CN101259387A - Controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane and preparation - Google Patents
Controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane and preparation Download PDFInfo
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- CN101259387A CN101259387A CNA2007100603668A CN200710060366A CN101259387A CN 101259387 A CN101259387 A CN 101259387A CN A2007100603668 A CNA2007100603668 A CN A2007100603668A CN 200710060366 A CN200710060366 A CN 200710060366A CN 101259387 A CN101259387 A CN 101259387A
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Abstract
The invention relates to a protein pollution-resistant polyether sulfone ultrafiltration membrane with controllable flux and a preparation method thereof. The invention takes polyether sulfone and Pluronic F127 as the raw materials according to a mass percentage of 21.6 to 36 percent. The preparation method includes: Pluronic F127 is added in the polyether sulfone solution of the N, N-dimethylformamide; the mixture is sufficiently stired and mixed to be prepared into a membrane casting solution which is cooled after standing and being defoamed; the membrane casting solution is poured on a glass plate for membrane scraping, stands, and is put into a water bath for being concreted and shaped into membrane; the membrane is dipped in water. The invention has a simple preparation method; the anti-pollution performance is greatly improved; simultaneously the invention has an excellent trapping characteristic on protein. The largest flux of the protein pollution-resistant polyether sulfone ultrafiltration membrane with controllable flux can reach more than 200L/ (m<2>h).
Description
Technical field
The present invention relates to milipore filter isolation technics, particularly a kind of controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane and preparation method thereof.
Background technology
Ultrafiltration is a kind of membrane process that separates according to separated material molecular weight difference.It has been generally acknowledged that ultra-filtration process is a screening process relevant with membrane aperture size, the pressure differential of film both sides is a motive force, and milipore filter is a separating medium.In the separation of the reluctant material liquid mixture of conventional method, demonstrate special advantages.Ultrafiltration has the following advantages as a kind of new and effective membrane separation technique: (1) no phase transformation, and low energy consumption is about 1/2～1/5 of evaporation or freezing energy consumption; (2) operating condition gentleness.Separate under normal temperature and low pressure, the variation of matter does not take place in material in the concentrating and separating process, be suitable for the processing of heat-sensitive substance; (3) the no third component is introduced.Milipore filter is the even non-individual body of being made by high molecular polymerization, does not in use have any impurity and comes off, and guarantees that ultrafiltrate is pure; (4) technological process is simple.The ultra-filtration and separation process is simple pressurized delivered liquid, and technological process is simple, the easy operating management.Because ultrafiltration has above advantage, ultrafiltration is applied to purify usually, separates and the three big fields of concentrating.
Though hyperfiltration technique is regarded as the most promising new technology of separating bio product, up to the present separative efficiency is also lower, is particularly also fully being used aspect the separating substances of biologically actives such as protein.Its principal element is divided into two aspects: the one, because the film that the interaction that exists between water-soluble macromolecule and the film surface causes pollution, the 2nd, generally do not have higher flux owing to have the milipore filter of good separation effect.Thereby, select, the design new material pollutes for suppressing film, it is extremely important to increase membrane flux, seeks a kind ofly both can carry out surface modification to having membrane material now, can strengthen the additive of pore effect again, become and solve that polymer ultrafiltration membrane pollutes and the effective way of flux problems.
In the membrane material of daily use, polyether sulfone has obtained using widely with its excellent comprehensive performance (machinery, physics and chemical stability, film forming characteristics, economy etc.).But the hydrophobic property that poly (ether sulfone) film is stronger makes it cause a large amount of absorption of protein on the film surface easily, causes separative efficiency to descend.The whole bag of tricks is applied to membrane surface modification, strengthens the anti pollution property on film surface, as chemical graft, and uv photo initiated grafting, low temperature plasma method, blending method etc.Easy and be widely used with blending method again in numerous method of modifying, improve membrane flux but in modifying process, often need to add pore-foaming agent.Therefore, adopt a kind of additive as modifier and pore-foaming agent, thereby it is controlled to prepare flux, and the maximized anti-protein-contamination milipore filter of surface modification density is most important for the application of ultrafiltration.
