CN101219350B - Method for producing hydrophilic polyethersulfone millipore filter - Google Patents
Method for producing hydrophilic polyethersulfone millipore filter Download PDFInfo
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Abstract
The invention discloses a method for preparing a hydrophilic polyethersulfone microporous filterable membrane, which comprises that polyethersulfone solid polymer is dissolved into high-polar organic solvent, in which polyvinylpyrrolidone and polymer mixture of ethylene acetate ester and polyoxazoline are added as specific additives, the solution is laid on a roller that continuously rotates or a conveyer belt that continuously rotates to cause conditioned air to contact with the solution, then initial filterable membrane on the roller or on the conveyer is put into a water bath of 5-80 DEG C for final molding; finally, the molded microporous filterable membrane is washed before post treatment and being dried, thus obtaining dried finished products. The invention has simple technique and easy operation, so the polyethersulfone microporous filterable membrane prepared has good filtering retention rate, flow rate and flux and extremely high bursting strength.
Description
Technical field:
The present invention relates to a kind of miillpore filter.
Background technology:
By the filter membrane that artificial synthetic method manufacturing is come out, aperture and range of application according to its product can roughly be divided into miillpore filter, milipore filter, reverse osmosis membrane etc.In the method for manufacturing, the most common method is via " inversion of phases " process, the filter membrane master material that is dissolved in the solution, through physical dissolution degree variation principle, is precipitated out with solid-state form from solution and makes filter membrane.
The method of making miillpore filter via " inversion of phases " process is repeatedly delivered at filter membrane circle.Generally speaking, the definition of miillpore filter is: the average diameter of three dimensions internal orifice dimension is at 0.01 micron porous filter membrane to 20 micrometer ranges in the filter membrane.Basically, mostly miillpore filter is the solid matter of dull and stereotyped paper or doughnut form, and its internal structure is formed by the continuous shape rule of crisscross genuine shape or irregular little shape aperture.When under stress, the fluid that contains solid impurity or particle is during by miillpore filter, and contained solid impurity or particle promptly can be stuck in the top or the inside of the miniature aperture of miillpore filter in the fluid.In principle, as long as solid impurity or the particle bigger than miillpore filter inside micro small aperture promptly can be intercepted, filter the effect of removing solid impurity or particle thereby reach.Sometimes, though when containing in the fluid than little solid impurity in miillpore filter aperture or particle, the solid impurity of this small size or particle, because the scrambling of physical form, the irregularly shaped duct by filter membrane interior three-dimensional spatial continuity that also can part is adsorbed or block, and filters the effect of removing solid impurity or particle thereby also can reach.
Miillpore filter can be categorized as two kinds of symmetry miillpore filter and asymmetry miillpore filters on the structure, though it is distinguished and is not exclusively clear and definite, the former miillpore filter is inner to be the micropore that contains roughly the same aperture, and this kind micropore is evenly distributed in filter membrane integral thickness layer but generally speaking.And latter's miillpore filter inside is the micropore that contains different apertures, and the micropore in the different apertures of this kind, and the gradual layering that is systematicness is in filter membrane integral thickness layer.That is to say, in the miillpore filter structure of typical asymmetry, the distribution of its pore size, be the superiors from the filter membrane integral thickness to orlop, change gradually.
Miillpore filter also can be categorized as two kinds of hydrophily and hydrophobicitys on the surface nature.Basically, in a single day the former contacts with pure water by miillpore filter, once light pressure or without any extra pressure, pure water can wetting at once microporous membrane surface, and can be diffused to the filter membrane inner body by the filter membrane absorbed inside, to cause the light transmission that is far longer than dry position in the light transmission at wetting position.Latter's miillpore filter is then fully opposite, and when contacting with pure water, under no extra pressure, its pure water is only controlled in the scope that is limited to the filter membrane contact point, and can not increased its range of scatter by the filter membrane absorbed inside.And,, there is no obvious difference comparing with the dry filter membrane of light transmission and remainder in the pure water contact range.
At present, the high-tech miillpore filter has comprised hydrophily, hydrophobicity, symmetrical expression and asymmetric etc., can reach the quality product of commercialization and industrialization volume production, be all the product of America and Europe or other advanced countries, and the many patent applied fors of production method, for example U.S. Patent number 4,203,804 U.S. Patent numbers 4,340,479 U.S. Patent numbers, 4,261,834 U.S. Patent numbers 4,629,563 U.S. Patent numbers 6,994,789 U.S. Patent numbers, 7,208,200 grades only are its example.
