CN113694742A - Nano-silver antibacterial ultrafiltration membrane and preparation method thereof - Google Patents
Nano-silver antibacterial ultrafiltration membrane and preparation method thereof Download PDFInfo
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- CN113694742A CN113694742A CN202110922385.7A CN202110922385A CN113694742A CN 113694742 A CN113694742 A CN 113694742A CN 202110922385 A CN202110922385 A CN 202110922385A CN 113694742 A CN113694742 A CN 113694742A
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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
- B01D69/10—Supported membranes; Membrane supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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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
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
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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
- B01D2325/24—Mechanical properties, e.g. strength
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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
- B01D2325/38—Hydrophobic 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
- B01D2325/48—Antimicrobial properties
Abstract
The invention provides a nano-silver antibacterial ultrafiltration membrane which is sequentially provided with a porous support membrane, a separation functional layer and an antibacterial coating from bottom to top; the antibacterial coating comprises an adhesive coating and an inorganic nano coating; the nano silver of the ultrafiltration membrane prepared by the method belongs to an inorganic antibacterial agent, and has the broad antibacterial effect of difficult generation of drug resistance, strong heat resistance and longer acting, the high-density cation of the polyethyleneimine coating can endow the ultrafiltration membrane with the retention property on ions, and the polyethyleneimine and silver ions have strong chelation, so that the ultrafiltration membrane cannot easily fall off due to repeated cleaning and long-time friction, the pollution caused by the falling of the silver ions is avoided, and the water treatment membrane also has long-term antibacterial property.
Description
Technical Field
The invention relates to the technical field of sewage treatment filter membranes, in particular to a nano-silver antibacterial ultrafiltration membrane and a preparation method thereof.
Background
In the field of sewage treatment filter membrane technology, the filter membrane water treatment is a solid-liquid separation technology, and is characterized by that it uses membrane pores to filter water and retain impurities in water, and uses said membrane to mainly remove colloid and plankton, remove insoluble iron and manganese and remove fungi. However, the sterilization process cannot be omitted in order to avoid the bacteria from being regenerated in the clean water tank. In the raw water directly connected to the plate-and-frame type and spiral type membranes, suspended matter in the raw water should be removed before flowing into the membranes so that the membrane pores are not closed. The polyamide membrane is made of organic polymer materials, so that bacteria pollution is easily caused by adsorption, growth and reproduction of a large number of microorganisms on the surface of the membrane, and the performance of the membrane is reduced due to the fouling and blocking of the membrane.
The membrane separation technology is adopted to provide necessary operation pressure for raw water supply, the filter membrane is flushed only by running for a long time without other processes, the membrane device is operated to be automated easily under the condition, unmanned management is achieved, and automation is achieved by conventional treatment and is not easy. The micromolecules which are easy to generate drug resistance, easy to bring secondary pollution and easy to decompose into toxic and side effects have poor heat resistance. Therefore, the invention provides the nano-silver antibacterial ultrafiltration membrane and the preparation method thereof, which are used for solving the problems of poor antibacterial effect, easy fouling and low water flux of the ultrafiltration membrane, improving the antibacterial effect on the ultrafiltration membrane and prolonging the service life of the ultrafiltration membrane.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a nano-silver antibacterial ultrafiltration membrane and a preparation method thereof.
