CN103357275A - Ultrafiltration membrane after-treatment modification method - Google Patents
Ultrafiltration membrane after-treatment modification method Download PDFInfo
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- CN103357275A CN103357275A CN2013102598320A CN201310259832A CN103357275A CN 103357275 A CN103357275 A CN 103357275A CN 2013102598320 A CN2013102598320 A CN 2013102598320A CN 201310259832 A CN201310259832 A CN 201310259832A CN 103357275 A CN103357275 A CN 103357275A
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Abstract
The invention provides an ultrafiltration membrane after-treatment modification method. The ultrafiltration membrane after-treatment modification method comprises the following steps of: (1) preparing an after-treatment solution, namely preparing a surface active agent, hydrophilic polymer, an anticorrosive, a humectant and RO purified water into the after-treatment solution according to a certain proportion; (2) heating, namely heating the after-treatment solution obtained in the step (1) to a certain temperature; (3) soaking or spraying, namely performing soaking or spraying on an ultrafiltration membrane with the after-treatment solution obtained in the step (2); and (4) drying, namely suspending the soaked ultrafiltration membrane for natural air-drying or drying the soaked ultrafiltration membrane. According to the method provided by the invention, the hydrophilicity of the ultrafiltration membrane can be improved, and the membrane keeps high flux at a dry state; meanwhile, the method has the advantages of being easy to operate and obvious in effect, easily realizing production running, and the like.
Description
Technical field
The present invention relates to a kind of milipore filter post processing method of modifying, be specifically related to a kind of hollow fiber ultrafiltration membrane and flat plate ultrafiltration membrane post processing method of modifying.
Background technology
Over nearly 30 years, the development of hyperfiltration technique is very rapid, not only original effect is being arranged aspect the separation of special solution, and is also using more and morely aspect industrial water supply.For example in the preparation of desalinization, pure water and high purity water, ultrafiltration can be used as pre-processing device, guarantees the long-term safety stable operation of the follow-up equipments such as counter-infiltration.In food and drink, mineral water were produced, important function had also been brought into play in ultrafiltration.Because the impurity such as suspension, colloidal particles and bacterium in the water are only removed in ultrafiltration, and have kept the mineral matter useful to health.
Ultrafiltration is a kind of membrane separation technique, and its film is the porous dissymmetrical structure.Filter process is take both sides differential pressure of membrane as driving force, and take a kind of solution separation process of mechanical grading principle as the basis, working pressure is generally 0.01～0.03MPa, and the screening aperture is from 0.005～0.1 μ m, and molecular cut off is about 1000～500,000 dalton.Milipore filter has normal temperature, low pressure, without phase transformation, energy consumption is low, efficient is high, the characteristics such as easy and simple to handle, be used widely aspect many at drink water purifying, water for industrial use processing, beverage, biology, food, medicine, environmental protection, chemical industry, metallurgy, oil etc. at present.
Milipore filter is hollow fiber ultrafiltration membrane and flat plate ultrafiltration membrane using more form now, the material that can be used for making ultrafiltration is a lot, comprising: Kynoar (PVDF), polyether sulfone (PES), polypropylene (PP), polyethylene (PE), polysulfones (PS), polypropylene nitrile (PAN), polyvinyl chloride (PVC) etc.At the beginning of the nineties, polyether sulfone materials has commercially obtained application; And the end of the nineties, the Kynoar ultrafiltration of more excellent performance begins to be widely used in water treatment field.Therefore Kynoar and polyether sulfone become at present the most widely used milipore filter material.
When ultrafiltration and micro-filtration were used for water treatment, the chemical stability of its material and hydrophily were two most important character.Chemical stability has determined the life-span of material under the effect of soda acid, oxidant, microorganism etc., and it also is directly connected to the method that cleaning can be taked; Hydrophily has then determined the degree of absorption of membrane material to organic pollutants, affects the flux of film.
Generally speaking, the separation system of film is aqueous phase system.Hydrophilic film surface forms hydrogen bond with water, makes it to be in ordered structure, will must break this ordered structure near the film surface when hydrophobic solute, obviously is difficult for carrying out, so that face is difficult for is contaminated.Water on hydrophobic surface is without hydrogen bond action, and hydrophobic solvent is to increase the entropy spontaneous process near the film surface, and then film is easily polluted by hydrophobic solute.
