CN1365849A - Low-separation extreme-hydrophilic mixing ultrafilter membrane and its preparing process - Google Patents
Low-separation extreme-hydrophilic mixing ultrafilter membrane and its preparing process Download PDFInfo
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- CN1365849A CN1365849A CN 01108190 CN01108190A CN1365849A CN 1365849 A CN1365849 A CN 1365849A CN 01108190 CN01108190 CN 01108190 CN 01108190 A CN01108190 A CN 01108190A CN 1365849 A CN1365849 A CN 1365849A
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- 238000000926 separation method Methods 0.000 title claims abstract description 24
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- 238000000034 method Methods 0.000 title claims description 8
- 230000008569 process Effects 0.000 title description 2
- 238000002360 preparation method Methods 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229920002689 polyvinyl acetate Polymers 0.000 claims abstract description 20
- 239000011118 polyvinyl acetate Substances 0.000 claims abstract description 20
- 239000011148 porous material Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 239000002033 PVDF binder Substances 0.000 claims abstract description 12
- 239000012046 mixed solvent Substances 0.000 claims abstract description 12
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 12
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
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- 229920001477 hydrophilic polymer Polymers 0.000 claims description 5
- 230000010148 water-pollination Effects 0.000 claims description 5
- 238000013459 approach Methods 0.000 claims description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
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- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 claims description 2
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- FDJOLVPMNUYSCM-UVKKECPRSA-L cobalt(3+);[(2r,3s,4r,5s)-5-(5,6-dimethylbenzimidazol-1-yl)-4-hydroxy-2-(hydroxymethyl)oxolan-3-yl] [(2r)-1-[3-[(2r,3r,4z,7s,9z,12s,13s,14z,17s,18s,19r)-2,13,18-tris(2-amino-2-oxoethyl)-7,12,17-tris(3-amino-3-oxopropyl)-3,5,8,8,13,15,18,19-octamethyl-2,7, Chemical compound [Co+3].N#[C-].C1([C@H](CC(N)=O)[C@@]2(C)CCC(=O)NC[C@@H](C)OP([O-])(=O)O[C@H]3[C@H]([C@H](O[C@@H]3CO)N3C4=CC(C)=C(C)C=C4N=C3)O)[N-]\C2=C(C)/C([C@H](C\2(C)C)CCC(N)=O)=N/C/2=C\C([C@H]([C@@]/2(CC(N)=O)C)CCC(N)=O)=N\C\2=C(C)/C2=N[C@]1(C)[C@@](C)(CC(N)=O)[C@@H]2CCC(N)=O FDJOLVPMNUYSCM-UVKKECPRSA-L 0.000 abstract 1
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
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Abstract
本发明公开了一种低分离极限亲水性共混超滤膜及其制备方法。它是由11－20%的聚偏氟乙烯,0.2－1.2%的聚醋酸乙烯酯,2－7%的成孔剂和76－83%的强极性混合溶剂用相转化法制备而成,然后用弱溶剂浸泡处理。该超滤膜分离极限低——对维生素B12的截留率大于90%,水通量大——在0.1MPa下,通量为80－100L/M2h。并用专用的制备方法,以增加超滤膜在低分离极限范围的应用和提高超滤膜的化学稳定性,它特别适用于食品饮料、医药卫生和生物技术领域分离分子量100－2000的物质。The invention discloses a low separation limit hydrophilic blended ultrafiltration membrane and a preparation method thereof. It is prepared by phase inversion method from 11-20% polyvinylidene fluoride, 0.2-1.2% polyvinyl acetate, 2-7% pore forming agent and 76-83% strong polar mixed solvent. Then soak it in a weak solvent. The ultrafiltration membrane has a low separation limit—the rejection rate of vitamin B 12 is greater than 90%, and the water flux is large—at 0.1 MPa, the flux is 80-100 L/M 2 h. And a special preparation method is used to increase the application of the ultrafiltration membrane in the low separation limit range and improve the chemical stability of the ultrafiltration membrane. It is especially suitable for separating substances with a molecular weight of 100-2000 in the fields of food and beverage, medicine and health, and biotechnology.
