CN100386136C - Method for producing porose semi-permeation filtering film - Google Patents
Method for producing porose semi-permeation filtering film Download PDFInfo
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- CN100386136C CN100386136C CNB2006100233613A CN200610023361A CN100386136C CN 100386136 C CN100386136 C CN 100386136C CN B2006100233613 A CNB2006100233613 A CN B2006100233613A CN 200610023361 A CN200610023361 A CN 200610023361A CN 100386136 C CN100386136 C CN 100386136C
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Abstract
The present invention discloses a method for producing a porose semi-permeation filter film which comprises: engineering plastics or polymer materials are dissolved in an organic solvent, and a water soluble polymer additive is added; the solution is flatly tiled on a roller or a conveyer belt which continuously rotates, air-conditioned air is in contact with the solution, and then, a primary filter film on the roller or the conveyer belt is put in water plunge bath with the temperature of 5 to 50 DEG C to be finally shaped; then the shaped filter film is stripped from the roller or the conveyer belt, post-processing is carried out, etc. The present invention has the advantages of simple process, easy operation, and good filtration flow rate and flux and good filter performance of the produced filter film.
Description
Technical field:
The present invention relates to a kind of filter membrane.
Background technology:
In aqueous solution miillpore filter is used, when for example removing the solid impurity case, the semi-permeable filter membrane of optimal porous is to have good hygroscopicity immediately (hydrophily immediately), high opening rate is to provide flow (flux) high in the unit interval, filter membrane self leachable is low, and aperture diameter on average waits character.At present, the high-tech porose semi-permeation filtering film can reach commercialization and industrialization volume production and superior in quality product, is all the product of America and Europe or other advanced countries.World-famous porose semi-permeation filtering film manufacturer is U.S. Pall, Millipore, minorities such as German Sartorius, Japanese Fuji.So far, Chinese filter membrane science and technology industry does not still have the enterprise that any family reaches the commercialization volume production before 40 years.At present, there is defective in common porose semi-permeation filtering film at aspects such as water imbibition, percent openings.
Summary of the invention:
The object of the present invention is to provide a kind of have good filtering traffic and flux, the production method of the porose semi-permeation filtering film that strainability is good.
Technical solution of the present invention is:
A kind of production method of porose semi-permeation filtering film is characterized in that: comprise the following steps: successively
(1) will be when suction gas equalization point, suction gas is that 2%～4% engineering plastics or polymeric solid material dissolves are in organic solvent, and add and to form compatible water soluble polymer additive with above-mentioned engineering plastics or polymeric solid material, make uniform solution, engineering plastics or polymeric solid material account for 10% to 30% total weight parts in this solution, organic solvent accounts for 15% to 30% total weight parts, and the water soluble polymer additive accounts for 40% to 75% total weight parts;
(2) above-mentioned solution temperature is transferred be made as 10～50 ℃ after, be tiled on the roller or conveyer belt of continuous rotation, to regulate back relative humidity is 40%～95%, dry-bulb temperature is 10～50 ℃, dew-point temperature is that 10～50 ℃ air contacts with solution, to put into 5～50 ℃ 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 25～80 ℃, carry out drying then, get product through cleaning agent.
Engineering plastics or macromolecular material are polysulfones, polyether sulfone, nylon 6, polyvinylidene fluoride, celluloid, cellulose mixture, poly-peptide or polyester.This type of material before use, material is most to be hydrophobicity (only minority is a hydrophily), but the finished product of porous semipermeable membrane then mostly is hydrophily (only minority still is hydrophobicity).When using the aqueous solution to filter, needn't be again through chemicals with alcohol or other low surface tensions, for example wetting agent or preliminary treatment such as interfacial agent can directly be used.The hydrophily speciality of the semi-permeable finished film of this porous comes from polyethylene glycol or other water-soluble and compatible with the raw material macromolecule additives that contains 1% to 6% (finished film weight ratio).
As for material qualitative whether be the standard of hydrophobicity or hydrophily (hygroscopicity at once), be to revise with reference to Unite States Standard method of testing (being ASTM D570) to form.This patent invention for the definition of hydrophobic material is: engineering plastics or macromolecular material, under solid-state form, in 24 hours, only can absorb 0.5% moisture content that is less than weight under the former drying regime of material, or when material reaches its suction gas equalization point, absorb 4% moisture content that is less than former weight under the former drying regime of material.Its physics visual appearance is, if when ranging hydrophobic material or hydrophobic porous property semipermeable membrane according to above-mentioned definition, if the water droplet or the globule are arranged on its surface, its water droplet or the globule are when tilting material, can be subjected to its deadweight and tumble, and not have visual visible hangover or water stain vestige.