Summary of the invention:
The object of the present invention is to provide a kind of have splendid filtration flux and flow, the new production process of the hydrophilic polyethersulfone millipore filter that strainability is good.On the emphasis, the present invention has used other patents or has delivered in the document from original special hydrophily additive, after in case this additive is compatible with the polyether sulfone material, be difficult for breaking away from, and can increase the intensity of finished product hydrophilic polyethersulfone membrane greatly, for finished film becomes in the process of filter core in following process, provide the adequate condition of handling ease.
Technical solution of the present invention is:
A kind of production method of hydrophilic polyethersulfone millipore filter is characterized in that: comprise the following steps: successively
(1) the polyether sulfone solid-state polymer is dissolved in the organic solvent, and adds specific water soluble polymer additive;
(2) above-mentioned solution is tiled on the roller or conveyer belt of continuous rotation, air after overregulating is contacted with solution, to put into 5～80 ℃ of sea water baths at the formation thing on the roller or on the conveyer belt then and carry out final shaping unit, then with the filter membrane of moulding from roller or conveyer belt peel off;
(3) post processing: filter membrane is carried out variable speed or constant speed stretching, and clean, under 25～120 ℃, carry out drying then, get product through cleaning agent.
Whether for polyethersulfone millipore filter is hydrophily or hydrophobic standard, is to form with reference to Unite States Standard method of testing (being ASTMD570) correct.This patent invention for hydrophilic definition is: when dry finished product miillpore filter lies on the pure water that leaves standstill or the distilled water plane, and between 5～80 ℃ of temperature ranges, can be in 10 seconds, can more than 90% of wetting its finished product miillpore filter area.If meet above-mentioned definition, then this film is classified in the hydrophilic microporous filter membrane.Its physics visual appearance is: this miillpore filter after wetting by pure water or distilled water, the place's irradiation of subtend light can find that obviously by pure water or the wetting part of distilled water, its light transmittance is far longer than the miillpore filter under the drying regime.
In this patent invention, the macromolecular material of containing main topic promptly is a polyether sulfone, and its chemical structural formula is summarized as follows:
Its molecular weight is about tens thousand of between millions of, and physical state is the solid state white coloured particles at normal temperatures substantially.
The hydrophilic polyethersulfone millipore filter that this patent invention is contained, the scope of aperture between 0.01 micron to 20 microns, things such as solid impurity, particle, bacterium can be filtered accurately, but salt, anion, cation or the protein that is dissolved in the aqueous solution can not be filtered or remove.
Organic solvent in the step (1), the content that this patent invention is contained is dimethyl formamide, dimethylacetylamide, N-methyl pyrrolidone, dimethyl sulfoxide (DMSO), dioxane, or the mixture of above-mentioned organic solvent.Specific water soluble polymer additive is polyvinylpyrrolidone-ethene acetate Ji the macromolecular material of Ju oxazoline class (for example: mixture poly-2-ethyl-2-oxazoline).Polyether sulfone macromolecule in the step (1) accounts for 10% to 24% weight portion, and organic solvent accounts for 15% to 70% weight portion, and specific water soluble polymer additive accounts for 1% to 30% weight portion.Solution temperature is 10～60 ℃ in the step (2), the relative humidity of the air after overregulating is 10%～95%, dry-bulb temperature is 10～70 ℃, dew-point temperature is 10～70 ℃, air wind speed after overregulating is 0.1 meter per second～7 meter per seconds, and the air after overregulating contacts the processing time with solution be 2 seconds～20 minutes.Formation thing in the step (2) is put into 5～80 ℃ of sea water baths, and to carry out the final shaping unit processing time be 10 seconds～30 minutes.During post processing, cleaning agent is water, 5% acetone soln, ethanol, isopropyl alcohol, other water soluble alcohols organic solvents, or the mixture of above-mentioned solvent.Cleaning temperature is 10～90 ℃, and scavenging period is 1～120 minute.
Technology of the present invention is simple, processing ease, the hydrophilic polyethersulfone millipore filter of producing, have good filtering traffic and flux, strainability is good, and compare with the same aperture hydrophilic polyethersulfone millipore filter product made from additive method, have higher intensity, be difficult for the disconnected adequate condition in early stage of Zhe for follow-up filter core making provides.