Description
The present invention relates to a kind of low-separation extreme-hydrophilic mixing ultrafilter membrane and preparation method thereof, exactly, it is to belong to a kind of organic polymer thin-film material that possesses the isolated by filtration function, the pore size scope of film can the isolated molecule amount be material of 100-2000 and preparation method thereof from liquid at 5-50nm.
" grant of national natural science foundation guide " pointed out, functional high molecule material is one of three main directions of high-molecular organic material subject.Diffusion barrier is a big class important function macromolecular material, and milipore filter is a big class diffusion barrier that is used for liquid-phase system, and membrane separation technique is a green and energy-conservation high-tech industry technology of 21 century.The common advantage of its process is that efficient height, cost are low, normal-temperature operation, saving energy, pollution-free and recyclable utility.Membrane technology is applied more and more widely in fields such as petrochemical industry, environmental protection, food and drink, medical and health, electronics, electric power, metallurgy, industry light industry textile industry, desalinizations.Sales volume nineteen ninety of whole world polymeric membrane for separation is 2,200,000,000 dollars, reaches 8,800,000,000 dollars in 2000, and average annual growth rate is 14.9% over 10 years.Estimate that the annual growth of five to ten years whole world diffusion barriers is approximately 20% from now on.
Milipore filter separates has become one of the widest membrane technology of application, accounts for 1/5th of various application of membrane total amounts.The demand of milipore filter is mainly in fields such as food, medicine, wastewater treatment, pure water preparation, biotechnology, oil recoveries.In food industry, milipore filter is used for technologies such as mineral water, pure water, space water, and this class producer of the whole nation has surpassed 6000 families at present; The clarification filtration degerming removal of impurities of drinks, there are several thousand families in the producer that the whole nation produces wine; The clarification degerming of fruit juice, tea beverage and other food and drinks.The whey processing is a big market of milipore filter in the processing of farm products.Milipore filter is used to filter alcohol, acid, extract, concentrate, supplementing water, ammoniacal liquor etc. in a large number in antibiotic and other medical industries; Along with the issue of the new pharmacopeia of China, the depyrogenation of injection soup and infusion solutions water etc. will use milipore filter more.The example that milipore filter is used for waste water and liquid waste processing aspect has: the coating of electrophoretic coating process reclaims and the water reuse, realizes cleaner production; The processing of metal processing oily waste water; The processing of oil recovery re-injection water; The recovery of PVA in the textile industry sizing liquor; The concentrated recovery of waste liquid in the adhesives industries; The processing of paper industry plain boiled water; The water circulation of residential building; Or the like.In biotechnology, milipore filter is used for separating and concentrated component from zymotic fluid, and purifying concentrates various enzymes, hormone, albumen, collecting cell, and filter medium and culture medium, or the like.In power industry, milipore filter and other diffusion barriers are used for the processing of heat power equipment feedwater and recirculated water.In petroleum industry, milipore filter can become the key technology of handling oil-containing re-injection water, and the re-injection water in the several elephant of China every year has several hundred million tons.
The separation extreme of various milipore filters (claiming molecular cut off MWCO again) differs greatly, scope from 1000 to hundreds of thousands.The domestic producer that is engaged in milipore filter production mainly produces the milipore filter of MWCO at 1-10 ten thousand, and the main dependence on import of low-separation extreme milipore filter (MWCO=1000-10000), along with the application of milipore filter isolation technics enlarges day by day, increasing to the demand of high flux low-separation extreme milipore filter.It is raw material that present domestic and international commercial low-separation extreme milipore filter adopts polysulfones, cellulose acetate and derivative thereof more, these membrane materials all exist the bad shortcoming of chemical stability, particularly easy swelling and cause the rapid decline of water flux in organic solvents such as ethanol.And present low-separation extreme milipore filter ubiquity the higher shortcoming of operating pressure.Therefore press for the good low-separation extreme-hydrophilic milipore filter of a kind of chemical stability.
By retrieval as can be known, Yu Sanchuan that " water technology " 1999 the 2nd phases deliver and the Gao paper " development of small-bore PVDF milipore filter " from exhausting has proposed the scheme of hydrophilic ultrafiltration membrane.This scheme has many advantages, but shortcoming is also arranged: to use inorganic salts in (1) preparation liquid, and complicated; (2) use heat treated post-processing approach, rejection is descended, promptly separation extreme is low inadequately.