Table one: the water imbibition data of letter several engineering plastics of example or macromolecular material are as reference
According to the definition of this patent invention, PEI, polysulfones and polyether sulfone listed in the table one all range hydrophobic material.And nylon 66, Nomex and cellulose acetate can range hydrophilic material.
Engineering plastics or macromolecular material that this patent invention is contained are to meet the material that the hydrophobicity definition of approval is adopted in this patent invention.In a single day this kind material is used and the porose semi-permeation filtering film that produces, as long as filter membrane contains polyethylene glycol or other macromolecule additives water-soluble and can be compatible with raw material of some.The certain possess hydrophilic property of finished product filter membrane then, and can be wetting at once by aqueous water.
The porose semi-permeation filtering film that this patent invention is contained, the scope of aperture between 0.01 micron to 20 microns can be filtered solid impurity, particle accurately, things such as bacterium, but can not filter or remove salt, anion, cation or the protein that is dissolved in the aqueous solution.
The definition of used " can be wetting at once by aqueous water " is in this patent invention: when dry finished film lies in the pure water that leaves standstill or distilled water plane, can be in 10 seconds, and can more than 50% of wetting its finished film area.If meet above-mentioned definition, then this film is the scope of classified belonging to " can be wetting at once by aqueous water ".
Organic solvent in the step (1) for example is a dimethyl formamide, dimethylacetylamide, N-methyl pyrrolidone, dimethyl sulfoxide (DMSO), dioxane, or the mixture of above-mentioned organic solvent.The water soluble polymer additive is a polyethylene glycol, or other can form compatible water soluble polymer additive with engineering plastics or the macromolecular material that this patent invention is contained.Air wind speed in the step (2) after overregulating is 0.1 meter per second～7 meter per seconds, and contacting the processing time with solution is 10 seconds～20 minutes.Forming thing in the step (2) puts into sea water bath to carry out the final shaping unit processing time is 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, and is easy to operate, and the filter membrane of production has good filtering traffic and flux, and strainability is good.
The specific embodiment:
Get the macromolecular material polysulfones that meets hydrophobic material definition (or polyether sulfone, nylon 6, polyvinylidene fluoride, celluloid, cellulose mixture, poly-peptide, polyester), earlier through stirring and dissolving in the organic solvent of high polarity for example dimethyl formamide or dimethylacetylamide, N-methyl pyrrolidone, dimethyl sulfoxide (DMSO), dioxane, or the mixture of above-mentioned organic solvent, add polyethylene glycol or the similar additive of other water soluble polymers then through mixing.Aspect the formula concentration gross weight compares, macromolecular material accounts for 10% to 30% (example 10%, 20%, 30%), organic solvent accounts for 15% to 30% (example 15%, 23%, 30%), and polyethylene glycol or the similar additive of other water soluble polymers account for 40% to 75% (example 40%, 60%, 75%).After the solution preparation is finished, use coating cutter or additive method to comprise that method of radiation is coated in solution on the roller of continuous rolling uniformly, or on the conveyer belt of the metal that rotates continuously or other materials.Contact with solution at the stable air of sending after overregulating above the roller or above the conveyer belt, to carry out the phase transformation process.Air after overregulating must be adjusted into 40% to 95% relative humidity (example 40%, 70%, 95%), or dry-bulb temperature is 10 ℃ to 50 ℃ (10 ℃, 30 ℃, 50 ℃ of examples), or dew-point temperature is 10 ℃ to 50 ℃ (10 ℃, 30 ℃, 50 ℃ of examples), or the air wind speed after overregulating 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), also adjusts solution temperature simultaneously and be 10 ℃ to 50 ℃ (10 ℃, 30 ℃, 50 ℃ of examples) (method of adjustment is carried out for heating or freezing mode).After this preformed step is finished, time is between 10 seconds to 20 minutes (example 10 seconds, 10 minutes, 20 minutes), enter the sea water bath that water temperature is controlled at 5 ℃ to 50 ℃ (5 ℃, 25 ℃, 50 ℃ 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 porose semi-permeation filtering film.After porose semi-permeation filtering film creates, to peel off from roller or conveyer belt with mechanical system, filter membrane enters last handling process then, and 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% (gross weight ratio) aqueous acetone solution, or the mixture of isopropyl alcohol equal solvent or pure water cleaning or above-mentioned solvent.The solvent clean temperature is (10 ℃, 30 ℃, 60 ℃, 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 80 ℃ (25 ℃, 50 ℃, 80 ℃ of examples), and drying mode can be the formula of leaving standstill or blowing-type.The filter membrane of dry back as long as contain the remaining polyethylene glycol of 1% to 6% (finished film weight ratio), or other macromolecule additives water-soluble and can be compatible with the filter membrane raw material, promptly belongs to hydrophilic filter membrane and can be at once by water-wet.