The specific embodiment:
Get polyether sulfone solid-state polymer material, earlier through baking oven with 100 ℃ to 110 ℃ temperature heating 24 hours to 48 hours, to remove the moisture content of surface absorption, then this material after drying of heating is put into hermetically sealed can and lowers the temperature naturally.After being cooled to room temperature, taking-up and stirring and dissolving are in the organic solvent of high polarity at once, for example dimethyl formamide, dimethylacetylamide, N-methyl pyrrolidone, dimethyl sulfoxide (DMSO), dioxane, or the mixture of above-mentioned organic solvent, (for example: poly-2-ethyl-2-oxazoline) additive is through mixing to add polyvinylpyrrolidone-ethene acetate then Ji the macromolecular material of Ju Evil quinoline class.Aspect the formula concentration weight ratio, polyether sulfone accounts for 10% to 24% (example 10%, 18%, 24%), organic solvent accounts for 15% to 70% (example 15%, 45%, 70%), and polyvinylpyrrolidone-ethene acetate is Ji the macromolecular material mixture of Ju Evil quinoline class accounts for 1% to 30% (example 1%, 15%, 30%).Its polyvinylpyrrolidone-ethene acetate is Yu the total weight parts ratio of the macromolecular material of Ju oxazoline class is 10 to 20 to 1.
After solution preparation is finished, use coating cutter or additive method to comprise that method of radiation is coated in solution on the conveyer belt of the roller of continuous rolling or the metal that rotates continuously or other materials uniformly.Above the roller or above the conveyer belt, the stable air of sending after regulating contacts with solution, to carry out the phase transformation process.Air after regulating must be adjusted into 10% to 95% relative humidity (example 10%, 50%, 95%), and dry-bulb temperature is 10 ℃ to 70 ℃ (10 ℃, 40 ℃, 70 ℃ of examples), and dew-point temperature is 10 ℃ to 70 ℃ (10 ℃, 40 ℃, 70 ℃ of examples), and the air wind speed after regulating is 0.1 meter per second to 7 meter per second (example 0.1 meter per second, 4 meter per seconds, 7 meter per seconds), and also adjusting solution temperature simultaneously is 10 ℃ to 60 ℃ (10 ℃, 30 ℃, 60 ℃ of examples) (method of adjustment is that heating or freezing mode carry out).After this preformed step is finished, time is between 2 seconds to 20 minutes (example 2 seconds, 10 minutes, 20 minutes), enter the sea water bath that water temperature is controlled at 5 ℃ to 80 ℃ (5 ℃, 50 ℃, 80 ℃ of examples) at once at the formation thing on the roller or on the conveyer belt and carry out the final shaping unit step, the final shaping unit time is between 10 seconds to 30 minutes (example 10 seconds, 15 minutes, 30 minutes), to form polyethersulfone millipore filter.After polyethersulfone millipore filter creates, to peel off from roller or conveyer belt with mechanical system, polyethersulfone millipore filter enters last handling process then.Post-processing step has comprised variable speed or constant speed longitudinal stretching and solvent clean.Can use for example alcohol of water-miscible organic solvent during cleaning, or 5% (weight ratio) aqueous acetone solution, or the isopropyl alcohol equal solvent, or the pure water cleaning, or the mixture of above-mentioned solvent.The solvent clean temperature is (10 ℃, 50 ℃, 90 ℃) between 10 ℃ to 90 ℃.Scavenging period was 1 minute to 120 minutes (example 1 minute, 60 minutes, 120 minutes), or the longer time.Cleaning way can be diffusion into the surface cross-flow mode or rectilinear direct current mode.After cleaning was finished, filter membrane enters bellows or hothouse carries out drying.Baking temperature is between 25 ℃ to 120 ℃ (25 ℃, 70 ℃, 120 ℃ of examples), and drying mode can be the formula of leaving standstill or blowing-type.Dried polyethersulfone millipore filter possess hydrophilic property and high-intensity characteristic.
Before this patent invention, search through document and patent, never be mentioned or quoted the mixture of the macromolecular material that uses polyvinylpyrrolidone-ethene acetate and poly-oxazoline class simultaneously, to make polyethersulfone millipore filter as water-soluble additive.Use this water-soluble additives mixed thing in making polyethersulfone millipore filter, real is the important foundation invention of this patent.Moreover, we also find: do not use the macromolecular material of poly-oxazoline class if only use polyvinylpyrrolidone-ethene acetate, the hydrophilic microporous filter membrane that the intensity of the hydrophilic microporous filter membrane that it is made is made much smaller than the mixture of the macromolecular material that uses polyvinylpyrrolidone-ethene acetate and poly-oxazoline class.And only use the macromolecular material of Ju oxazoline class and do not use polyvinylpyrrolidone-produced miillpore filter of ethene acetate, its hydrophily is far smaller than the miillpore filter that the use polyvinylpyrrolidone-the ethene acetate is made, unless the macromolecular material consumption of poly-oxazoline class significantly improves.Significantly, for producing high-hydrophilic and high strength polyethersulfone millipore filter, use polyvinylpyrrolidone-ethene acetate Ji the mixture of the macromolecular material of Ju oxazoline class is one and plays a decisive role and important factor.
