CN112316754A - Anti-pollution hollow fiber ultrafiltration membrane and preparation method thereof - Google Patents
Anti-pollution hollow fiber ultrafiltration membrane and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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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
- B01D67/0002—Organic membrane manufacture
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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
- B01D69/08—Hollow fibre membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/26—Polyalkenes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
- B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
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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
- B01D2325/36—Hydrophilic 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
- B01D2325/46—Magnetic properties
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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 anti-pollution hollow fiber ultrafiltration membrane is characterized in that the ultrafiltration membrane is prepared by adding magnetic nanoparticles into a membrane casting solution by a blending method and then spinning, wherein the content of the magnetic nanoparticles in the membrane casting solution is 0.1-5% by weight. The invention also discloses a preparation method of the anti-pollution hollow fiber ultrafiltration membrane. By adding the magnetic nanoparticles into the membrane casting solution, the prepared hollow fiber ultrafiltration membrane has magnetism and can swing under the action of a magnetic field, and pollutants can be favorably cleaned from the surface and the hollow interior of the membrane wire.
Description
Technical Field
The invention relates to a water filtering membrane, in particular to an ultrafiltration membrane. The invention also relates to a preparation method of the water filtering membrane.
Background
At present, ultrafiltration is widely applied to industries such as medicine, water treatment, electronic industry, medicine, chemical industry and the like. The hydrophobicity of the membrane main body material enables hydrophobic substances in water to be easily deposited on the surface or in the pores of the polymer membrane, so that membrane pollution is caused. How to improve the anti-pollution performance of the ultrafiltration membrane has become one of the research hotspots. At present, the main method for improving the anti-pollution performance of the ultrafiltration membrane is to improve the hydrophilicity of the membrane or add antibacterial substances such as silver and the like in the membrane preparation process.
The current method for improving the hydrophilicity of the membrane material can only effectively reduce the membrane pollution and can not fundamentally solve the problem of the membrane pollution. The antibacterial substance added in the membrane preparation process has too single function, can only prevent the membrane from being polluted by bacteria, and cannot ensure that the membrane is not polluted by other hydrophobic substances such as protein and the like.
The researchers made many studies:
the Chinese patent with application number 202010320430.7 discloses a strong anti-pollution composite gradient ultrafiltration membrane and a preparation method thereof (application publication number CN111589310A), the ultrafiltration membrane is prepared by chemically bonding graphene oxide surface to magnetic nanoparticles to form a graphene oxide-magnetic nanoparticle hybrid, then uniformly dispersing the graphene oxide-magnetic nanoparticle hybrid, organic fluorosilane and a pore-forming agent in a high-molecular polysulfone PSf solution, adopting a solution casting film-forming method, and carrying out phase conversion by magnetic field assisted non-solvent induction. Can overcome the defects that organic pollutants are easy to adhere to and block membrane pores, the separation efficiency is low, the membrane is not easy to clean, the flux recovery rate is low and the like in the ultrafiltration separation process of the traditional polymer membrane material.
The application number of the Chinese invention patent application with the application number of 201911394496.4 discloses an anti-pollution hollow fiber ultrafiltration membrane and a preparation method thereof (the application publication number is CN111036087A), the ultrafiltration membrane adopts a blending method to add polyether sulfone with photosensitivity and rigidity, hydrophilic group sorbitol and zinc oxide with antibacterial property, photosensitivity and nano-characteristics into polyvinylidene fluoride, and an ultraviolet grafting technology is used for grafting the hydrophilic group and the antibacterial group on a polyvinylidene fluoride-polyether sulfone molecular chain in the processes of dissolving and stirring of a casting membrane liquid and forming of membrane wires. Compared with the common hollow fiber ultrafiltration membrane, the polyvinylidene fluoride hollow fiber ultrafiltration membrane has better hydrophilicity, rigidity and antibacterial property, and the production process is simple and easy for industrial production. Solves the problems of easy pollution, short service life and high membrane cost of the traditional hollow fiber ultrafiltration membrane.
The invention discloses a preparation method of an antibacterial and anti-pollution hollow fiber membrane (application publication No. CN110813103A) in Chinese patent application No. 201911142805.9. According to the preparation method of the antibacterial and anti-pollution hollow fiber membrane, the antibacterial and anti-pollution hollow fiber membrane is obtained by controlling the contents of the polymer resin, the solvent and the nano silver particle/graphene composite material and the technological parameters of wet spinning, the hydrophilicity of the hollow fiber membrane is increased by introducing the nano silver particle/graphene composite material, a hydration layer is formed on the surface of the membrane, the adsorption effect of pollution on the surface of the membrane can be effectively prevented, the anti-pollution performance of the hollow fiber membrane is increased, the protein structure of microorganisms is destroyed by adding the nano silver particles, the microorganisms are killed, and the propagation of bacteria is inhibited.