Listed macromolecular material and corresponding water imbibition thereof in inspecting table one, demonstrate,proving routine result with above experiment compares, discovery have 2 with foreign patent that has authenticated at present or document in the phenomenon of record never, promptly be: first, the listed low macromolecule of water imbibition in the table one, the filter membrane that routine method manufactures is demonstrate,proved in experiment according to this patent invention statement, belongs to hydrophilic filter membrane and can be at once by water-wet unexpectedly.The second, the listed low similar macromolecule of several water imbibitions in the table one is demonstrate,proved the filter membrane that routine method manufactures according to the experiment of this patent invention statement, and distinct characteristic is arranged unexpectedly.These several macromolecules have comprised polyether sulfone and polyamide-imides at least.
In this patent invention, contained the macromolecule of main topic, promptly be polyether sulfone, its chemical structural formula summary
Listed polyether sulfone and two kinds of macromolecules of polysulfones of table one in this patent invention, in materials classification was learned, a class is often mentioned in the same breath and be classified as to these two kinds of macromolecules.Their chemical constitution and water imbibition are very similar, and all belong to hydrophobic polymer.Only demonstrate,prove the filter membrane that routine method manufactures through the listed experiment of this patent, the filter membrane of polyether sulfone is a hydrophily and can be at once by water-wet.On the contrary, the filter membrane of polysulfones then is a hydrophobicity, and can not be by water-wet.Significantly, whether hydrophilic or hydrophobic two kinds of high molecular characteristics of thin portion's difference be to make filter membrane decisive factor after qualitative these two kinds of Process Technologies of Polymer.The method of thin portion difference before this patent invention, never is mentioned or quoted, and this patent invention defines the method for using, and is one of basis of this patent invention.
Wherein 2 kinds of macromolecular materials that this patent invention is quoted are polyether sulfone and polyamide-imides.Remove this, other macromolecule additives, except polyethylene glycol, we have also found also can produce filter membrane possess hydrophilic property and can be at once by the characteristic of water-wet such as polyvinylpyrrolidone after adding.Moreover we have also found that the polysulfones filter membrane also might have hydrophilic and can be at once by the characteristic of water-wet if use a large amount of polyvinylpyrrolidones.
Also reported in this patent, added other additives, plasticiser for example also can produce hydrophilic and can be at once by the filter membrane of water-wet.This type of plasticiser embraces a wide spectrum of ideas, and only enumerates numerical example, such as ethylene glycol, and glycerine or the like.This type of plasticiser or additive also are included within this patent invention scope.
Polyether sulfone is contained in this patent invention or the polysulfones prescription mainly contains following several compositions: the first, and engineering plastics or macromolecular material, content be 12% (total weight parts) for example.The second, additive content is 68% (total weight parts) for example.The 3rd, solvent and additive content is 20% (total weight parts) for example.
Processing procedure and step are contained in this patent invention.Except comprising the laboratory or making by hand on a small quantity the flow process, main and emphasis is to have contained the continuous production procedure of pipeline system, is to aim at the flow process mode of batch process to answer commercialization to use.Its step evenly is tiled in solution on the continuity conveyer belt or roller surface for after at first preparing formula solution, uses scraper or other flatters (for example pushing the ejaculation formula), the thickness of control masking liquid.Then, this solution enters the pre-profiling process, meticulous control, and temperature, humidity, wind speed, pressure, with the holdup time, phase transformation (or phase transfer) process of finishing with stable forms initial filter membrane.After the initial filter membrane moulding, enter the post processing case again, stretch to carry out vertical variable speed or constant speed, typing is cleaned, and drying and other steps is with the semi-permeable filter membrane of the porous of finally making solid-state dull and stereotyped paper formula.
According to prescription and the flow process that this patent invention is revealed, the filter membrane average pore size that manufactures and belongs to hydrophilic filter membrane between 0.01 micron to 20 microns, and can be at once by water-wet.Utilize the produced filter membrane of this patent inventive method, and splendid semi-permeable filterability is arranged, and 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 filter membrane, filter membrane also can be again through high-temperature heat treatment, for example 150 ℃ to 250 ℃, improves the intensity of filter membrane once more.Other characteristics of filter membrane after excessive temperature is handled, for example too big variation can't take place in discharge steam bubble point 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.
Embodiment 1: make 0.2 micron hydrophilic polyethersulfone filter membrane
Part by weight with 13 to 18 to 69, the solid-state thing of polyether sulfone macromolecule and dimethyl formamide and polyethylene glycol-400 uniform dissolution with mix.Between 20 to 30 ℃ 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 porose semi-permeation filtering film at last.
