CN101003005A - Method for preparing ultrafiltration film of poly-ether-sulfone and anti-protein-contamination type - Google Patents
Method for preparing ultrafiltration film of poly-ether-sulfone and anti-protein-contamination type Download PDFInfo
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Abstract
A process for preparing the ultrafiltering polyethersulfone membrane resisting against protein pollution includes such steps as preparing PVC solution and borax solution, washing the raw ultrafiltering polyethersulfone membrane, drying in the air, immersing in the PVC solution, washing, drying, immersing in the borax solution, washing, drying, and repeating the last 6 steps several times.
Description
Technical field
The present invention relates to a kind of preparation method of ultrafiltration film of poly-ether-sulfone and anti-protein-contamination type.Belong to the milipore filter technology of preparing.
Background technology
Ultrafiltration is the liquid phase sieve aperture separation process of carrying out under the effect of differential static pressure motive force, according to the molecular weight difference of separated material it is separated, and screening process is relevant with the membrane aperture size.The molecular cut off of ultrafiltration is about 500～500000, field such as be applied to the purification, separation of macromolecular substances usually and concentrate.Ultra-filtration process has the following advantages: (1) does not have to transform between phase, can separate under normal temperature and low pressure, thereby energy consumption is lower; (2) equipment volume is little, and is simple in structure, and investment cost is low; (3) the film separation process is simple pressurized delivered fluid, and technological process is simple, the easy operating management; (4) variation of matter does not take place in material in the concentrating and separating process, is suitable for protecting the processing of flavor and heat-sensitive substance; (5) be fit to concentrating of the valuable macromolecular recovery of trace and low concentration macromolecular substances in the weak solution; (6) can be with the material classification fractionation of different relative molecular masses; (7) film is the uniform non-individual body of being made by high molecular polymer, does not in use have any impurity and comes off, and has guaranteed the pure of filtrate.Owing to have above-mentioned advantage, hyperfiltration technique has broad application prospects in the industrial separation process.
The main reason of restriction hyperfiltration technique extensive use is that film pollutes.The factor that influences the film pollution has a lot, comprises membrane material, operating condition, feed liquid character or the like.Wherein film is a main cause to the absorption of solute molecule.At present mostly the milipore filter of commercial Application is by the hydrophobic material preparation, and in fields such as biological products separations, oily waste water processing, the big molecule in the system for handling easily adsorbs in that hydrophobic film is surperficial, influences the separating property of milipore filter.Studies show that the hydrophily that increases the film surface, can increase its repulsive force, reduce the suction-operated of solute molecule, thereby improve the anti-protein-contamination performance of milipore filter on the film surface to solute molecule.
Polyether sulfone is a kind of common membrane material, has advantages such as mechanical strength height, physics and chemical stability are good, film forming characteristics is good, cheap and easy to get, therefore is used widely.But the polyether sulfone hydrophobicity is stronger, causes a large amount of absorption on the film surface of protein or oil droplet molecule easily, causes serious film to pollute, and separative efficiency descends.There is several different methods to be applied to the poly (ether-sulfone) ultrafiltration membrane surface modification in the document,, strengthens its contamination resistance to improve the hydrophily on film surface.Method commonly used such as chemical graft, uv photo initiated grafting, low temperature plasma grafting etc.Most method of modifying complicated operations, the condition harshness, and modified effect is difficult to control, thereby the exploitation of new modification technology is significant; Have modifier now based on hydrophilic chain polymer, as polyethylene glycol, phospholipid.Polyvinyl alcohol has strongly hydrophilic, studies show that it has good anti-protein and oils absorption property, and the hydrophily that is used for pore-free surface is at present improved more, there are some researches show that also polyvinyl alcohol has huge development potentiality in the porous surface modification.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of ultrafiltration film of poly-ether-sulfone and anti-protein-contamination type, this procedure is simple, and the milipore filter with the method preparation has stronger contamination resistance to protein and oils molecule.