The present invention seeks to invent the prescription of the good low-separation extreme-hydrophilic milipore filter of a kind of new preparation chemical stability, the milipore filter that adopts phase inversion to prepare carries out post processing with the raising hydrophily with certain Weak solvent again.That is to say, be a kind of low-separation extreme-hydrophilic mixing ultrafilter membrane of invention and preparation method thereof
Task of the present invention is: Kynoar is a kind of fluoropolymer, and chemical stability is fine, but hydrophobicity is strong.The present invention adopt the hydrophilic polymer polyvinyl acetate with it blend improve the hydrophily of polyvinylidene fluoride (PVDF) ultrafiltration membrane.Low-separation extreme-hydrophilic mixing ultrafilter membrane, its preparation liquid is formed preparation liquid by Kynoar, hydrophilic polymer, pore former and intensive polar solvent, and wherein, the percentage by weight of each component is as follows: 11-20% Kynoar (PVDF); 0.2-1.2% polyvinyl acetate (PVAc); The 2-7% pore former; 76-83% is by N, dinethylformamide (DMF) and N, and N-dimethylacetylamide (DMAc) is by the strong polarized mixed solvent that mixes at 1: 1.
Another task of the present invention is: prepare the post-processing approach of polymeric membrane by the step of phase inversion, make the milipore filter that comes 30 minutes to improve hydrophily with the Weak solvent immersion treatment of 60-80%, the steps include:
(1) earlier Kynoar (PVDF) and polyvinyl acetate (PVAc) are processed into powder, then add mixed solvent and pore former, about 60 ℃, stir according to proportioning.After polymer dissolves fully, continue to keep temperature to stir again 10 minutes, form the homogeneous phase preparation liquid;
(2) with preparation liquid under 60 ℃, left standstill 24 hours;
(3) with acetone glass plate is cleaned up earlier.Preparation liquid adopts the hydrostomia method scraping the nascent state film of making about 100 μ m on the clean glass plate, immerses gel solidification film forming in the water-bath then;
(4) made next milipore filter 30 minutes with a kind of Weak solvent immersion treatment, the concentration range of Weak solvent is 60-80%;
(5) water with 0.2MPa carries out promptly obtaining finished film after precompressed is handled to milipore filter in ultrafilter.
The characteristics that the present invention had are:
(1) the preparation liquid system is simpler, and inorganic salts of no use also can reach than water flux---under 0.1MPa, flux is 80-100L/M greatly
2h
(2) post-processing approach of polymeric membrane.The film of making is immersed in a kind of Weak solvent 30 minutes, and water flux can increase 8-10 doubly.
What the present invention relates to is a kind of polymer ultrafiltration membrane, uses in hydrophilic system.This milipore filter is specially adapted to the material of food and drink, medical and health and biological technical field isolated molecule amount 100-2000.The milipore filter that the present invention prepares has following characteristics:
(1) separation extreme is low---to Cobastab
12The rejection of (molecular weight is 1350) is greater than 90%.
(2) hydrophily is strong, and water flux is big under low operating pressure---and under 0.1MPa, flux is 80-100L/M
2H.
(3) chemical stability is good---and acidproof, alkaline-resisting, strong oxidizers such as anti-ozone, organic solvent-resistant.
Below the present invention is described in further detail by instantiation.
The phase inversion that the present invention relates to prepares the processing step of milipore filter and sees Figure of description.
Hydrophilic polymer is a polyvinyl acetate, and Weak solvent is glycerine-aqueous solution or ethanol-water solution.
(1) earlier Kynoar (PVDF) and polyvinyl acetate (PVAc) are processed into powder, then add mixed solvent and pore former, about 60 ℃, stir according to proportioning.After polymer dissolves fully, continue to keep temperature to stir again 10 minutes, form the homogeneous phase preparation liquid.
(2) with preparation liquid under 60 ℃, left standstill 24 hours.
(3) with acetone glass plate is cleaned up earlier.Preparation liquid adopts the hydrostomia method scraping the nascent state film of making about 100 μ m on the clean glass plate, immerses gel solidification film forming in the water-bath then.
