to the orientation depicted in the figures. For example, if the mechanism in the figures is turned over, elements described as "below" or "beneath" other elements or features would then be oriented "above" or "over" the other elements or features. Thus, the example term "below … …" can include both an orientation of above and below.
Example 1
25g of nickel sulfate hexahydrate, 50g of sodium pyrophosphate decahydrate, 45 ml of ammonia water (28%) and 1.5g of dimethylaminoborane are poured into 1 liter of deionized water, then 5 ml of silver nitrate (1.597 g/l) is poured into the dissolved solution, and after full reaction for 20 minutes at 25 ℃, solid precipitate-nickel is obtained, and the precipitate is taken out, dried and fully ground.
And (3) soaking the prepared nickel particles into 2 g/L dopamine solution, controlling the temperature to be 35 ℃, placing the nickel particles into a shaking incubator, shaking for 24 hours, and sucking out the nickel particles by using a magnet to obtain the dopamine-coated nickel particles. The dopamine acts to subsequently adhere zinc oxide (abbreviated as ZnO) particles. The dopamine-coated nickel particles prepared above were immersed in 200 ml of deionized water containing 3 g of zinc oxide, and stirred at normal temperature for 12 hours to obtain zinc oxide-adhered nickel particles. Putting the prepared nickel particles adhered with the zinc oxide into polyvinylidene fluoride (PVDF for short) casting solution, controlling the water bath temperature at 80 ℃, stirring for 12h, pouring the obtained solution onto the surface of glass, placing a magnet right above the glass plate for 30s in the process of scraping the film by a scraper with the diameter of 200 mu m, so that the Ni-ZnO particles are attracted to the surface of the film under the action of a magnetic field, and then putting the film into deionized water for phase conversion. Keeping the reaction for a set time, and finally obtaining the magnetic PVDF-Ni-ZnO composite separation membrane. The specific experimental method is shown in figure 1.
Example 2
In order to examine the morphology change of the particle surface before and after compounding, the film was subjected to SEM test in this example, as shown in fig. 2, wherein a (i) and a (ii) are SEM images of the particles before compounding at different magnifications, and b (i) and b (ii) are SEM images of the Ni-ZnO composite particles at different magnifications, wherein the magnifications of a (i) and b (i) are the same, and the magnifications of a (ii) and b (ii) are the same, and as a result, it was found that the morphology of the Ni-ZnO composite particles was greatly different from that of the original particles, and nickel and ZnO formed a network structure, thus proving the successful compounding of Ni and zinc oxide.
Example 3
In order to examine the morphology change of the membrane surface before and after the recombination, the SEM test of the membrane is carried out in the embodiment, as shown in FIG. 3, a is an SEM picture of the PVDF membrane before the recombination, and b is an SEM picture of the PVDF-Ni-ZnO composite separation membrane. As a result, the surface of the PVDF-Ni-ZnO composite separation membrane is found to have a raised grain structure, and the successful compounding of Ni on the surface of the PVDF membrane is proved.
Example 4
In order to measure the flux recovery rate of the PVDF-Ni-ZnO composite separation membrane in the example of the present invention, as shown in fig. 4, the PVDF-Ni-ZnO composite separation membrane is used in the example to filter four contaminants, such as humic acid (a), sodium alginate (b), bovine serum albumin (c), and yeast solution (d), and the initial pure water flux (the leftmost histogram in the a-d graph), the pure water flux after filtering the contaminants (the middle histogram in the a-d graph), the pure water flux after catalytic cleaning (the rightmost histogram in the a-d graph), and the flux recovery rate (the curve or the straight line graph in the a-d graph) are recorded. The flux recovery rate after filtering humic acid, sodium alginate, bovine serum albumin and yeast solution can reach 100%, 83% and 83%.
Example 5
In order to further examine the magnetic effects of the PVDF-Ni-ZnO composite separation film and the magnetic zinc oxide particles, the magnetic properties of the PVDF-Ni-ZnO composite separation film and the magnetic zinc oxide particles were examined in this example, and the results are shown in fig. 5, which shows that both the PVDF-Ni-ZnO composite separation film and the zinc oxide particles have magnetic properties.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a composite separation membrane is characterized by comprising the following steps:
putting the ferromagnetic metal-zinc oxide composite particles into a polymer membrane casting solution to obtain a blended membrane solution;
scraping the blended film solution, and adding an external magnetic field to attract the ferromagnetic metal-zinc oxide composite particles to the surface of the blended film solution in the scraping process; then, phase inversion is performed.
2. The method of manufacturing according to claim 1, wherein the method of manufacturing the ferromagnetic metal-zinc oxide composite particles comprises the steps of:
immersing the ferromagnetic metal particles into a dopamine solution, and sucking out the ferromagnetic metal particles by using a magnet after shaking to obtain dopamine-coated ferromagnetic metal particles; immersing the dopamine coated ferromagnetic metal particles in deionized water containing zinc oxide.
3. The method according to claim 2, wherein the oscillating time is: the shaking temperature is 30-35 ℃ for 20-24 h.
4. The preparation method according to claim 2, wherein the ferromagnetic metal particles are selected from nickel particles or iron particles, and the polymer is selected from any one of polyvinylidene fluoride, polysulfone, polyethylene or polypropylene, preferably the ferromagnetic metal particles are selected from nickel particles, and the polymer is selected from polyvinylidene fluoride.
5. The method according to claim 4, wherein the method for preparing the nickel particles comprises the steps of:
sequentially pouring nickel sulfate hexahydrate, sodium pyrophosphate decahydrate, ammonia water and dimethylamino borane into deionized water to obtain a dissolved solution; silver nitrate was poured into the dissolution.
6. The method according to claim 5, wherein the nickel particles are prepared by a method comprising the steps of: fully reacting at 25-30 ℃ for 20-25min to obtain solid nickel precipitate, taking out the solid nickel precipitate, drying and fully grinding.
7. The method according to any one of claims 1 to 6, wherein the scraping comprises scraping with a 200-250 μm scraper, and further comprising, before the scraping, the steps of: the blended film solution was poured onto the surface of a glass plate.
8. The preparation method according to claim 7, wherein the preparation conditions of the blended membrane solution comprise controlling the temperature to be 80-85 ℃, and stirring for 12-13 h; the adding of the external magnetic field comprises: and (3) placing a magnet right above the glass plate, and staying for 30-35 s.
9. A composite separation membrane produced by the production method according to any one of claims 1 to 8.
10. The composite separation membrane according to claim 9, wherein the flux recovery of the composite separation membrane is 83% to 100%.
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Cited By (2)
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| CN111468739A (en) * | 2020-03-26 | 2020-07-31 | 浙江师范大学 | Magnetic recyclable Ni-coated Ag core-shell structure composite nanoparticle, preparation method thereof and dye degradation method |
| CN113289506A (en) * | 2021-06-15 | 2021-08-24 | 江南大学 | Asymmetric magnetic oxygen-nitrogen separation membrane and preparation method thereof |
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