CN101695637B - Disposable polyether sulfone micro-filtration membrane and preparation method thereof - Google Patents
Disposable polyether sulfone micro-filtration membrane and preparation method thereof Download PDFInfo
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- CN101695637B CN101695637B CN2009101977662A CN200910197766A CN101695637B CN 101695637 B CN101695637 B CN 101695637B CN 2009101977662 A CN2009101977662 A CN 2009101977662A CN 200910197766 A CN200910197766 A CN 200910197766A CN 101695637 B CN101695637 B CN 101695637B
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Abstract
The invention provides a disposable polyether sulfone micro-filtration membrane and a preparation method thereof. The disposable polyether sulfone micro-filtration membrane is characterized by being prepared from the following raw materials in mass by weight: 10 to 15 percent of polyether sulfone, 57 to 87.5 percent of solvent, 1 to 10 percent of thickening agent, 1 to 8 percent of pore-forming agent, and 0.5 to 10 percent of hydrophilizing agent. The method for preparing the disposable polyether sulfone micro-filtration membrane comprises the steps of raw material stirring and mixing in proportion, knifing, solidifying, cleaning and drying. The disposable polyether sulfone micro-filtration membrane has the advantages of high percentage of opening, high flow and high filtering effect.
Description
Technical field
The present invention relates to a kind of disposable polyether sulfone micro-filtration membrane and preparation method thereof, be used for the particulate matter of filtering liquid medicine, belong to the micro-filtration membrane technical field.
Background technology
The material that is used for micro-filtration in the market, all there is different shortcomings as CAM, the molten spray fiber membrane of polypropylene, nylon membrane, nucleopore membranes: CAM, raw material refines from cotton, intensity difference, suitable efflorescence, and easily decomposed by many microbial attacks, when the chemical group of the kind of microorganism and replacement not simultaneously, the ruined degree of film properties is also inequality.
Polypropylene screen is owing to adopt high temperature to melt and spray fiber elongation method, and its film surface is made up of many exposed long fibres, its acid-fast alkali-proof, and intensity, but fiber easily comes off, and the membrane aperture of production is also bigger, is difficult to accomplish the film of 0.2 μ m～2 μ m.
Nylon membrane: the film of existing market uses nylon 66 mostly, the intensity height, good hydrophilic property, but the alkaline-resisting acid nonfast characteristic that also exists, and itself has hygroscopicity, along with hygroscopic increase, its yield strength descends, and membrane aperture easily changes, and for example diminishes, the time of using is long more, and its flow reduced rate is big more.
Nucleopore membranes: nucleopore membranes is the high energy particle radiation (radiation intensity is generally 1mev) that is produced by the radio isotope fission, vertical bump membrane material thin slice, material body is suffered damage and form track, erode the bulk material at track place then with aggressive agent, this track is enlarged, form the cylindrical hole of very narrow pore size distribution, because the film body plate is thin, has only 0.02～0.03 μ m, intensity is very poor, and percent opening extremely low (about 15%), assembling, use, flow etc. are restricted.
Polyether sulfone (Polyethersulfone is called for short PES) is that Britain ICI company is at exploitation in 1972 and the commercial a kind of special engineering plastics of success, because PES vitrification point height, thing, voltinism can be good, be used to make NF membrane, milipore filter and micro-filtration membrane abroad, also has hemodiafiltration device etc., the film of producing with its has the intensity height, good filtration effect, advantage such as flow velocity is fast.