Summary of the invention
The object of the present invention is to provide a kind of controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane and preparation method thereof.This milipore filter protein is had stronger contamination resistance and flux controlled, preparation method's process is simple.
A kind of controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane provided by the invention is to be that 12600 Pluronic F127 is a raw material with polyether sulfone (PES) and molecular weight, mass percent by Pluronic F127 and polyether sulfone is 0%～100%, prepare burden, its preparation method may further comprise the steps:
1) at N, in the polyether sulfone solution of dinethylformamide, add Pluronic F127 (polyoxyethylene/polyoxypropylene/polyoxyethylene amphiphilic block copolymer, letter is F127), stir fully and promptly be mixed with casting solution after the mixing;
2) after the casting solution standing and defoaming, be cooled to room temperature, casting solution is poured on knifing on the glass plate, places in air, puts into the water-bath freezing film again.
3) be soaked in water, obtain controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane.
The preparation method of a kind of controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane provided by the invention may further comprise the steps:
1) at N, in the polyether sulfone solution of dinethylformamide, (polyoxyethylene/polyoxypropylene/polyoxyethylene amphiphilic block copolymer, letter is F127, HO (CH to add Pluronic F127
2-CH
2-O)
98-(CH (CH
3)-CH
2-O)
67-(CH
2-CH
2-O)
98H), stirring promptly is mixed with casting solution after fully mixing;
2) casting solution is 50～60 ℃ of following standing and defoaming after 5～12 hours, still casting solution is poured on knifing on the glass plate after being cooled to room temperature, in air, place 10～30 seconds after, put into the water-bath freezing film again.
3) be soaked in water 24～36 hours, changed water one time, and obtained controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane in per 4～5 hours.
The invention has the advantages that: the preparation method is easy, and the antifouling property of the poly (ether-sulfone) ultrafiltration membrane that makes is improved largely, and simultaneously protein is had the good characteristic of holding back.By regulating the mass percent that adds additive, on the basis that keeps antifouling property, obtained a series of flux and be the antipollution milipore filter that line style increases.Existing poly (ether-sulfone) ultrafiltration membrane is keeping rejection to be higher than under 95% the situation, and flux mostly is 100L/ (m greatly
2And the prepared controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane flux peak of the present invention can reach 200L/ (m h),
2H) more than.
The specific embodiment
The preparation of embodiment 1 controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane (film 1)
Take by weighing 3.60g polyether sulfone and 15.68g N, dinethylformamide is put into there-necked flask, puts into 60 ℃ water bath with thermostatic control and heats, and stirring and dissolving is about 0.5 hour under the 900r/min rotating speed.All after the dissolving, take by weighing the 0.72g molecular weight and be 12600 Pluronic F127 as additive, stirring and dissolving is 3.5 hours under same temperature.After mixing, 60 ℃ of following standing and defoaming 5～12 hours.After being cooled to room temperature casting solution is poured on the glass plate, with the metallic spatula knifing, in air, place 10～30 seconds after, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, changed deionized water one time, and obtained controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane in per 5 hours.
Prepared controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane 1 is through ESEM, infrared spectrum analysis, contact angle and X-ray diffraction analysis, this film mechanical strength height, pore-creating character is good, and fenestra is evenly distributed, narrow pore size distribution range, block polymer Pluronic F127 is even in the film surface distributed, good hydrophilic property.Be used to separate concentrating 1g/L bovine serum albumin(BSA) cushioning liquid, flux can maintain 50L/ (m
2H), the bovine serum albumin(BSA) rejection is 99.90%.After waterpower was cleaned, this film had the higher flux recovery rate, and flux still is in higher level after long-term ultrafiltration.