Add hydrophilic substance in the milipore filter production process, make the film surface in water, present hydrophily, in case but after the film drying, hydrophily will lose, change waterproof, and the damage that very easily fractureed that becomes fragile of hollow membrane silk, dull and stereotyped diaphragm also can be because of dry and crispatura, even peel off with nonwoven and to separate.So in process of production in order to keep the performance of film, usually adopt the mode that seals, adds hygroscopic agent to make milipore filter keep hygrometric state, but milipore filter is long term storage under hygrometric state, and following drawback is arranged: (1) microbial proliferation causes biological pollution (even Pore Blocking) and biodegradation; (2) be unfavorable for the membrane module processing and manufacturing.For example, normal curing, the sealing of the moisture damage hollow-fiber module end socket of wet film and rolling assembly film back side periphery adhesive; (3) if film is dipped in the sterilized solution to be stored, though can overcome biological pollution and biodegradation, but still be unfavorable for the membrane module processing and manufacturing and be not easy to transportation and storage.Therefore, milipore filter answers dry state to store.
There is now multiple diverse ways to can be used for the milipore filter post processing and preserves, mainly be divided into the physics and chemistry method.With adding the dull and stereotyped MF of 200ppm polyethylene glycol (PEG2000-8000) RO purified rinse water or UF film number minute, mainly be in order to improve the purpose of surface hydrophilicity such as patent US2004/0140259A1.Chemistry and its purpose of radiation modifying method are coated with last layer hydrophilic PEG layer such as (1) patent CN1509804A and CN1704152A with cross-linking reaction in order to apply more for a long time one deck hydrophilic layer or direct some hydrophilic radicals of grafting on the skeleton of tunica fibrosa; (2) patent CN1772359A describes some hydrophilies of direct grafting and ion exchangeable group process; (2) patent CN1539550A, CN1546214A, CN1067412C, US5531900 uses radiotechnology to process such as plasma resonance, the UV radiation, electron beam irradiation and corona radiation etc., the free group of film Surface Creation that the surface of processing the hydrophobic fiber film is and being activated, then make hydrophilic little molecule or greatly molecule be chemically bound on the surface of hollow fiber ultrafiltration membrane.Make surface hydrophilicity can keep for a long time and have resistance tocrocking by the radiotechnology surface modification, select separating effect.Be all Shortcomings parts of physics or chemical modification method, although that the physics cladding process fixes surface agent technique by physisorption is simple, surface of solids agent is easily run off.Apply one deck hydrophilic layer by chemical crosslink reaction, cause membrane aperture to diminish because coating layer thickness is difficult to control, although hydrophilic enhancing, water flux reduces.The surface of using various inorganic strong alkali chemical conversion films often not only the surface nature of film change but also the skeleton of film also changes such as film silk remitted its fury, face and nonwoven are easily peeled off and are come off, the hydrophilic radical that the film surface forms for example-OH ,-COOH ,-NH
2Deng oxidized in air and lose hydrophily.Radiotechnology disposal methods process is more complicated often, and equipment and technology requires high and expensive, and large-scale industrial production is still had any problem.Milipore filter natural-dehydration drying will cause the avalanche of fenestra, thereby have a strong impact on permeability and the mechanical strength of film.Therefore needing that film is made dry state processes.
Summary of the invention
Have the shortcoming and defect that in milipore filter dry state store method, exists now for overcoming, the invention provides a kind of hollow fiber film yarn and dull and stereotyped diaphragm of making and under drying regime, carry high-throughout milipore filter post processing method of modifying.
A kind of milipore filter post processing method of modifying of the present invention may further comprise the steps:
(1) preparation post-treatment solution: with surfactant, hydrophilic polymer, anticorrisive agent, NMF is mixed with according to certain ratio with RO water (pure water) and mixes post-treatment solution, wherein, the mass percentage content of mixing surfactant in the aftertreatment fluid is 0.2%～1%, the quality percentage composition of hydrophilic polymer is 0.1%～10%, and anticorrisive agent quality percentage composition is 0.5%～8%, and the quality percentage composition of NMF is 1%～60%;
(2) heating: the post-treatment solution of step (1) gained is heated to 45 ℃～65 ℃.
(3) soak or spray: milipore filter is sprayed or soak more than 1 hour with the aftertreatment fluid of step (2) gained.
(4) drying: the milipore filter after will soaking perhaps got final product 35 ℃～65 ℃ oven dry 5～8 hours in air-dry 2～3 days at normal temperatures.
In order better to realize the present invention:
Wherein, the described milipore filter of described ultrafiltration can be hollow fiber ultrafiltration membrane or flat plate ultrafiltration membrane.
A kind of in the preferred tween of surfactant described in the described step (1), OP phosphate, APES, NPE, polyethylene glycol oxide benzene sulfonamide acid ammonium salt, detergent alkylate naphthenic acid sodium or the dodecyl naphthenic acid sodium or more than one mixture.
A kind of in the preferred polyethylene glycol of hydrophilic polymer (PEG) described in the described step (1), polyvinylpyrrolidone (PVP), PEO or inorganic nano-particle aluminium oxide, the titanium dioxide or more than one mixture.