The present invention is achieved through the following technical solutions.A kind of preparation method of ultrafiltration film of poly-ether-sulfone and anti-protein-contamination type is characterized in that may further comprise the steps:
(1) polyether sulfone is after under 110 ℃～150 ℃ dry 12 hours, be dissolved in 60 ℃ of N, in the dinethylformamide, be mixed with mass concentration and be 16～18% solution, add mass concentration and be 10～15%, molecular weight be 2000 polyethylene glycol as pore-foaming agent, mix promptly being mixed with casting solution a after stirring fully;
(2) with the prepared casting solution a of step (1) 50～70 ℃ of following standing and defoaming 2～4 hours, after being cooled to room temperature casting solution is poured on knifing on the glass plate, after in air, placing 10～30 seconds, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, obtain blank poly (ether-sulfone) ultrafiltration membrane b;
(3) polyvinyl alcohol is added in the deionized water, 90 ℃ of following stirring and dissolving are mixed with mass concentration and are 0.1～2.0% poly-vinyl alcohol solution c;
(4) be that 0.001% NaOH is dissolved in the deionized water with borax and mass concentration, be mixed with mass concentration and be 0.5～1.0% borax soln d;
(5) with the blank film b deionized water clean surface of step (2) gained, dry surface moisture, put into the solution c of step (3) gained, soaked 10 minutes;
(6) film is taken out from solution c, use the deionized water clean surface, dry moisture, put into the solution d of step (4) gained, soaked 10 minutes;
(7) set by step the process repetitive operation of (5) and (6) is 3～6 times, obtains modified poly (ether-sulfone) anti-protein-contamination milipore filter.
The invention has the advantages that: the preparation method of antipollution milipore filter is easy, mild condition, by borax to polyvinyl alcohol crosslinked reaction, can controlling diaphragm the adsorbance of surface polyvinyl alcohol, improve the stability of polyvinyl alcohol modification film simultaneously, by the Modified Membrane that this method obtains, surface hydrophilicity improves significantly, improve the ability of anti-protein and oils molecular contamination, had stability preferably simultaneously.
The specific embodiment
Embodiment one
The preparation of modified poly (ether-sulfone) anti-protein-contamination milipore filter (film 1)
Take by weighing 7.2 gram polyether sulfones and 26.8 gram N, dinethylformamide is put into there-necked flask, and the heating stir about is 0.5 hour in 60 ℃ water bath with thermostatic control.Polyether sulfone is all after the dissolving, take by weighing 6.0 gram-molecular weights and be 2000 polyethylene glycol and add in the solution as pore-foaming agent, 60 ℃ down the heating stirring and dissolving obtain casting solution a after mixing about 4 hours, 60 ℃ of following standing and defoaming 2 hours.After being cooled to room temperature casting solution a is poured on knifing on the glass plate, in air, place 10～30 seconds after, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, obtain blank poly (ether-sulfone) ultrafiltration membrane b;
Take by weighing 1.0 gram polyvinyl alcohol, add in the 199.0 gram deionized waters, adding thermal agitation under 90 ℃, to be mixed with mass concentration be 0.5% poly-vinyl alcohol solution c; Take by weighing 5 gram boraxs, 10 milligrams of NaOH is dissolved in that to be mixed with 1000 gram mass concentration in the deionized water be 0.5% borax soln d;
With blank film b deionized water clean surface, dry surface moisture, put into solution c and soaked 10 minutes; Then film is taken out from solution c, use the deionized water clean surface, dry moisture, put into solution d, soaked 10 minutes; Be dipped into successively among solution c and the solution d after again film being cleaned subsequently and repeat said process, finish 3 circulations, obtain modified poly (ether-sulfone) ultrafiltration membrane capable (film 1).
Reaction as shown in Equation 1 takes place in above-mentioned milipore filter preparation process, the carrying out that promotes preparation process:
Formula 1
Prepared modified poly (ether-sulfone) anti-protein-contamination milipore filter is through ESEM, contact angle and x-ray photoelectron spectroscopy analysis, find that this film has typical milipore filter composite construction, fenestra is evenly distributed, narrow pore size distribution range, the film surface hydrophilicity strengthens, and has the polyvinyl alcohol molecule to exist.The film pure water flux reaches 108.8L/ (m
2H), separating 1g/L bovine serum albumin(BSA) cushioning liquid, is 100% to the bovine serum albumin(BSA) rejection, and after waterpower was cleaned, this film had the higher flux recovery rate, and flux still is in higher level after long-term ultrafiltration.