With the filter membrane that this manufactured is come out, possess hydrophilic property and can be at once by the characteristic of water-wet.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, discharge is 28 seconds/100 ml pure water/9.62 square centimeter filter areas.
Embodiment 2: make 0.2 micron hydrophobicity polysulfones filter membrane
Except using polysulfones with the polyether sulfone used among the replacement embodiment 1, this polysulfones filter membrane manufacture method is identical with step described in the embodiment 1.The polysulfones filter membrane that manufacturing is come out is not had a hydrophily, and can't be wetting at once by water, is to belong to the hydrophobicity filter membrane.95% alcohol steam bubble point of this film is 2 kg/cm.After using 95% alcohol dampening in advance, survey its discharge, under 20 inches mmhg pressures, be 36 seconds/100 ml pure water/9.62 square centimeter filter areas.
Embodiment 3: make 0.1 micron hydrophilic polyethersulfone filter membrane
Part by weight with 15 to 18 to 66.5 to 0.5 is polyether sulfone solid-state polymer and dimethyl formamide and polyethylene glycol-400 and glycerine homogeneous solution and mix.The step of making this filter membrane is identical with described in the embodiment 1 basically.With the polyether sulfone filter membrane that this manufactured is come out, possess hydrophilic property and can be at once by the characteristic of water-wet, and the steam bubble point is arranged is 6.3 kg/cm.Discharge under 20 inches mmhg pressures is 84 seconds/100 ml pure water/9.62 square centimeter filter areas.
Claims (7)
1. the production method of a porose semi-permeation filtering film is characterized in that: comprise the following steps: successively
(1) will be when suction gas equalization point, suction gas is that 2%～4% polymeric solid material dissolves is in the organic solvent of high polarity, and add and to form compatible water soluble polymer additive with above-mentioned polymeric solid material, make uniform solution, the polymeric solid material accounts for 10% to 30% total weight parts in this solution, organic solvent accounts for 15% to 30% total weight parts, and the water soluble polymer additive accounts for 40% to 75% total weight parts;
(2) above-mentioned solution temperature is transferred be made as 10～50 ℃ after, be tiled on the roller or conveyer belt of continuous rotation, to regulate back relative humidity is 40%～95%, dry-bulb temperature is 10～50 ℃, dew-point temperature is that 10～50 ℃ air contacts with solution, to put into 5～50 ℃ 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 25～80 ℃, carry out drying then, get product through cleaning agent.
2. the production method of porose semi-permeation filtering film according to claim 1 is characterized in that: the polymeric solid material in the step (1) is polysulfones, polyether sulfone, nylon 6, polyvinylidene fluoride, celluloid, cellulose mixture, poly-peptide or polyester.
3. the production method of porose semi-permeation filtering film according to claim 1, it is characterized in that: the organic solvent in the step (1) is dimethyl formamide, dimethylacetylamide, N-methyl pyrrolidone, dimethyl sulfoxide (DMSO), dioxane, or the mixture of above-mentioned organic solvent.
4. the production method of porose semi-permeation filtering film according to claim 1, it is characterized in that: the water soluble polymer additive in the step (1) is a polyethylene glycol, or other can form compatible water soluble polymer additive with polymeric solid material according to claim 2.
5. the production method of porose semi-permeation filtering film 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, contacting the processing time with solution is 10 seconds～20 minutes.
6. the production method of porose semi-permeation filtering film according to claim 1 is characterized in that: form thing in the step (2) and put into sea water bath to carry out the final shaping unit processing time be 10 seconds～30 minutes.
7. the production method of porose semi-permeation filtering film 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 alcohols 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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| CNB2006100233613A CN100386136C (en) | 2006-01-17 | 2006-01-17 | Method for producing porose semi-permeation filtering film |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101219350B (en) * | 2007-10-11 | 2010-06-02 | 亚美滤膜（南通）有限公司 | Method for producing hydrophilic polyethersulfone millipore filter |
| CN103372380B (en) * | 2012-04-28 | 2015-03-25 | 亚美滤膜（南通）有限公司 | Preparation method of hydrophobic polyvinylidene difluoride microporous filter membrane |
| CN103418253A (en) * | 2012-05-16 | 2013-12-04 | 亚美滤膜（南通）有限公司 | Nitrocellulose microporous filtration membrane production process |
| CN103865090B (en) * | 2014-03-14 | 2016-04-27 | 山东理工大学 | A kind of method that polycaprolactone and polyoxyethylene glycol improve poly-peptide film wetting ability |
| CN106178971A (en) * | 2016-08-18 | 2016-12-07 | 嘉兴德永纺织品有限公司 | The manufacture method of wet method micro-porous film |
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