In order to realize the aim, the invention provides a preparation method of a nano-silver antibacterial ultrafiltration membrane, which comprises the following steps:
s1 porous support membrane formation, the porous support membrane 20 is prepared as a support, and the porous support membrane 20 is a membrane capable of forming an ultrafiltration separation function layer on its surface, there is no particular limitation, as long as the porous support membrane 20 is an ultrafiltration membrane in which a microporous ultrafiltration separation functional layer having an average pore diameter of 0.001 to 0.4 μm is formed on the porous support layer, and generally a polyester nonwoven fabric, as a material for forming the microporous ultrafiltration separation functional layer, for example, polyaryl ether sulfones such as polysulfone and polyethersulfone, polyimide, polyvinylidene fluoride, etc. can be mentioned, and polysulfone, polyaryl ether sulfone or polyimide can be used from the viewpoint of chemical stability, mechanical stability and thermal stability, in addition, a self-supporting porous support membrane made of a thermosetting resin such as an epoxy resin having the above average pore diameter may also be used. The thickness of the porous support membrane 20 is not particularly limited, and may be, for example, in the range of 10 μm to 200 μm, or in the range of 20 μm to 65 μm;
s2 polymer layer preparation, contacting an aqueous solution containing a polymer with the separation functional layer 30 to form a polymer-containing layer, and then drying the polymer-containing layer; the method of bringing the aqueous solution into contact with the separation functional layer 30 is not particularly limited, and the separation functional layer 30 and the porous support membrane 20 may be immersed in the aqueous solution, or the aqueous solution may be applied to the surface of the separation functional layer 30, and the contact time of the separation functional layer 30 and the aqueous solution is, for example, 10 seconds to 10 minutes, and after the separation functional layer 30 is brought into contact with the aqueous solution, a washing step of removing excess aqueous solution from the separation functional layer 30 may be performed, and the solvent of the aqueous solution may contain a polar solvent other than water, such as alcohol, in addition to water, or may contain a polar solvent other than water, such as alcohol, instead of water;
the polymer is a copolymer consisting of a polymer with quaternary phosphine cations as a first monomer and a polymer with a second monomer, wherein the second monomer can use only one or more selected from 3-chloro-2-hydroxypropyl diallyl amine hydrochloride, allylamine and acrylamide, and the copolymer can be a random copolymer or a block copolymer.
S31 bond coat preparation, bond coat 401 may be formed by: the polymer-containing layer is formed by contacting an aqueous solution containing a polymer with the separation functional layer 30, and then the polymer-containing layer is dried. The method of contacting the aqueous solution with the separation functional layer 30 is not particularly limited. The separation functional layer 30 may be immersed in an aqueous solution together with the porous support membrane 20, or an aqueous solution may be applied to the surface of the separation functional layer 30. The contact time of the separation functional layer 30 with the aqueous solution is, for example, 10 seconds to 10 minutes. After the separation functional layer 30 is brought into contact with the aqueous solution, a cleaning step of removing excess aqueous solution from the separation functional layer 30 may be performed. The solvent of the aqueous solution may contain a polar solvent such as alcohol other than water in addition to water. A polar solvent other than water, such as alcohol, may be used instead of water.
Furthermore, polyethyleneimine is a partially branched polymer comprising primary, secondary and tertiary amines, and can be subjected to a variety of chemical modifications. Polyethyleneimine has three distinct characteristics: the highest cation density in existing materials; very high reactivity; the water solubility is strong. Due to the polar group (amino) and hydrophobic group (vinyl) structure, the material can be combined with different substances. The high cationic property enables the polyethyleneimine to exist in the form of polymeric cations in water, so that heavy metal ions can be chelated. The polyethyleneimine has a high-reactivity amino group in a molecular chain, and can react with epoxy, acid, isocyanate compounds, acidic gases and the like. The load electrochemical treatment on the surface of the water treatment membrane is beneficial to more firmly coating the polyethyleneimine on the surface of the membrane, and the risk of stripping is reduced.
S32 preparation of the inorganic antibacterial layer, wherein the surface of the bonding coating 401 is completely immersed in the antibacterial treating agent for 0.01-60 minutes at the immersion temperature of 20-50 ℃. The antibacterial treatment agent comprises the following components in percentage by mass: 0.01-15 wt% of nano silver ions with the size of 5-50 nm, 0.01-5 wt% of sodium hydroxide and 80-99.98 wt% of diluent, and the components are mixed for 0.5-24 hours under stirring to prepare the nano silver ion water-based paint; the diluent is water or ethanol or a mixture of water and ethanol in any ratio; the nano silver particles are any one of silver nitrate, silver carbonate and silver chloride; next, the polymer-containing layer is heated and dried. By heat-treating the polymer-containing layer, the mechanical strength, heat resistance, and the like of the antibacterial coating layer 402 can be improved. The heating temperature is, for example, 50 ℃ to 80 ℃. The heating time is, for example, 30 seconds to 300 seconds; the inorganic antibiotic layer 402 is formed.