(4) made next milipore filter 30 minutes with a kind of Weak solvent immersion treatment, the concentration range of Weak solvent is 60-80%.
(5) water with 0.2MPa carries out promptly obtaining finished film after precompressed is handled to milipore filter in ultrafilter.
Embodiment one:
The preparation preparation liquid.Kynoar (PVDF) and polyvinyl acetate (PVAc) are processed into powder, add mixed solvent and pore former: PVDF15%, PVAc0.5%, pore former (ethyl acetate) 4.5%, DMF and DMAc mixed solvent 80% according to following percentage by weight.About 60 ℃, stir.After polymer dissolves fully, continue to keep temperature to stir again 10 minutes, form transparent homogeneous phase preparation liquid.Preparation liquid under 60 ℃, was left standstill 24 hours.
System film: with acetone base plate is cleaned up earlier.Preparation liquid adopts the hydrostomia method to scrape on clean glass plate and makes the nascent state film, immerses gel solidification film forming in the water-bath then.
Post processing: made next milipore filter 30 minutes with 75% ethanol-water solution immersion treatment.Water with 0.2MPa in ultrafilter carries out promptly obtaining finished film after precompressed is handled to milipore filter.
Measure performance: the water flux J (L/M that under 0.1MPa, measures finished film with ultrafilter
2H) with to Cobastab
12Rejection R (%).
Embodiment two:
Preparation preparation liquid: Kynoar (PVDF) and polyvinyl acetate (PVAc) are processed into powder, add mixed solvent and pore former: PVDF13.5% according to following percentage by weight, PVAc0.7%, pore former (phosphoric acid) 4.8%, DMF and DMAc mixed solvent 81%.About 60 ℃, stir.After polymer dissolves fully, continue to keep temperature to stir again 10 minutes, form transparent homogeneous phase preparation liquid.Preparation liquid under 60 ℃, was left standstill 24 hours.
System film: with acetone base plate is cleaned up earlier.Preparation liquid adopts the hydrostomia method to scrape on clean glass plate and makes the nascent state film, immerses gel solidification film forming in the water-bath then.
Post processing: the glycerine with 60%-aqueous solution soaking is handled and was made next milipore filter 30 minutes.Water with 0.2MPa in ultrafilter carries out promptly obtaining finished film after precompressed is handled to milipore filter.
Measure performance: the water flux J (L/M that under 0.1MPa, measures finished film with ultrafilter
2H) with to Cobastab
12Rejection R (%).
Embodiment three:
Preparation preparation liquid: Kynoar (PVDF) and polyvinyl acetate (PVAc) are processed into powder, add mixed solvent and pore former: PVDF17.5% according to following percentage by weight, PVAc1%, pore former (acetone) 4%, DMF and DMAc mixed solvent 77.5%.About 60 ℃, stir.After polymer dissolves fully, continue to keep temperature to stir again 10 minutes, form transparent homogeneous phase preparation liquid.Preparation liquid under 60 ℃, was left standstill 24 hours.
System film: with acetone base plate is cleaned up earlier.Preparation liquid adopts the hydrostomia method to scrape on clean glass plate and makes the nascent state film, immerses gel solidification film forming in the water-bath then.
Post processing: made next milipore filter 30 minutes with 80% ethanol-water solution immersion treatment.Water with 0.2MPa in ultrafilter carries out promptly obtaining finished film after precompressed is handled to milipore filter.
Measure performance: the water flux J (L/M that under 0.1MPa, measures finished film with ultrafilter
2H) with to Cobastab
12Rejection R (%).
Milipore filter performance measurement result
Water flux J
Rejection R (%)
(L/M
2H) embodiment one 92.5 91.3 embodiment 2 88.2 92.6 embodiment 3 83.6 93.0
Claims (4)
1. low-separation extreme-hydrophilic mixing ultrafilter membrane and preparation method thereof, it is characterized in that: low-separation extreme-hydrophilic mixing ultrafilter membrane, its preparation liquid is formed preparation liquid by Kynoar, hydrophilic polymer, pore former and intensive polar solvent, wherein, the percentage by weight of each component is as follows: 11-20% Kynoar (PVDF); 0.2-1.2% polyvinyl acetate (PVAc); The 2-7% pore former; 76-83% is by N, dinethylformamide (DMF) and N, and N-dimethylacetylamide (DMAc) is by the strong polarized mixed solvent that mixes at 1: 1.