Disclosure of Invention
The first technical problem to be solved by the present invention is to provide an anti-pollution hollow fiber ultrafiltration membrane in addition to the above technical state.
The second technical problem to be solved by the present invention is to provide a method for preparing an anti-pollution hollow fiber ultrafiltration membrane in view of the above technical situation.
The technical scheme adopted by the invention for solving the first technical problem is as follows: the anti-pollution hollow fiber ultrafiltration membrane is characterized in that the ultrafiltration membrane is prepared by adding magnetic nanoparticles into a membrane casting solution by a blending method and then spinning, wherein the content of the magnetic nanoparticles in the membrane casting solution is 0.1-5% by weight.
Preferably, the magnetic nanoparticles are prepared by inducing silver to deposit on the surfaces of the magnetic particles by adopting seeds.
Preferably, the magnetic nanoparticles can be prepared by the following steps:
firstly, synthesizing polydopamine functional ferroferric oxide nano particles, then synthesizing sodium citrate modified gold nano particles with the particle size of 3-20 nm, adsorbing the gold nano particles on the polydopamine functional ferroferric oxide nano particles to be used as seed crystals to obtain the gold nano modified dopamine functional ferroferric oxide nano particles, and then adding AgNO into the particle solution in batches3And ascorbic acid, and reducing the silver ions to obtain the silver-loaded magnetic nanoparticles.
The AgNO3And the addition amount of ascorbic acid meets the following requirements: AgNO3The mass ratio of the ascorbic acid to the ascorbic acid is 1: 1-5: 1; AgNO3The weight ratio of the added particles is 1/60-1/15 of the particle solution; the weight ratio of the ascorbic acid added is 1/60-1/15 of the particle solution.
Preferably, the main polymer of the ultrafiltration membrane is at least one of polysulfone, polyethersulfone, polyvinylidene fluoride, polyacrylonitrile and polypropylene, and the content of the main polymer in the membrane casting solution is 10-30%.
Preferably, the pore-forming agent in the membrane casting solution for preparing the ultrafiltration membrane is at least one of polyethylene glycol, polyvinylpyrrolidone and diethylene glycol, and the content of the pore-forming agent in the membrane casting solution is 10-40%.
Preferably, the solvent in the casting solution is at least one of dimethylformamide and dimethylacetamide, and the content in the casting solution is 25% to 79.9%.
The technical scheme adopted by the invention for solving the second technical problem is as follows: a preparation method of an anti-pollution hollow fiber membrane is characterized by comprising the following steps:
adding a main polymer, a pore-forming agent and magnetic nanoparticles into a solvent, heating and stirring until the solution is clear and transparent to obtain a membrane casting solution;
extruding the prepared casting solution through a metering pump spinneret, forming a hollow fiber membrane through a coagulating bath, and rolling to obtain the anti-pollution hollow fiber ultrafiltration membrane.
Compared with the prior art, the invention has the advantages that: by adding the magnetic nanoparticles into the membrane casting solution, the prepared hollow fiber ultrafiltration membrane has magnetism and can swing under the action of a magnetic field, so that pollutants can be favorably cleaned from the surface and the hollow interior of the membrane wire; furthermore, the magnetic nanoparticles contain hydrophilic polydopamine, so that the hydrophilicity of the membrane filaments can be improved, and the anti-pollution performance of the membrane filaments is improved; the magnetic nano particles contain silver, so that the antibacterial performance of the membrane wire can be improved, and the anti-pollution performance of the membrane wire is improved.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
(1) taking PDA-Fe3O4(28.35mg/mL)1.06mL is put into a beaker, 60mL of sodium citrate modified gold nano solution (5nm) is added, ultrasonic treatment is carried out for 2min, standing is carried out for 20min, magnetic separation is carried out, after clear liquid is removed, 30mL of water is dispersed and added into a three-neck flask, and stirring is carried out (600 r/min); take 0.5mL AgNO3(37.2mg/mL) of the solution was added to a three-necked flask, and after 30min, 0.5mL of ascorbic acid (19.2mg/mL) was added; adding 0.5ml of LAgNO after 60min3(37.2mg/mL) and 0.5mL ascorbic acid (19.2 mg/mL); repeating the steps for 2 times; the product was magnetically separated, washed 2 times with water, and dispersed in 30mL of water in a reaction flask. Adding 8mL of 4-nitrophenol solution (the concentration is 1mmol/L) and NaBH40.0367g, 1mL of PDA Fe was added3O4The water dispersion of @ Ag is catalyzed at room temperature. At regular intervals, separation was performed with a magnet. Thus preparing PDA Fe3O4@ Ag nanoparticles;
(2) 68 parts of dimethylformamide, 20 parts of polyether sulfone, 10 parts of polyethylene glycol and PDA Fe are prepared according to the weight3O42 parts of @ Ag nano particles are added into a reaction kettle, heated and stirred to prepare an ultrafiltration membrane casting solution;
(3) and (3) extruding the prepared casting solution into a hollow fiber form from a ring-shaped spinneret through a metering pump, then entering a gel tank for split-phase curing and forming, and rolling by a rolling device to obtain the anti-pollution hollow fiber ultrafiltration membrane.