By performing the above steps, the separation membrane 10 having the porous support membrane 20, the separation functional layer 30, and the coating layer 40 can be obtained. The thickness of the coating layer 40 is not particularly limited, and is, for example, 10nm to 2000 nm. The presence of the coating 40 can be confirmed using transmission electron microscopy. The composition analysis of the polymer contained in the coating layer 40 can be performed, for example, by fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), or time-of-flight secondary ion mass spectrometry (TOF-SIMS).
In addition, the invention also provides a nano-silver antibacterial ultrafiltration membrane,
the ultrafiltration membrane 10 is sequentially provided with a porous support membrane 20, an ultrafiltration separation functional layer 30 and an antibacterial coating 40 from bottom to top, wherein the ultrafiltration separation functional layer 30 and the antibacterial coating 40 are supported by the porous support membrane 20, the ultrafiltration separation functional layer 30 is arranged on the porous support membrane 20, the antibacterial coating 40 is arranged on the ultrafiltration separation functional layer 30, the antibacterial coating 40 is in direct contact with the ultrafiltration separation functional layer 30, and the antibacterial coating 40 is divided into an adhesive layer 401 and an inorganic nano coating 402.
The functional ultrafiltration layer 30 is composed of a microporous layer having an average pore diameter of 0.001 to 0.4 μm. The antimicrobial coating 40 may kill and/or inhibit bacterial material on the surface of the separation membrane.
In the present specification, the "average pore diameter" refers to a value calculated by the following method. First, the surface or cross section of the film or layer is observed with an electron microscope (e.g., a scanning electron microscope), and the diameters of a plurality of observed holes (e.g., any 10 holes) are measured. The average of the measured values of the diameters of the pores is defined as "average pore diameter"; the "diameter of the hole" refers to the major diameter of the hole, and more specifically, refers to the diameter of the smallest circle that can surround the hole.
Compared with the prior art, the invention has the following beneficial effects:
1. the nano silver inorganic antibacterial agent has the advantages of difficult generation of drug resistance, strong heat resistance and longer-acting broad-spectrum antibacterial effect.
2. In addition, the quaternary phosphonium salt coating covers the hydrophobic material on the separation surface layer of the original ultrafiltration membrane, so that the hydrophilicity of the surface layer of the antibacterial ultrafiltration membrane is greatly improved, the pollution resistance is better, and the water yield is high.
3. The high density cation of the polyethyleneimine coating can impart ion rejection to the ultrafiltration membrane, particularly for positively charged ionic species.
4. The polyethyleneimine can provide firmer combined action of ionic bonds, hydrogen bonds, van der waals force and the like, has strong chelation between the polyethyleneimine and silver ions, cannot easily fall off due to repeated cleaning and long-time friction, avoids pollution caused by the falling of the silver ions, and also enables the water treatment membrane to have long-term antibacterial property.