According to prescription and the flow process that this patent invention is revealed, the polyethersulfone millipore filter average pore size that manufactures and belongs to hydrophilic filter membrane between 0.01 micron to 20 microns.Utilizing the produced filter membrane of this patent inventive method is to have splendid filterability, high heat endurance, and high-tension, high strength, elastomeric material.Be to use at once in the micro porous filtration territory, to solve the predicament that high-grade filtering material difficulty is asked within Chinese territory.
After producing hydrophilic polyethersulfone millipore filter, this filter membrane also can be through high-temperature heat treatment, for example 150 ℃ to 250 ℃, improves the intensity of filter membrane once more.Other characteristics of this filter membrane after excessive temperature is handled, for example too big variation can't take place in steam bubble point, rate of flow of water etc.
Term definition:
The steam bubble point: the test of steam bubble point is an easy means a kind of commonly used of measuring the hydrophilic filter membrane aperture.During test, wetting hydrophilic filter membrane earlier with pure water, air pressure then edges up, use compressed air that air is clamp-oned in the filter membrane by in the hole of water blockage, when air pressure reaches a certain numerical value, water in hole can squeeze at once and drain, and can squeeze the i.e. steam bubble point of filter membrane for this reason of the minimum pressure drain to water this moment.On the principle, the aperture is bigger in the filter membrane, and corresponding steam bubble point is lower.In filter membrane circle, often use the steam bubble point to define the pore size of filter membrane.
Rate of flow of water: under quantitative pure water volume, the filter membrane of unit are, under specified pressure, the required time of the pure water that filters.Basically, the millipore water flow rate is higher, and institute's quantitative pure water required time that filters is fewer, and shown filter membrane percent opening is healed greatly, and this term is also used always by filter membrane circle.
Burst strength: above or below the dry filter membrane of particular area, apply air pressure, cause dry filter membrane explosion and must be minimum pressure.On the principle, filter membrane intensity and toughness are bigger, and its burst strength is bigger.
Embodiment 1: make 0.2 micron hydrophilic polyethersulfone millipore filter
In the laboratory, the ratio with 15% to 70% to 14% to 1% is polyether sulfone solid-state polymer material and dimethyl formamide, polyvinylpyrrolidone-ethene acetate and the poly-even stirring and dissolving of 2-ethyl-2-oxazoline.Between 20 to 40 ℃ of room temperatures, this solution is evenly coated on the flat board, make sample path length about in the of 0.4 millimeter, the steam that slowly is blown into relative humidity 60% to 70% then above solution bleaches until solution is visual.Solution after bleaching steadily enters in the pond at once to soak about 20 minutes, to do last typing.Between water temperature keeps 15 ℃ to 25 ℃ during typing.Then, through repeatedly (15 ℃ to 90 ℃) cleaning, to remove the residue chemistry product in the nascent filter membrane.After cleaning was finished, filter membrane entered drying baker with oven dry moisture content, makes dry flat polyethersulfone millipore filter at last.
With the filter membrane that this manufactured is come out, the characteristic of possess hydrophilic property and high burst strength.This filter membrane is done bacterium and is held back when challenging also according to U.S. HIMA standard, uses 10
7The bacterium of quantity, can 100% hold back the B.dimunita bacterium.
Its steam bubble point of filter membrane that comes out with this manufactured is 3.5 kg/cm, and under 20 inches mmhg pressures, rate of flow of water is 28 seconds/100 ml pure water/9.62 square centimeter filter areas.The burst strength of testing 23 millimeters dry diaphragms of circle of its diameter is 1.4 kg/cm.
Embodiment 2: make 0.2 micron hydrophilic polyethersulfone millipore filter
In the laboratory, ratio according to 15% to 70% to 15%, polyether sulfone solid-state polymer material and dimethylacetylamide, the polyvinylpyrrolidone-even stirring and dissolving of ethene acetate, between 20 to 40 ℃ of room temperatures, this solution is evenly coated on the flat board, make sample path length about in the of 0.4 millimeter, the steam that slowly is blown into relative humidity 60% to 70% then above solution bleaches until solution is visual.Solution after bleaching steadily enters the pond at once to soak about 20 minutes, to do last typing.Between water temperature keeps 15 ℃ to 25 ℃ during typing.Then, through repeatedly (15 ℃ to 90 ℃) cleaning, to remove the residue chemistry product in the nascent filter membrane.After cleaning was finished, filter membrane entered drying baker with oven dry moisture content, makes dry flat polyethersulfone millipore filter at last.