2. low-separation extreme-hydrophilic mixing ultrafilter membrane according to claim 1 and preparation method thereof, it is characterized in that: hydrophilic polymer is a polyvinyl acetate.
3. one kind is exclusively used in the preparation method who makes low-separation extreme-hydrophilic mixing ultrafilter membrane, it is characterized in that: the post-processing approach of preparing polymeric membrane by the step of phase inversion, make the milipore filter that comes 30 minutes to improve hydrophily with the Weak solvent immersion treatment of 60-80%, the steps include:
(1) earlier Kynoar (PVDF) and polyvinyl acetate (PVAc) are processed into powder, then add mixed solvent and pore former, about 60 ℃, stir according to proportioning.After polymer dissolves fully, continue to keep temperature to stir again 10 minutes, form the homogeneous phase preparation liquid;
(2) with preparation liquid under 60 ℃, left standstill 24 hours;
(3) with acetone glass plate is cleaned up earlier.Preparation liquid adopts the hydrostomia method scraping the nascent state film of making about 100 μ m on the clean glass plate, immerses gel solidification film forming in the water-bath then;
(4) made next milipore filter 30 minutes with a kind of Weak solvent immersion treatment, the concentration range of Weak solvent is 60-80%;
(5) water with 0.2MPa carries out promptly obtaining finished film after precompressed is handled to milipore filter in ultrafilter.
4. low-separation extreme-hydrophilic mixing ultrafilter membrane preparation method according to claim 3 is characterized in that: Weak solvent is glycerine-aqueous solution or ethanol-water solution.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100337729C (en) * | 2005-10-22 | 2007-09-19 | 燕山大学 | Chemical modification technique for microfiltering separation film of polyvinylidene fluoride |
| CN100357350C (en) * | 2005-03-16 | 2007-12-26 | 福州大学 | The pH sensitive film with polyvinylidene fluoride/polyurethane mixture film as base film and its prepn process |
| CN101195084B (en) * | 2007-06-14 | 2010-11-17 | 海南立昇净水科技实业有限公司 | Hydrophilic polyvinyl chloride alloy ultrafiltration membrane and production method thereof |
| CN101472671B (en) * | 2006-06-27 | 2012-05-23 | 东丽株式会社 | Polymer separation film and preparation method thereof |
| CN107362698A (en) * | 2017-07-31 | 2017-11-21 | 苏州苏净环保新材料有限公司 | A kind of preparation method and applications of durable hydrophilic property polyvinylidene fluoride film |
-
2001
- 2001-04-06 CN CN 01108190 patent/CN1132668C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100357350C (en) * | 2005-03-16 | 2007-12-26 | 福州大学 | The pH sensitive film with polyvinylidene fluoride/polyurethane mixture film as base film and its prepn process |
| CN100337729C (en) * | 2005-10-22 | 2007-09-19 | 燕山大学 | Chemical modification technique for microfiltering separation film of polyvinylidene fluoride |
| CN101472671B (en) * | 2006-06-27 | 2012-05-23 | 东丽株式会社 | Polymer separation film and preparation method thereof |
| US9259690B2 (en) | 2006-06-27 | 2016-02-16 | Toray Industries, Inc. | Polymer separation membrane and process for producing the same |
| CN101195084B (en) * | 2007-06-14 | 2010-11-17 | 海南立昇净水科技实业有限公司 | Hydrophilic polyvinyl chloride alloy ultrafiltration membrane and production method thereof |
| CN107362698A (en) * | 2017-07-31 | 2017-11-21 | 苏州苏净环保新材料有限公司 | A kind of preparation method and applications of durable hydrophilic property polyvinylidene fluoride film |
| CN107362698B (en) * | 2017-07-31 | 2020-12-15 | 苏州苏净环保新材料有限公司 | Preparation method and application of lasting hydrophilic polyvinylidene fluoride membrane |
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