Drawings
FIG. 1 is a schematic structural diagram of a nano-silver antibacterial ultrafiltration membrane;
reference numerals: 10-ultrafiltration membrane, 20-porous support membrane, 30-separation functional layer, 40-antibacterial coating, 401-adhesive coating and 402-inorganic antibacterial layer.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to specific embodiments below so that those skilled in the art can fully understand the technical contents of the present invention. It should be noted that the specific embodiments described herein are merely illustrative of the concepts of the invention and are not intended to limit the invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
As shown in fig. 1, a nano-silver antibacterial ultrafiltration membrane, the ultrafiltration membrane 10 is provided with a porous support membrane 20, an ultrafiltration separation functional layer 30 and an antibacterial coating 40 in sequence from bottom to top, wherein the ultrafiltration separation functional layer 30 and the antibacterial coating 40 are supported by the porous support membrane 20, the ultrafiltration separation functional layer 30 is disposed on the porous support membrane 20, the antibacterial coating 40 is disposed on the ultrafiltration separation functional layer 30, the antibacterial coating 40 is in direct contact with the ultrafiltration separation functional layer 30, and the antibacterial coating 40 is divided into an adhesive layer 401 and an inorganic nano-coating 402; the ultrafiltration separation functional layer 30 is composed of a microporous layer having an average pore diameter of 0.001 to 0.4 μm; the antimicrobial coating 40 may kill and/or inhibit bacterial material on the surface of the separation membrane.
The preparation method of the nano-silver antibacterial ultrafiltration membrane of the invention comprises the following steps,
example 1 (sample 1 comparative):
mixing 16 wt% of polysulfone membrane material, 2.0 wt% of PEG20000 and an organic solvent N, N-dimethylacetamide (DMAc), heating to 80 ℃, stirring for 24 hours, cooling to 25 ℃, standing and defoaming for 8 hours to obtain a membrane casting solution A; and coating the casting solution A on a polyester non-woven fabric mechanical support body in a blade mode, and preparing the flat ultrafiltration membrane separation functional layer by using pure water at 35 ℃ as a coagulating bath through a phase inversion method.
Example 2 (sample 2):
placing the sample 1 into 0.5 wt% polyethyleneimine water solution with the weight-average molecular weight of 70000Da for 30 seconds, scraping redundant water solution, washing with pure water for 3 minutes, and immersing in an antibacterial treatment agent at 25 ℃ for 1 minute; the antibacterial treatment agent is prepared by stirring and mixing 1% of silver nitrate nano silver ions with the size of 10-40 nm, 0.5% of sodium hydroxide and 98.5% of water for 24 hours under the assistance of ultrasonic waves. Subsequently, after removing the excess antimicrobial treatment agent, the mixture was heated at 50 ℃ for 5 minutes to dry.
Evaluation of antibacterial property: the evaluation of antibacterial performance is made with reference to test method 100-2004 of the American Association of textile chemical stainers (AATCC). Coli (e.coli) was selected as a representative cell, and the antibacterial performance of the modified membrane was evaluated. Evaluation of film properties: the desalting and permeation performance was tested at 500ppm MgCl2 in water at 25 ℃ and 4bar operating pressure.
Table 1: nano-silver antibacterial ultrafiltration membrane antibacterial performance evaluation table
It should be noted that the above-mentioned preferred embodiments are merely illustrative of the technical concepts and features of the present invention, and are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A preparation method of a nano-silver antibacterial ultrafiltration membrane is characterized by comprising the following steps:
s1 forming a porous supporting membrane, preparing a porous supporting membrane (20) serving as a supporting body, wherein the ultrafiltration membrane on the porous supporting membrane (20) which is provided with a microporous ultrafiltration separation functional layer with the average pore diameter of 0.001-0.4 mu m is a polyester non-woven fabric;
s2 preparation of a polymer layer, wherein an aqueous solution containing a polymer is contacted with a separation functional layer (30) to form a polymer-containing layer, then the polymer-containing layer is dried, the separation functional layer (30) and a porous support membrane (20) are immersed in the aqueous solution, the contact time of the separation functional layer (30) and the aqueous solution is 10 seconds to 10 minutes, and after the separation functional layer (30) is contacted with the aqueous solution, the cleaning of the aqueous solution is removed from the separation functional layer (30);
s3 preparing a bonding coating 401 and preparing an inorganic antibacterial layer 402;
s31 a bonding coat preparation step of forming a polymer-containing layer by bringing an aqueous solution containing a polymer into contact with a separating functional layer (30) and then drying the polymer-containing layer, wherein the contact time of the separating functional layer (30) with the aqueous solution is, for example, 10 seconds to 10 minutes, and after the separating functional layer (30) is brought into contact with the aqueous solution, a cleaning step of removing excess aqueous solution from the separating functional layer (30) to obtain a bonding coat (401);
s32 preparation of an inorganic antibacterial layer, wherein the surface of the bonding coating (401) is completely immersed in an antibacterial treating agent for 0.01-60 minutes at 20-50 ℃, and the polymer-containing layer is heated at 50-80 ℃ for 30-300 seconds; an inorganic antibacterial layer (402) is formed.