The prepared hollow fiber membrane has the water flux of 240LMH, the effective molecular weight cutoff of 30w, the membrane wire contact angle of 6 degrees and the membrane wire antibacterial property of 98 percent.
Example 2:
(1) taking PDA-Fe3O4(28.35mg/mL)1.06mL is put into a beaker, 60mL of sodium citrate modified gold nano solution (5nm) is added, ultrasonic treatment is carried out for 2min, standing is carried out for 20min, magnetic separation is carried out, after clear liquid is removed, 30mL of water is dispersed and added into a three-neck flask, and stirring is carried out (600 r/min); taking 0.5ml of LAgNO3(37.2mg/mL) of the solution was added to a three-necked flask, and after 30min, 0.5mL of ascorbic acid (19.2mg/mL) was added; adding 0.5ml of LAgNO after 60min3(37.2mg/mL) and 0.5mL ascorbic acid (19.2 mg/mL); repeating the steps for 2 times; the product was magnetically separated, washed 2 times with water, and dispersed in 30mL of water in a reaction flask. Adding 8mL of 4-nitrophenol solution (the concentration is 1mmol/L) and NaBH40.0367g, 1mL of PDA Fe was added3O4The water dispersion of @ Ag is catalyzed at room temperature. At regular intervals, separation was performed with a magnet. Thus preparing PDA Fe3O4@ Ag nanoparticles;
(2) 65 parts of dimethylformamide, 25 parts of polyether sulfone, 9 parts of polyethylene glycol and PDA Fe are prepared according to the weight3O41 part of @ Ag nano particles are added into a reaction kettle, heated and stirred to prepare an ultrafiltration membrane casting solution;
(3) and (3) extruding the prepared casting solution into a hollow fiber form from a ring-shaped spinneret through a metering pump, then entering a gel tank for split-phase curing and forming, and rolling by a rolling device to obtain the anti-pollution hollow fiber ultrafiltration membrane.
The water flux of the prepared hollow fiber membrane is 123LMH, the effective molecular weight cut-off is 15w, the membrane wire contact angle is 11 degrees, and the membrane wire antibacterial property is 94 percent.
Example 3:
(1) taking PDA-Fe3O4(28.35mg/mL)1.06mL in a beaker, 60mL of sodium citrate modified gold nanoparticle solution (5nm) was added, and 2mi ultrasound was performedn, standing for 20min, carrying out magnetic separation, removing clear liquid, dispersing with 30mL of water, adding into a three-neck flask, and stirring (600 r/min); take 0.5mL AgNO3(37.2mg/mL) of the solution was added to a three-necked flask, and after 30min, 0.5mL of ascorbic acid (19.2mg/mL) was added; adding 0.5ml of LAgNO after 60min3(37.2mg/mL) and 0.5mL ascorbic acid (19.2 mg/mL); repeating the steps for 2 times; the product was magnetically separated, washed 2 times with water, and dispersed in 30mL of water in a reaction flask. Adding 240mL of 4-nitrophenol solution (the concentration is 1mmol/L) and NaBH41g, and carrying out catalytic reaction at room temperature. At regular intervals, separation was performed with a magnet. Thus preparing PDA Fe3O4@ Ag nanoparticles;
(2) 60 portions of dimethylformamide, 25 portions of polyethersulfone, 14.5 portions of diglycol and PDA Fe are prepared according to the weight portion3O40.5 part of @ Ag nano particles are added into a reaction kettle, heated and stirred to prepare an ultrafiltration membrane casting solution;
(3) and (3) extruding the prepared casting solution into a hollow fiber form from a ring-shaped spinneret through a metering pump, then entering a gel tank for split-phase curing and forming, and rolling by a rolling device to obtain the anti-pollution hollow fiber ultrafiltration membrane.
The prepared hollow fiber membrane has the water flux of 112LMH, the effective molecular weight cutoff of 10w, the membrane wire contact angle of 18 degrees and the membrane wire antibacterial property of 92 percent.
Claims (17)
1. The anti-pollution hollow fiber ultrafiltration membrane is characterized in that the ultrafiltration membrane is prepared by adding magnetic nanoparticles into a membrane casting solution by a blending method and then spinning, wherein the content of the magnetic nanoparticles in the membrane casting solution is 0.1-5% by weight.
2. The anti-fouling hollow fiber ultrafiltration membrane of claim 1, wherein the magnetic nanoparticles are prepared by seed-induced silver deposition on the surface of the magnetic particles.