The preparation of embodiment 2 controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membranes (film 2)
Take by weighing 3.60g polyether sulfone and 14.96g N, dinethylformamide is put into there-necked flask, puts into 60 ℃ water bath with thermostatic control and heats, and stirring and dissolving is about 0.5 hour under the 900r/min rotating speed.All after the dissolving, take by weighing the 1.44g molecular weight and be 12600 Pluronic F127 as additive, stirring and dissolving is 3.5 hours under same temperature.After mixing, 60 ℃ of following standing and defoaming 5～12 hours.After being cooled to room temperature casting solution is poured on the glass plate, with the metallic spatula knifing, in air, place 10～30 seconds after, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, changed deionized water one time, and obtained controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane in per 5 hours.
Prepared controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane 2 is through ESEM, infrared spectrum analysis, contact angle and X-ray diffraction analysis, this film mechanical strength height, pore-creating character is good, and fenestra is evenly distributed, narrow pore size distribution range, block polymer Pluronic F127 is even in the film surface distributed, good hydrophilic property.Be used to separate concentrating 1g/L bovine serum albumin(BSA) cushioning liquid, flux can maintain 100L/ (m
2H), the bovine serum albumin(BSA) rejection is 99.17%.After waterpower was cleaned, this film had the higher flux recovery rate, and flux still is in higher level after long-term ultrafiltration.
The preparation of embodiment 3 controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membranes (film 3)
Take by weighing 3.60g polyether sulfone and 14.24g N, dinethylformamide is put into there-necked flask, puts into 60 ℃ water bath with thermostatic control and heats, and stirring and dissolving is about 0.5 hour under the 900r/min rotating speed.All after the dissolving, take by weighing the 2.16g molecular weight and be 12600 Pluronic F127 as additive, stirring and dissolving is 3.5 hours under same temperature.After mixing, 60 ℃ of following standing and defoaming 5～12 hours.After being cooled to room temperature casting solution is poured on the glass plate, with the metallic spatula knifing, in air, place 10～30 seconds after, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, changed deionized water one time, and obtained controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane in per 5 hours.
Prepared controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane 3 is through ESEM, infrared spectrum analysis, contact angle and X-ray diffraction analysis, this film mechanical strength height, pore-creating character is good, and fenestra is evenly distributed, narrow pore size distribution range, block polymer Pluronic F127 is even in the film surface distributed, good hydrophilic property.Be used to separate concentrating 1g/L bovine serum albumin(BSA) cushioning liquid, flux can maintain 142L/ (m
2H), the bovine serum albumin(BSA) rejection is 98.45%.After waterpower was cleaned, this film had the higher flux recovery rate, and flux still is in higher level after long-term ultrafiltration.
The preparation of embodiment 4 controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membranes (film 4)
Take by weighing 3.60g polyether sulfone and 13.52g N, dinethylformamide is put into there-necked flask, puts into 60 ℃ water bath with thermostatic control and heats, and stirring and dissolving is about 0.5 hour under the 900r/min rotating speed.All after the dissolving, take by weighing the 2.88g molecular weight and be 12600 Pluronic F127 as additive, stirring and dissolving is 3.5 hours under same temperature.After mixing, 60 ℃ of following standing and defoaming 5～12 hours.After being cooled to room temperature casting solution is poured on the glass plate, with the metallic spatula knifing, in air, place 10～30 seconds after, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, changed deionized water one time, and obtained controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane in per 5 hours.
Prepared controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane 4 is through ESEM, infrared spectrum analysis, contact angle and X-ray diffraction analysis, this film mechanical strength height, pore-creating character is good, and fenestra is evenly distributed, narrow pore size distribution range, block polymer Pluronic F127 is even in the film surface distributed, good hydrophilic property.Be used to separate concentrating 1g/L bovine serum albumin(BSA) cushioning liquid, flux can maintain 184L/ (m
2H), the bovine serum albumin(BSA) rejection is 97.82%.After waterpower was cleaned, this film had the higher flux recovery rate, and flux still is in higher level after long-term ultrafiltration.
The preparation of embodiment 5 controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membranes (film 5)
Take by weighing 3.60g polyether sulfone and 12.80g N, dinethylformamide is put into there-necked flask, puts into 60 ℃ water bath with thermostatic control and heats, and stirring and dissolving is about 0.5 hour under the 900r/min rotating speed.All after the dissolving, take by weighing the 3.60g molecular weight and be 12600 Pluronic F127 as additive, stirring and dissolving is 3.5 hours under same temperature.After mixing, 60 ℃ of following standing and defoaming 5～12 hours.After being cooled to room temperature casting solution is poured on the glass plate, with the metallic spatula knifing, in air, place 10～30 seconds after, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, changed deionized water one time, and obtained controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane in per 5 hours.