2. The method of preparing a nano-silver antibacterial ultrafiltration membrane according to claim 1, wherein the polyfunctional amine in the step S2 is an amine having a plurality of reactive amino groups; the polyfunctional amine is aromatic polyfunctional amine, or aliphatic polyfunctional amine, or alicyclic polyfunctional amine.
3. The method for preparing the nano-silver antibacterial ultrafiltration membrane according to claim 1, wherein the material of the bonding coating (401) in the step S31 is polyethyleneimine, and the molecular weight of the polyethyleneimine is 10000-100000.
4. The method for preparing the nano-silver antibacterial ultrafiltration membrane according to claim 1, wherein the polyethyleneimine of the step S31 is a partially branched polymer containing primary amine, secondary amine and tertiary amine.
5. The preparation method of the nano-silver antibacterial ultrafiltration membrane according to claim 1, wherein the antibacterial treatment agent in the step S32 comprises the following components in percentage by mass: 0.01-15 wt% of nano silver ions with the size of 5-50 nm, 0.01-5 wt% of sodium hydroxide and 80-99.98 wt% of diluent, and the components are mixed for 0.5-24 hours under stirring to prepare the nano silver ion water-based paint.
6. The method for preparing the nano-silver antibacterial ultrafiltration membrane according to claim 5, wherein the diluent is water or ethanol or a mixture of water and ethanol in any ratio.
7. The method for preparing the nano-silver antibacterial ultrafiltration membrane according to claim 5, wherein the nano-silver particles are any one or a mixture of silver nitrate, silver carbonate or silver chloride.
8. The preparation method of the nano-silver antibacterial ultrafiltration membrane according to claim 1, wherein the thickness of the porous support membrane (20) is 10-200 μm.
9. A nano-silver antibacterial ultrafiltration membrane is characterized in that the ultrafiltration membrane (10) prepared by the preparation method according to any one of claims 1 to 8 is provided with a porous support membrane (20), an ultrafiltration separation functional layer (30) and an antibacterial coating (40) in sequence from bottom to top; the antibacterial coating (40) comprises a bonding coating (401) and an inorganic nano coating (402).
10. The nanosilver antimicrobial ultrafiltration membrane of claim 9, wherein said ultrafiltration separation functional layer (30) and antimicrobial coating (40) are supported by said porous support membrane (20); the ultrafiltration separation functional layer (30) is arranged on the porous support membrane (20); the antibacterial coating (40) is arranged on the ultrafiltration separation functional layer (30); the antibacterial coating (40) is in direct contact with the ultrafiltration separation functional layer (30), and the ultrafiltration separation functional layer (30) is composed of a microporous layer with an average pore diameter of 0.001-0.4 mu m.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010808750.7A CN112169602A (en) | 2020-08-12 | 2020-08-12 | Nano-silver antibacterial ultrafiltration membrane and preparation method thereof |
| CN2020108087507 | 2020-08-12 |
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| CN113634135B (en) * | 2021-08-30 | 2022-05-17 | 北京赛诺膜技术有限公司 | Hollow fiber composite nanofiltration membrane and preparation method thereof |
| CN113856497A (en) * | 2021-10-18 | 2021-12-31 | 科盛环保科技股份有限公司 | Nano-silver composite treating agent for improving anti-pollution capability of MBR (membrane bioreactor) membrane and application thereof |
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