With the filter membrane that this manufactured is come out, the possess hydrophilic property characteristic.But burst strength with use embodiment 1 in produced filter membrane compare, obviously lower.This filter membrane is done bacterium and is held back when challenging when according to U.S. HIMA standard, uses 10
7The bacterium of quantity, also can 100% hold back the B.dimunita bacterium.
Its steam bubble point of filter membrane that comes out with this manufactured is 3.3 kg/cm, and under 20 inches mmhg pressures, rate of flow of water is 25 seconds/100 ml pure water/9.62 square centimeter filter areas.The burst strength of testing 23 millimeters dry diaphragms of circle of its diameter is 0.7 kg/cm.
Claims (6)
1. the production method of a hydrophilic microporous filter membrane is characterized in that: comprise the following steps: successively
(1) with the solid-state polymer material dissolves in organic solvent, and add and to form compatible water soluble polymer additive with this solid-state polymer material, this water soluble polymer additive is that polyvinylpyrrolidone-ethene acetate is Ji the mixture of the macromolecular material of Ju oxazoline, make uniform solution, the solid-state polymer material accounts for 10% to 24% total weight parts in this solution, organic solvent accounts for 15% to 70% total weight parts, polyvinylpyrrolidone-ethene acetate is Ji the mixture of the macromolecular material of Ju oxazoline accounts for 1% to 30% total weight parts, described organic solvent is a dimethyl formamide, dimethylacetylamide, the N-methyl pyrrolidone, dimethyl sulfoxide (DMSO), dioxane, or the mixture of above-mentioned organic solvent;
(2) above-mentioned solution temperature is adapted to 10～60 ℃ after, be tiled on the roller or conveyer belt of continuous rotation, to regulate back relative humidity is 10%～95%, dry-bulb temperature is 10～70 ℃, dew-point temperature is that 10～70 ℃ air contacts with solution, to put into 5～80 ℃ of sea water baths at the formation thing on roller or the conveyer belt then and carry out final shaping unit, then with the filter membrane of moulding from roller or conveyer belt peel off;
(3) post processing: filter membrane is carried out variable speed or constant speed stretching, and clean, under 25 ℃～120 ℃, carry out drying then, get product through cleaning agent.
2. the production method of miillpore filter according to claim 1, it is characterized in that: the solid-state material of macromolecule in the step (1) is a polyether sulfone.
3. the production method of miillpore filter according to claim 1 is characterized in that: polyvinylpyrrolidone in the step (1)-ethene acetate is Yu the total weight parts ratio of the macromolecular material of Ju oxazoline is 10 to 20 to 1.
4. the production method of miillpore filter according to claim 1, it is characterized in that: the air wind speed in the step (2) after overregulating is 0.1 meter per second～7 meter per seconds, the time that contacts with solution is 2 seconds～20 minutes.
5. the production method of miillpore filter according to claim 1 is characterized in that: forming thing in the step (2), to put into the time that sea water bath carries out final shaping unit be 10 seconds～30 minutes.
6. the production method of miillpore filter according to claim 1, it is characterized in that: during post processing in the step (3), cleaning agent is that water, weight concentration are 5% acetone soln, ethanol, isopropyl alcohol, other water-soluble alcohol organic solvents, or the mixture of above-mentioned solvent, cleaning temperature is 10～90 ℃, and scavenging period is 1～120 minute.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107803122A (en) * | 2017-11-24 | 2018-03-16 | 杭州易膜环保科技有限公司 | Hydrophilic milipore filter of one kind copolymers of VA containing PVP and preparation method thereof |
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| CN103418253A (en) * | 2012-05-16 | 2013-12-04 | 亚美滤膜（南通）有限公司 | Nitrocellulose microporous filtration membrane production process |
| CN109224876A (en) * | 2018-11-26 | 2019-01-18 | 迈凯特殊材料（苏州工业园区）有限公司 | A kind of hydrophilic polysulfone membrane preparation method and applications |
| US20230017950A1 (en) * | 2019-11-21 | 2023-01-19 | Emd Millipore Corporation | Hydrophilic membranes |
| CN112642292A (en) * | 2020-09-22 | 2021-04-13 | 迈博瑞生物膜技术（南通）有限公司 | Super-hydrophilic graphene flat microporous filter membrane and preparation method thereof |
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