A kind of in the preferred sodium hydrogensulfite of anticorrisive agent, Sodium Benzoate or the calcium propionate described in the described step (1) or more than one mixture.
NMF preferably glycerine described in the described step (1), propane diols or sorbierite a kind of or more than one mixture.
The quality percentage composition of the hydrophilic polymer in the described step (1) is preferably 0.5%～8%.
The quality percentage composition of the anticorrisive agent in the described step (1) is preferably 0.5%～5%.
The quality percentage composition of the NMF in the described step (1) is preferably 5%～30%.
Milipore filter post processing method of modifying of the present invention and application thereof compared with prior art have the following advantages:
(1) the present invention is applicable to hollow fiber ultrafiltration membrane and the flat plate ultrafiltration membrane thereof of various materials.
(2) after the ultrafiltration membrane filaments after the present invention processes or diaphragm are immersed in the water, but the immediate recovery hygrometric state, protective agent is rinsed totally within very short time, and hydrophily is recovered rapidly, and water flux improves.
(3) film silk or diaphragm after the present invention processes can keep certain pliability, become fragile after the solution film silk drying, peel off the problem of separating with nonwoven after the diaphragm drying.
(4) milipore filter of this fermentation processing is dry film, and water content descends in a large number, has solved wet film and has been unfavorable for membrane module processing and manufacturing and transportation hard problem because microbial proliferation causes biological pollution (even Pore Blocking) and biodegradation and wet film.
(5) milipore filter after the present invention processes was placed in air 30 days, and having no moisture increases or over-drying situation, thoroughly solved milipore filter and wet because the suction of adding protective agent and producing causes the film silk again to become and cause the storage difficult problem
(6) technological operation of the present invention is simple, and production cost is low, easily moves in large-scale production process.
The specific embodiment
In order to further specify the superiority of processing method of the present invention, below for some embodiment, but the specific embodiment of the present invention is not limited in this.
Embodiment 1
(1) preparation post-treatment solution: get OP phosphate, polyethylene glycol (PEG-400), sodium hydrogensulfite, glycerine and be mixed with the mixing aftertreatment fluid, wherein mix and contain the 0.5%OP phosphate in the aftertreatment fluid, 5% polyethylene glycol (PEG-400), 0.5% sodium hydrogensulfite, 20% glycerine;
(2) heating: the post-treatment solution of step (1) gained is heated to 45 ℃.
(3) immersion or spray: the aftertreatment fluid with step (2) gained soaks the PES hollow fiber ultrafiltration membrane, and soak time is 2 hours.
(4) drying: the PES hollow fiber ultrafiltration membrane after will soaking in air natural drying 48 hours.Obtain processing caudacoria silk moisture content＜5%, placed 15 days in air, having no moisture increases.Without the film silk water flux of any processing and after the immersion treatment drying water flux referring to table one.
Embodiment 2
(1) preparation post-treatment solution: get NPE, polyvinylpyrrolidone (PVP-K17), Sodium Benzoate, glycerine and be mixed with the mixing aftertreatment fluid, wherein mix and contain 0.3% NPE in the aftertreatment fluid, 8% polyvinylpyrrolidone (PVP-K17), 1% Sodium Benzoate, 25% glycerine;
(2) heating: the post-treatment solution of step (1) gained is heated to 50 ℃.
(3) immersion or spray: the aftertreatment fluid with step (2) gained soaks the PVDF Flat Membrane, and soak time is 5 hours.
(4) drying: the PVDF Flat Membrane after will soaking in air natural drying 48 hours.Obtain processing rear film moisture content＜5%, placed 15 days in air, having no moisture increases.Without the diaphragm water flux of any processing and after the immersion treatment drying water flux referring to table two.
Embodiment 3
(1) preparation post-treatment solution: get Tween-80, polyethylene glycol (PEG-6000), sodium hydrogensulfite, propane diols and be mixed with the mixing aftertreatment fluid, wherein mix and contain 1% Tween-80 in the aftertreatment fluid, 4% polyethylene glycol (PEG-6000), 1% sodium hydrogensulfite, 30% propane diols;
(2) heating: the post-treatment solution of step (1) gained is heated to 60 ℃.
(3) immersion or spray: the aftertreatment fluid with step (2) gained sprays the PES hollow fiber ultrafiltration membrane, and spray time is 3 hours.
(4) drying: the PES hollow fiber ultrafiltration membrane after will soaking in air natural drying 48 hours.Obtain processing caudacoria silk moisture content＜5%, placed 15 days in air, having no moisture increases.Without the film silk water flux of any processing and after the immersion treatment drying water flux referring to table one.