Prepared controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane 5 is through ESEM, infrared spectrum analysis, contact angle and X-ray diffraction analysis, this film mechanical strength height, pore-creating character is good, and fenestra is evenly distributed, narrow pore size distribution range, block polymer Pluronic F127 is even in the film surface distributed, good hydrophilic property.Be used to separate concentrating 1g/L bovine serum albumin(BSA) cushioning liquid, flux can maintain 209L/ (m
2H), the bovine serum albumin(BSA) rejection is 97.20%.After waterpower was cleaned, this film had the higher flux recovery rate, and flux still is in higher level after long-term ultrafiltration.
The preparation of Comparative Examples 1 poly (ether-sulfone) ultrafiltration membrane (film 6)
Take by weighing 3.60g polyether sulfone and 12.80g N, dinethylformamide is put into there-necked flask, puts into 60 ℃ water bath with thermostatic control and heats, and stirring and dissolving is about 0.5 hour under the 900r/min rotating speed.All after the dissolving, take by weighing the 3.60g molecular weight and be 2000 polyethylene glycol as pore-foaming agent, stirring and dissolving is 3.5 hours under same temperature.After mixing, 60 ℃ of following standing and defoaming 5～12 hours.After being cooled to room temperature casting solution is poured on the glass plate, with the metallic spatula knifing, in air, place 10～30 seconds after, put into the water-bath freezing film again, soaked 24～36 hours with deionized water, changed deionized water one time, and obtained poly (ether-sulfone) ultrafiltration membrane in per 5 hours.
Prepared controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane 6 process ESEMs, infrared spectrum analysis, contact angle and X-ray diffraction analysis, this film mechanical strength height, pore-creating character is better, the fenestra distribution uniform.Be used to separate concentrating 1g/L bovine serum albumin(BSA) cushioning liquid, flux can maintain 105L/ (m
2H), the bovine serum albumin(BSA) rejection is 95.21%.
Table 1 is depicted as the stalling characteristic result of the concentrated 1g/L bovine serum albumin(BSA) of ultra-filtration and separation of embodiment and the prepared film of Comparative Examples.
Table 1
From The above results as can be known, the present invention be that the prepared controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane performance of additive obviously is better than with the polyethylene glycol with Pluronic F127 one-component is the prepared poly (ether-sulfone) ultrafiltration membrane of pore-foaming agent.
Claims (3)
1, a kind of controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane, it is characterized in that it is is that 12600 Pluronic F127 is a raw material with polyether sulfone (PES) and molecular weight, mass percent by Pluronic F127 and polyether sulfone is 0%～100%, prepare burden, its preparation method may further comprise the steps:
1) at N, in the polyether sulfone solution of dinethylformamide, add Pluronic F127, stir fully and promptly be mixed with casting solution after the mixing;
2) after the casting solution standing and defoaming, be cooled to room temperature, casting solution is poured on knifing on the glass plate, places in air, puts into the water-bath freezing film again;
3) be soaked in water, obtain controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane.
2, the preparation method of the described controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane of claim 1 is characterized in that may further comprise the steps:
1), in the polyether sulfone solution of dinethylformamide, adds Pluronic F127 (HO (CH at N
2-CH
2-O)
98-(CH (CH
3)-CH
2-O)
67-(CH
2-CH
2-O)
98H), stirring promptly is mixed with casting solution after fully mixing;
2) casting solution is 50～60 ℃ of following standing and defoaming after 5～12 hours, still casting solution is poured on knifing on the glass plate after being cooled to room temperature, in air, place 10～30 seconds after, put into the water-bath freezing film again;
3) be soaked in water 24～36 hours, changed water one time, and obtained controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane in per 4～5 hours.