Traditional disposable polyether sulfone micro-filtration membrane is made by following raw material by percentage to the quality: membrane material: PES, 10～35%; Solvent: dimethyl formamide, 30～75%; Surfactant: polyvinylpyrrolidone, 12～15%; Stripping agent: sodium chloride, 0～10% and the gas evaporation agent: calcium carbonate, 20～60%.Its preparation technology is: membrane material, solvent, additive are put into container, in 25 ℃～85 ℃ temperature ranges, stir 0.5～6h and make abundant dissolving, through filtering [film] deaeration, place slaking, make the PES casting solution, casting solution is poured on glass plate or other supporter, use the scraper knifing, the gap of scraper is 0.03～0.18mm, 20 ℃～45 ℃ of the operating temperatures of knifing, relative humidity 50～90%.Enter phase I of inversion of phases from knifing, nascent film is evaporation in 20～150 seconds, precipitation in air, preliminary gel.After the pore-forming film forming, enter first coagulating bath, coagulation bath temperature is controlled at 15 ℃～45 ℃, keeps 3～20min.First coagulating bath composition comprises: water, hydrochloric acid (0～12%), surfactant (0～2.5%), and hydrochloric acid in first coagulating bath and the calcium carbonate reaction in the film are produced carbon dioxide, form pore; Second stepping goes in second water-bath to clean, and second water-bath is a purified water, and temperature is 20 ℃～90 ℃, keep 10～60min, enter the 3rd sea water bath then, also soak with mass ratio 0～3% surfactant, time 4～20min is dried in 30 ℃～80 ℃ temperature at last.Its shortcoming is: owing to adopt gas to force hole forming method in the above-mentioned prescription, have the shortcoming that percent opening is low, flow is low, filter effect is low, also have use therein hydrochloric acid that environment, soil, underground water are all had no small harm.
Summary of the invention
The purpose of this invention is to provide high disposable polyether sulfone micro-filtration membrane of a kind of percent opening height, flow height and filter effect and preparation method thereof.
In order to achieve the above object, technical scheme of the present invention provides a kind of disposable polyether sulfone micro-filtration membrane, it is characterized in that, is made by following raw material by percentage to the quality:
Polyether sulfone 10%～15%;
Solvent 57%～87.5%;
Thickener 1%～10%;
Pore former 1%～8%;
Hydrophilizing agent 0.5%～10%.
Described polyether sulfone is PES 3000P.
Described solvent is dimethylacetylamide, dimethyl formamide or N-N-methyl-2-2-pyrrolidone N-(NMP).
Described thickener is that molecular weight is 2 * 10
3～2 * 10
6Polyvinylpyrrolidone (PVP), polyethylene glycol (PEG) 200, PEG400 or Macrogol 600.
Described pore former is acetone, absolute ethyl alcohol, ethylene glycol or water.
Described hydrophilizing agent is polysorbas20 or Tween 80.
The present invention also provides the preparation method of above-mentioned disposable polyether sulfone micro-filtration membrane, it is characterized in that, concrete steps are:
The first step: in proportion polyether sulfone and solvent are joined in the mixer, stir 3～5h at 25 ℃～80 ℃ with rotating speed 490～510rpm, add thickener, pore former and hydrophilizing agent in proportion, continue to stir 8～10h again, cross 200 mesh filter screens, vacuum defoamation 8～12h obtains casting solution;
Second step: the casting solution that the first step is obtained casts on the supporter, obtains nascent film with the scraper knifing, and wherein, the clearance height of scraper is 0.15～0.35mm, and scraping film temperature is 25 ℃～40 ℃, relative humidity 40%～80%;
The 3rd step: the nascent film that second step was obtained stops 30～180s with the solvent evaporates pore-forming in air, enter first coagulating bath then successively, second cleaner bath and the 3rd bathing pool, has 25 ℃～40 ℃ apyrogeneity purified water in described first coagulating bath, has 25 ℃～50 ℃ apyrogeneity purified water in second cleaner bath, has 40 ℃～80 ℃ the hydrophilizing agent aqueous solution in the 3rd bathing pool, described hydrophilizing agent is a dodecyl sodium sulfate, lauryl sodium sulfate or neopelex, its mass concentration is 0.5%～3%, and described nascent film is in first coagulating bath, the time of staying in second cleaner bath and the 3rd bathing pool is respectively 5～20min, 5～20min and 2～8min; To obtain the micro-filtration membrane that the aperture is 0.2 μ m～10 μ m at 70 ℃～100 ℃ oven dry 2～15min through the micro-filtration membrane of the 3rd bathing pool.