Embodiment 4
(1) preparation post-treatment solution: get detergent alkylate naphthenic acid sodium, inorganic nano-particle aluminium oxide, calcium propionate, glycerine and be mixed with the mixing aftertreatment fluid, wherein mix and contain 0.2% detergent alkylate naphthenic acid sodium in the aftertreatment fluid, 2% inorganic nano-particle aluminium oxide, 1% calcium propionate, 30% glycerine;
(2) heating: the post-treatment solution of step (1) gained is heated to 60 ℃.
(3) immersion or spray: the aftertreatment fluid with step (2) gained sprays the PVDF Flat Membrane, and spray time is 2 hours.
(4) drying: the PVDF Flat Membrane after will soaking in air natural drying 48 hours.Obtain processing rear film moisture content＜5%, placed 15 days in air, having no moisture increases.Without the diaphragm water flux of any processing and after the immersion treatment drying water flux referring to table two.
Embodiment 5(effect comparing embodiment)
Get the PES hollow fiber ultrafiltration membrane, the film silk is after cleaning, directly in the air natural drying 48 hours at normal temperatures, obtain dry caudacoria silk water content＜5% of processing, without the wet silk water flux of any processing and the water flux after direct natural drying in normal temperature air referring to table one.
Embodiment 6(effect comparing embodiment)
Get the PVDF flat plate ultrafiltration membrane, diaphragm is after cleaning, directly in the air natural drying 48 hours at normal temperatures, obtain dry rear film water content＜5% of processing, without the humidity strip water flux of any processing and the water flux after direct natural drying in normal temperature air referring to table two.
Table one
Table two
Claims (9)
1. milipore filter post processing method of modifying may further comprise the steps:
(1) preparation post-treatment solution: with surfactant, hydrophilic polymer, anticorrisive agent, NMF is mixed with according to certain ratio with RO water and mixes post-treatment solution, wherein, the mass percentage content of mixing surfactant in the aftertreatment fluid is 0.2%～1%, the quality percentage composition of hydrophilic polymer is 0.1%～10%, and anticorrisive agent quality percentage composition is 0.5%～8%, and the quality percentage composition of NMF is 1%～60%;
(2) heating: the post-treatment solution of step (1) gained is heated to 45 ℃～65 ℃;
(3) soak or spray: milipore filter is sprayed or soak more than 1 hour with the aftertreatment fluid of step (2) gained;
(4) drying: the milipore filter after will soaking perhaps got final product 35 ℃～65 ℃ oven dry 5～8 hours in air-dry 2～3 days at normal temperatures.
2. a kind of milipore filter post processing method of modifying as claimed in claim 1, it is characterized in that: described milipore filter is hollow fiber ultrafiltration membrane or flat plate ultrafiltration membrane.
3. a kind of milipore filter post processing method of modifying as claimed in claim 1 is characterized in that: the surfactant described in the described step (1) is a kind of in tween, OP phosphate, APES, NPE, polyethylene glycol oxide benzene sulfonamide acid ammonium salt, detergent alkylate naphthenic acid sodium or the dodecyl naphthenic acid sodium or more than one mixture.
4. a kind of milipore filter post processing method of modifying as claimed in claim 1 is characterized in that: the hydrophilic polymer described in the described step (1) is a kind of in polyethylene glycol (PEG), polyvinylpyrrolidone (PVP), PEO or inorganic nano-particle aluminium oxide, the titanium dioxide or more than one mixture.
5. a kind of milipore filter post processing method of modifying as claimed in claim 1 is characterized in that: the anticorrisive agent described in the described step (1) is a kind of in sodium hydrogensulfite, Sodium Benzoate or the calcium propionate or more than one mixture.
6. a kind of milipore filter post processing method of modifying as claimed in claim 1, it is characterized in that: the NMF described in the described step (1) is glycerine, propane diols or sorbierite a kind of or more than one mixture.
7. a kind of milipore filter post processing method of modifying as claimed in claim 1, it is characterized in that: the quality percentage composition of the hydrophilic polymer described in the described step (1) is 0.5%～8%.
8. a kind of milipore filter post processing method of modifying as claimed in claim 1, it is characterized in that: the quality percentage composition of the anticorrisive agent described in the described step (1) is 0.5%～5%.
9. a kind of milipore filter post processing method of modifying as claimed in claim 1, it is characterized in that: the quality percentage composition of the NMF described in the described step (1) is 5%～30%.
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| CN112390976B (en) * | 2020-10-27 | 2022-09-06 | 刘洪江 | Method for hydrophilizing surface of hydrophobic article |
| CN112619421A (en) * | 2020-11-03 | 2021-04-09 | 蓝星（杭州）膜工业有限公司 | Nanofiltration dry film humectant |
| CN113648841A (en) * | 2021-08-05 | 2021-11-16 | 苏州中色德源环保科技有限公司 | Dry-state preservation method for hollow fiber membrane |
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