3, the preparation of the described controllable-flux protein-pollution-resistance poly (ether-sulfone) ultrafiltration membrane of claim 1 is characterized in that can be used for the antipollution milipore filter of protein separation.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102160970A (en) * | 2011-03-31 | 2011-08-24 | 天津大学 | Flux controllable anti-oxidation polyethersulfone nanofiltration membrane and preparation method thereof |
| CN102397758A (en) * | 2010-09-07 | 2012-04-04 | 中国石油天然气股份有限公司 | Preparation method for anti-pollution modified polyether sulfone nanofiltration membrane |
| CN108579437A (en) * | 2018-05-16 | 2018-09-28 | 天津工业大学 | A kind of big flux resistance to compression ultrafiltration membrane and preparation method thereof |
| CN108654385A (en) * | 2018-04-26 | 2018-10-16 | 天津大学 | A kind of preparation method having both highly selective high osmosis ultrafiltration membrane |
| CN110548420A (en) * | 2019-08-06 | 2019-12-10 | 天津大学 | Preparation method of zero-flux attenuation chemical heterogeneous hydrogel ultrafiltration membrane |
| CN111389226A (en) * | 2020-04-17 | 2020-07-10 | 浙江理工大学 | Permanent hydrophilic ultrafiltration membrane and preparation method thereof |
| CN115262233A (en) * | 2022-07-06 | 2022-11-01 | 中城国网(北京)综合能源有限公司 | Macromolecular antioxidant anti-condensation material capable of circularly absorbing and releasing moisture and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102397758A (en) * | 2010-09-07 | 2012-04-04 | 中国石油天然气股份有限公司 | Preparation method for anti-pollution modified polyether sulfone nanofiltration membrane |
| CN102397758B (en) * | 2010-09-07 | 2013-07-31 | 中国石油天然气股份有限公司 | Preparation method for anti-pollution modified polyether sulfone nanofiltration membrane |
| CN102160970A (en) * | 2011-03-31 | 2011-08-24 | 天津大学 | Flux controllable anti-oxidation polyethersulfone nanofiltration membrane and preparation method thereof |
| CN108654385A (en) * | 2018-04-26 | 2018-10-16 | 天津大学 | A kind of preparation method having both highly selective high osmosis ultrafiltration membrane |
| CN108579437A (en) * | 2018-05-16 | 2018-09-28 | 天津工业大学 | A kind of big flux resistance to compression ultrafiltration membrane and preparation method thereof |
| CN110548420B (en) * | 2019-08-06 | 2021-12-17 | 天津大学 | Preparation method of zero-flux attenuation chemical heterogeneous hydrogel ultrafiltration membrane |
| CN110548420A (en) * | 2019-08-06 | 2019-12-10 | 天津大学 | Preparation method of zero-flux attenuation chemical heterogeneous hydrogel ultrafiltration membrane |
| CN111389226A (en) * | 2020-04-17 | 2020-07-10 | 浙江理工大学 | Permanent hydrophilic ultrafiltration membrane and preparation method thereof |
| CN111389226B (en) * | 2020-04-17 | 2022-07-05 | 浙江理工大学 | Permanent hydrophilic ultrafiltration membrane and preparation method thereof |
| CN115262233A (en) * | 2022-07-06 | 2022-11-01 | 中城国网(北京)综合能源有限公司 | Macromolecular antioxidant anti-condensation material capable of circularly absorbing and releasing moisture and preparation method thereof |
| CN115262233B (en) * | 2022-07-06 | 2023-10-13 | 中城国网(北京)综合能源有限公司 | Macromolecule antioxidant anti-condensation material capable of circularly absorbing and releasing moisture and preparation method thereof |
| CN115738743A (en) * | 2022-12-08 | 2023-03-07 | 哈尔滨工业大学 | Method for preparing durable high-performance ultrafiltration membrane based on supermolecular assembly reinforced blending method |
| CN115738743B (en) * | 2022-12-08 | 2023-12-29 | 哈尔滨工业大学 | Method for preparing durable high-performance ultrafiltration membrane based on supermolecule assembly reinforced blending method |
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