The present invention is the inversion of phases anisotropic membrane, and promptly a face of film is greater than or less than the hole of another side, so claim anisotropic membrane.Because being organic polymer PES and all kinds of solvents, the composition of casting solution forms, so organic polymer is to be linked by a lot of very little molecule monomers, the macromolecule casting solution makes macromolecule precipitating from homogeneous phase solution come out by all means, promptly be divided into two-phase: one forms polymeric membrane mutually at last for the macromolecule richness mutually, another is that macromolecule is stingy mutually, become the hole in the film at last, in identical casting solution is formed, only need simple temperature, humidity, the evaporation time that changes environment, just can change the evaporation rate constant, thereby obtain the film in different apertures.
Advantage of the present invention is: the present invention adopts best in the world plastics PES, by liquid liquid phase separation method, technology is simple, product cost is low, meet Chinese consumption situation, the product of being produced has percent opening height (60%～80%), flow height (make filter with the film of Φ 25, the 1m differential pressure flow is greater than 700ml), filter effect height (the particulate rejection rate of right 〉=2 μ m is greater than 95%), promptly possessed three high performances.Owing to have only-SO in the polyether sulfone macromolecular structure
2-ehter bond and phenyl ring skeleton do not have-the C-C-chain, do not contain the great biphenyl structural of rigidity yet, so its hear resistance, resistance to ag(e)ing, chemical proofing, stability are high.The PES film can use down continuously at 140 ℃, repeatedly moise-heat sterilization, and do not add sulfonation PES (all adopting sulfonation PES to make hydrophilizing agent) in the prescription of the present invention abroad, only with the single macromolecular material of PES, the PES micro-filtration membrane intensity height of being produced, safe in utilization, reliable, convenient.
The specific embodiment
Specify the present invention below in conjunction with embodiment.
Embodiment 1
Disposable polyether sulfone micro-filtration membrane, (molecular weight is 2 * 10 to the polyether sulfone PES 3000P that is produced by U.S. Su Wei company
4～5 * 10
5), solvent, thickener, pore former and hydrophilizing agent make.Its preparation method is: polyether sulfone and solvent are joined in the mixer stir in proportion, add thickener, pore former and hydrophilizing agent, continue to stir, cross 200 mesh filter screens, vacuum defoamation obtains casting solution; Casting solution is cast on the supporter, obtain nascent film with the scraper knifing, the film of will coming into being stops 30～180s with the solvent evaporates pore-forming in air, enter first coagulating bath, second cleaner bath and the 3rd bathing pool then successively, and oven dry obtains the micro-filtration membrane that the aperture is 0.2 μ m～10 μ m.Wherein, described concrete parameter such as following table:
Embodiment 2
Be similar to embodiment 1, difference is that concrete parameter is as follows:
Embodiment 3
Be similar to embodiment 1, difference is that concrete parameter is as follows:
The molecular weight of PVP is 2 * 10
3～2 * 10
6
Embodiment 4
Embodiment 1-4 properties of product test result sees the following form:
Polyether sulfone filter membrane of the present invention is mainly used in the particulate matter in the medical and clinical filtering liquid medicine.
At first filter membrane is made the shape that regulation is wanted, made liquid medicine filter.Liquid medicine filter divides upper shell, lower house, housing be by the medical high polymer plastics through injection mo(u)lding, put filter membrane of the present invention, filtration then in the middle of it.Upper and lower casing and filter membrane assembling back are carried out integrally welded with ultrasonic wave, one end feed liquor, soup be through behind the filter membrane, and particulate matter wherein can be filtered that film is held back and filtering, from the clean relatively soup of other end output, make transfusion reach safe and effective purpose clinically then.