Embodiment two
The preparation of modified poly (ether-sulfone) anti-protein-contamination milipore filter (film 2)
Take by weighing 7.2 gram polyether sulfones and 26.8 gram N, dinethylformamide is put into there-necked flask, and the heating stir about is 0.5 hour in 60 ℃ water bath with thermostatic control.Polyether sulfone is all after the dissolving, take by weighing 6.0 gram-molecular weights and be 2000 polyethylene glycol and add in the solution as pore-foaming agent, 60 ℃ down the heating stirring and dissolving obtain casting solution a after mixing about 4 hours, 60 ℃ of following standing and defoaming 2 hours.After being cooled to room temperature casting solution a is poured on knifing on the glass plate, in air, place 10～30 seconds after, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, obtain blank poly (ether-sulfone) ultrafiltration membrane b;
Take by weighing 2.0 gram polyvinyl alcohol, add in the 198.0 gram deionized waters, adding thermal agitation under 90 ℃, to be mixed with mass concentration be 1.0% poly-vinyl alcohol solution c; Take by weighing 5 gram boraxs, 10 milligrams of NaOH is dissolved in that to be mixed with 1000 gram mass concentration in the deionized water be 0.5% borax soln d;
With blank film b deionized water clean surface, dry surface moisture, put into solution c and soaked 10 minutes; Then film is taken out from solution c, use the deionized water clean surface, dry moisture, put into solution d, soaked 10 minutes; Be dipped into successively among solution c and the solution d after again film being cleaned subsequently and repeat said process, finish 3 circulations, obtain modified poly (ether-sulfone) ultrafiltration membrane capable (film 2).
Prepared modified poly (ether-sulfone) anti-protein-contamination milipore filter is through ESEM, contact angle and x-ray photoelectron spectroscopy analysis, find that this film has typical milipore filter composite construction, fenestra is evenly distributed, narrow pore size distribution range, the film surface hydrophilicity strengthens, and has the polyvinyl alcohol molecule to exist.The film pure water flux reaches 128.7L/ (m
2H), separating 1g/L bovine serum albumin(BSA) cushioning liquid, is 100% to the bovine serum albumin(BSA) rejection, and after waterpower was cleaned, this film had the higher flux recovery rate, and flux still is in higher level after long-term ultrafiltration; The oil-water emulsion that separates the configuration of 900ppm edible oil is 100% to the rejection of oil, the more blank poly (ether sulfone) film height of flux recovery rate.
Embodiment three
The preparation of modified poly (ether-sulfone) anti-protein-contamination milipore filter (film 3)
Take by weighing 7.2 gram polyether sulfones and 26.8 gram N, dinethylformamide is put into there-necked flask, and the heating stir about is 0.5 hour in 60 ℃ water bath with thermostatic control.Polyether sulfone is all after the dissolving, take by weighing 6.0 gram-molecular weights and be 2000 polyethylene glycol and add in the solution as pore-foaming agent, 60 ℃ down the heating stirring and dissolving obtain casting solution a after mixing about 4 hours, 60 ℃ of following standing and defoaming 2 hours.After being cooled to room temperature casting solution a is poured on knifing on the glass plate, in air, place 10～30 seconds after, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, obtain blank poly (ether-sulfone) ultrafiltration membrane b;
Take by weighing 4.0 gram polyvinyl alcohol, add in the 196.0 gram deionized waters, adding thermal agitation under 90 ℃, to be mixed with mass concentration be 2.0% poly-vinyl alcohol solution c; Take by weighing 5 gram boraxs, 10 milligrams of NaOH is dissolved in that to be mixed with 1000 gram mass concentration in the deionized water be 0.5% borax soln d;
With blank film b deionized water clean surface, dry surface moisture, put into solution c and soaked 10 minutes; Then film is taken out from solution c, use the deionized water clean surface, dry moisture, put into solution d, soaked 10 minutes; Be dipped into successively among solution c and the solution d after again film being cleaned subsequently and repeat said process, finish 3 circulations, obtain modified poly (ether-sulfone) ultrafiltration membrane capable (film 3).