3. The anti-fouling hollow fiber ultrafiltration membrane of claim 2, wherein said magnetic nanoparticles are prepared by:
firstly, synthesizing polydopamine functional ferroferric oxide nano particles, then synthesizing sodium citrate modified gold nano particles with the particle size of 3-20 nm, adsorbing the gold nano particles on the polydopamine functional ferroferric oxide nano particles to be used as seed crystals to obtain the gold nano modified dopamine functional ferroferric oxide nano particles, and then adding AgNO into the particle solution in batches3And ascorbic acid, and reducing the silver ions to obtain the silver-loaded magnetic nanoparticles.
4. The anti-fouling hollow fiber ultrafiltration membrane of claim 3, wherein the AgNO is3And the addition amount of ascorbic acid meets the following requirements:
AgNO3the mass ratio of the ascorbic acid to the ascorbic acid is 1: 1-5: 1; AgNO3The weight ratio of the added particles is 1/60-1/15 of the particle solution; the weight ratio of the ascorbic acid added is 1/60-1/15 of the particle solution.
5. The anti-pollution hollow fiber ultrafiltration membrane according to claim 1, wherein the main polymer of the ultrafiltration membrane is at least one of polysulfone, polyethersulfone, polyvinylidene fluoride, polyacrylonitrile and polypropylene, and the content of the main polymer in the membrane casting solution is 10-30%.
6. The anti-pollution hollow fiber ultrafiltration membrane of claim 1, wherein the pore-forming agent in the membrane casting solution for preparing the ultrafiltration membrane is at least one of polyethylene glycol, polyvinylpyrrolidone and diethylene glycol, and the content of the pore-forming agent in the membrane casting solution is 10-40%.
7. The anti-pollution hollow fiber ultrafiltration membrane according to claim 1, wherein the solvent in the membrane casting solution is at least one of dimethylformamide and dimethylacetamide, and the content of the solvent in the membrane casting solution is 25-79.9%.
8. A preparation method of an anti-pollution hollow fiber membrane is characterized by comprising the following steps:
adding a main polymer, a pore-forming agent and magnetic nanoparticles into a solvent, heating and stirring until the solution is clear and transparent to obtain a membrane casting solution;
extruding the prepared casting solution through a metering pump spinneret, forming a hollow fiber membrane through a coagulating bath, and rolling to obtain the anti-pollution hollow fiber ultrafiltration membrane.
9. The process according to claim 8, wherein the heating temperature in the step (i) is 40 to 90 ℃.
10. The process according to claim 7, wherein the stirring time in the step (i) is 2 to 24 hours.
11. The method according to claim 8, wherein the coagulation bath in the step (II) is water.
12. The method according to claim 8, wherein the magnetic nanoparticles are prepared by seed-induced silver deposition on the surface of the magnetic particles.
13. The method of claim 9, wherein the magnetic nanoparticles are prepared by the steps of:
firstly, synthesizing polydopamine functional ferroferric oxide nano particles, then synthesizing sodium citrate modified gold nano particles with the particle size of 3-20 nm, adsorbing the gold nano particles on the polydopamine functional ferroferric oxide nano particles to be used as seed crystals to obtain the gold nano modified dopamine functional ferroferric oxide nano particles, and then adding AgNO into the particle solution in batches3And ascorbic acid, and reducing the silver ions to obtain the silver-loaded magnetic nanoparticles.
14. The anti-fouling hollow fiber ultrafiltration membrane of claim 13, wherein the AgNO is3And the addition amount of ascorbic acid meets the following requirements:
AgNO3the mass ratio of the ascorbic acid to the ascorbic acid is 1: 1-5: 1; AgNO3The weight ratio of the added particles is 1/60-1/15 of the particle solution; the weight ratio of the ascorbic acid added is 1/60-1/15 of the particle solution.
15. The preparation method according to claim 8, characterized in that the main polymer of the ultrafiltration membrane is at least one of polysulfone, polyethersulfone, polyvinylidene fluoride, polyacrylonitrile and polypropylene, and the content of the main polymer in the membrane casting solution is 10-30%.
16. The preparation method according to claim 8, characterized in that the pore-forming agent in the membrane casting solution for preparing the ultrafiltration membrane is at least one of polyethylene glycol, polyvinylpyrrolidone and diethylene glycol, and the content in the membrane casting solution is 10% -40%.
17. The production method according to claim 8, characterized in that the solvent in the casting solution is at least one of dimethylformamide and dimethylacetamide, and the content in the casting solution is 25% to 79.9%.
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Cited By (1)
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| CN115487686A (en) * | 2022-09-01 | 2022-12-20 | 成都博睿兴材科技有限公司 | Multifunctional electrospun fiber composite membrane and preparation method and application thereof |
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