Claims (4)
1. the preparation method of a disposable polyether sulfone micro-filtration membrane, described disposable polyether sulfone micro-filtration membrane is made by following raw material by percentage to the quality: polyether sulfone 10%～15%; Solvent 57%～87.5%; Thickener 1%～10%; Pore former 1%～8% and hydrophilizing agent 0.5%～10% is characterized in that, concrete steps are:
The first step: in proportion polyether sulfone and solvent are joined in the mixer, stir 3～5h at 25 ℃～80 ℃ with rotating speed 490～510rpm, add thickener, pore former and hydrophilizing agent in proportion, continue to stir 8～10h again, cross 200 mesh filter screens, vacuum defoamation 8～12h obtains casting solution; Described solvent is dimethylacetylamide, dimethyl formamide or N-N-methyl-2-2-pyrrolidone N-, and described thickener is that molecular weight is 2 * 10
3～2 * 10
6Polyvinylpyrrolidone, Macrogol 200, PEG400 or Macrogol 600;
Second step: the casting solution that the first step is obtained casts on the supporter, obtains nascent film with the scraper knifing, and wherein, the clearance height of scraper is 0.15～0.35mm, and scraping film temperature is 25 ℃～40 ℃, relative humidity 40%～80%;
The 3rd step: the nascent film that second step was obtained stops 30～180s with the solvent evaporates pore-forming in air, enter first coagulating bath then successively, second cleaner bath and the 3rd bathing pool, has 25 ℃～40 ℃ apyrogeneity purified water in described first coagulating bath, has 25 ℃～50 ℃ apyrogeneity purified water in second cleaner bath, the dodecyl sodium sulfate that has 40 ℃～80 ℃ in the 3rd bathing pool, lauryl sodium sulfate or sodium dodecyl benzene sulfonate aqueous solution, its mass concentration is 0.5%～3%, and described nascent film is in first coagulating bath, the time of staying in second cleaner bath and the 3rd bathing pool is respectively 5～20min, 5～20min and 2～8min; To obtain the micro-filtration membrane that the aperture is 0.2 μ m～10 μ m at 70 ℃～100 ℃ oven dry 2～15min through the micro-filtration membrane of the 3rd bathing pool.
2. the preparation method of disposable polyether sulfone micro-filtration membrane as claimed in claim 1 is characterized in that, described polyether sulfone is PES 3000P.
3. the preparation method of disposable polyether sulfone micro-filtration membrane as claimed in claim 1 is characterized in that, described pore former is acetone, absolute ethyl alcohol, ethylene glycol or water.
4. the preparation method of disposable polyether sulfone micro-filtration membrane as claimed in claim 1 is characterized in that, described hydrophilizing agent is polysorbas20 or Tween 80.
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| CN105268335A (en) * | 2014-07-23 | 2016-01-27 | 上海一鸣过滤技术有限公司 | Preparation method of hydrophilic polyether sulfone microporous film |
| CN104525004B (en) * | 2015-01-14 | 2017-09-01 | 安得膜分离技术工程(北京)有限公司 | A kind of polyether sulfone micro-filtration membrane and preparation method thereof |
| CN106310983A (en) * | 2015-06-23 | 2017-01-11 | 上海振浦医疗设备有限公司 | Disposable polyethersulfone air microfiltration membrane and preparation method thereof |
| CN106310422A (en) * | 2015-06-23 | 2017-01-11 | 上海振浦医疗设备有限公司 | Disposable precise filtering infusion apparatus for filleting bacterial endotoxin |
| CN106362600B (en) * | 2016-08-30 | 2018-10-02 | 泉州索爱膜科技开发有限公司 | The preparation method of the energy saving seperation film of low catching molecular and this application of energy saving seperation film in treatment of dyeing wastewater |
| CN111921385B (en) * | 2020-08-27 | 2023-02-14 | 苏州振浦医疗器械有限公司 | Preparation method of medical hydrophilic blend coating microfiltration membrane |
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