Prepared modified poly (ether-sulfone) anti-protein-contamination milipore filter is through ESEM, contact angle and x-ray photoelectron spectroscopy analysis, find that this film has typical milipore filter composite construction, fenestra is evenly distributed, narrow pore size distribution range, the film surface hydrophilicity strengthens, and has the polyvinyl alcohol molecule to exist.The film pure water flux reaches 113.0L/ (m
2H), separating 1g/L bovine serum albumin(BSA) cushioning liquid, is 100% to the bovine serum albumin(BSA) rejection, and after waterpower was cleaned, this film had the higher flux recovery rate, and flux still is in higher level after long-term ultrafiltration; The oil-water emulsion that separates the preparation of 900ppm edible oil is 100% to the rejection of oil, the more blank poly (ether sulfone) film height of flux recovery rate.
Embodiment four
The preparation of modified poly (ether-sulfone) anti-protein-contamination milipore filter (film 4)
Take by weighing 7.2 gram polyether sulfones and 26.8 gram N, dinethylformamide is put into there-necked flask, and the heating stir about is 0.5 hour in 60 ℃ water bath with thermostatic control.Polyether sulfone is all after the dissolving, take by weighing 6.0 gram-molecular weights and be 2000 polyethylene glycol and add in the solution as pore-foaming agent, 60 ℃ down the heating stirring and dissolving obtain casting solution a after mixing about 4 hours, 60 ℃ of following standing and defoaming 2 hours.After being cooled to room temperature casting solution a is poured on knifing on the glass plate, in air, place 10～30 seconds after, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, obtain blank poly (ether-sulfone) ultrafiltration membrane b;
Take by weighing 1.0 gram polyvinyl alcohol, add in the 199.0 gram deionized waters, adding thermal agitation under 90 ℃, to be mixed with mass concentration be 0.5% poly-vinyl alcohol solution c; Take by weighing 5 gram boraxs, 10 milligrams of NaOH is dissolved in that to be mixed with 1000 gram mass concentration in the deionized water be 0.5% borax soln d;
With blank film b deionized water clean surface, dry surface moisture, put into solution c and soaked 10 minutes; Then film is taken out from solution c, use the deionized water clean surface, dry moisture, put into solution d, soaked 10 minutes; Be dipped into successively among solution c and the solution d after again film being cleaned subsequently and repeat said process, finish 6 circulations, obtain modified poly (ether-sulfone) ultrafiltration membrane capable (film 4).
Prepared modified poly (ether-sulfone) anti-protein-contamination milipore filter is through ESEM, contact angle and x-ray photoelectron spectroscopy analysis, find that this film has typical milipore filter composite construction, fenestra is evenly distributed, narrow pore size distribution range, the film surface hydrophilicity strengthens, and has the polyvinyl alcohol molecule to exist.The film pure water flux reaches 84.0L/ (m
2H), separating 1g/L bovine serum albumin(BSA) cushioning liquid, is 100% to the bovine serum albumin(BSA) rejection, and after waterpower was cleaned, this film had the higher flux recovery rate, and flux still is in higher level after long-term ultrafiltration.
Comparative Examples one
The preparation of poly (ether-sulfone) ultrafiltration membrane (film 5)
Take by weighing 7.2 gram polyether sulfones and 26.8 gram N, dinethylformamide is put into there-necked flask, and the heating stir about is 0.5 hour in 60 ℃ water bath with thermostatic control.Polyether sulfone is all after the dissolving, take by weighing 6.0 gram-molecular weights and be 2000 polyethylene glycol and add in the solution as pore-foaming agent, 60 ℃ down the heating stirring and dissolving obtain casting solution a after mixing about 4 hours, 60 ℃ of following standing and defoaming 2 hours.After being cooled to room temperature casting solution a is poured on knifing on the glass plate, in air, place 10～30 seconds after, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, obtain blank poly (ether-sulfone) ultrafiltration membrane (film 5);
Prepared blank poly (ether-sulfone) ultrafiltration membrane finds that through ESEM, contact angle and x-ray photoelectron spectroscopy analysis this film has typical milipore filter composite construction, and fenestra is evenly distributed, narrow pore size distribution range.The film pure water flux reaches 154.3L/ (m
2H), separating 1g/L bovine serum albumin(BSA) cushioning liquid, is 100% to the bovine serum albumin(BSA) rejection, and after waterpower was cleaned, the flux recovery rate was lower.
Table 1 is depicted as the stalling characteristic of the concentrated 1g/L bovine serum albumin(BSA) cushioning liquid of ultra-filtration and separation of embodiment and the prepared film of Comparative Examples.
Table 1
| Numbering | Polyvinyl alcohol mass concentration (%) | Borax mass concentration (%) | Cycle-index | Pure water flux (L/m 2h) | Rejection (%) | Flux recovery rate (%) |
| Film 1 film 2 films 3 films 4 films 5 | 0.5 1.0 2.0 0.5 0 | 0.5 0.5 0.5 0.5 0 | 3 3 3 6 0 | 108.8 128.7 113.0 84.0 154.3 | 100 100 100 100 100 | 78.2 80.2 86.3 81.4 53.1 |
The ultra-filtration and separation that table 2 is depicted as embodiment and the prepared film of Comparative Examples concentrates the stalling characteristic of the 900ppm oil-water emulsion of edible oil preparation.
Table 2
| Numbering | Polyvinyl alcohol mass concentration (%) | Borax mass concentration (%) | Cycle-index | Pure water flux (L/m 2h) | Rejection (%) | Flux recovery rate (%) |
| Film 2 films 3 films 5 | 1.0 2.0 0 | 0.5 0.5 0 | 3 3 0 | 128.7 113.0 154.3 | 100 100 100 | 29.6 44.4 26.3 |
Claims (1)
1. the preparation method of a ultrafiltration film of poly-ether-sulfone and anti-protein-contamination type is characterized in that may further comprise the steps:
(1) polyether sulfone is after under 110 ℃～150 ℃ dry 12 hours, be dissolved in 60 ℃ of N, in the dinethylformamide, be mixed with mass concentration and be 16～18% solution, add mass concentration and be 10～15%, molecular weight be 2000 polyethylene glycol as pore-foaming agent, mix promptly being mixed with casting solution a after stirring fully;
(2) with the prepared casting solution a of step (1) 50～70 ℃ of following standing and defoaming 2～4 hours, after being cooled to room temperature casting solution is poured on knifing on the glass plate, after in air, placing 10～30 seconds, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, obtain blank poly (ether-sulfone) ultrafiltration membrane b;
(3) polyvinyl alcohol is added in the deionized water, 90 ℃ of following stirring and dissolving are mixed with mass concentration and are 0.1～2.0% poly-vinyl alcohol solution c;
(4) be that 0.001% NaOH is dissolved in the deionized water with borax and mass concentration, be mixed with mass concentration and be 0.5～1.0% borax soln d;
(5) with the blank film b deionized water clean surface of step (2) gained, dry surface moisture, put into the solution c of step (3) gained, soaked 10 minutes;
(6) film is taken out from solution c, use the deionized water clean surface, dry moisture, put into the solution d of step (4) gained, soaked 10 minutes;
(7) set by step the process repetitive operation of (5) and (6) is 3～6 times, obtains modified poly (ether-sulfone) anti-protein-contamination milipore filter.
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| CN101574629B (en) * | 2008-05-09 | 2011-04-20 | 中国石油天然气股份有限公司 | Method for preparing polyvinyl alcohol/polyether sulfone pervaporation composite membrane |
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| US4618533A (en) * | 1984-11-30 | 1986-10-21 | Millipore Corporation | Porous membrane having hydrophilic surface and process |
| WO1994017905A1 (en) * | 1993-02-02 | 1994-08-18 | North West Water Group Plc. | Polymer porous structure and process |
| US6837996B2 (en) * | 2000-05-23 | 2005-01-04 | Ge Osmonics, Inc. | Polysulfonamide matrices |
| AUPS295702A0 (en) * | 2002-06-17 | 2002-07-04 | Proteome Systems Intellectual Property Pty Ltd | Coated hydrophilic membranes for electrophoresis applications |
| BRPI0515961A (en) * | 2004-10-13 | 2008-08-12 | 3M Innovative Properties Co | hydrophilic polyethersulfone membrane manufacturing method |
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| CN113956480A (en) * | 2021-11-22 | 2022-01-21 | 彩虹高新材料（莱阳）有限公司 | Chemically modified polyether sulfone and preparation method thereof |
| CN113956480B (en) * | 2021-11-22 | 2023-05-05 | 彩虹高新材料（莱阳）有限公司 | Chemically modified polyethersulfone and preparation method thereof |
| CN115569536A (en) * | 2022-09-28 | 2023-01-06 | 浙江大学 | Anti-pollution ultrafiltration membrane and preparation method and application thereof |
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