CN102580559A - Hydrophilic single skin layer tubular high polymer porous membrane - Google Patents
Hydrophilic single skin layer tubular high polymer porous membrane Download PDFInfo
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- CN102580559A CN102580559A CN2012100448837A CN201210044883A CN102580559A CN 102580559 A CN102580559 A CN 102580559A CN 2012100448837 A CN2012100448837 A CN 2012100448837A CN 201210044883 A CN201210044883 A CN 201210044883A CN 102580559 A CN102580559 A CN 102580559A
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Abstract
The invention discloses a hydrophilic single skin layer tubular high polymer porous membrane, belonging to the tubular high polymer porous membrane. The porous membrane comprises an enhanced porous support pipe, wherein a high polymer porous layer is compounded on the inner wall of the enhanced porous support pipe, and a hydrophilic crosslinking polymer layer is arranged on the high polymer porous layer. Hydrolysis and crosslinking soaking are performed to the high polymer porous membrane with cellulose diacetate to form a hydrophilic single skin layer structure, thus the anti-pollution performance of the porous membrane is greatly increased. The separation performance of the hydrophilic single skin layer tubular high polymer porous membrane is not lower than that of the existing high polymer porous membrane and the preparation method is easier. The tubular high polymer porous membrane can be widely applied.
Description
Technical field
The present invention relates to the high-molecular porous film of a kind of tubular type, specifically be meant a kind of high-molecular porous film of tubular type with hydrophilic single skin structure.
Background technology
Membrane separation technique is a kind of efficient, energy-conservation green new separation technology; Have outstanding features such as equipment is simple, operating condition is gentle, treating capacity is big, separative efficiency height; Separate with resource, biological products with brackish water desalination, wastewater treatment at seawater, field such as environmental project, drink water purifying, air filtration and purification, material concentrating and separating is used widely, and obtained good economic and social benefit.
High-molecular porous film can be divided into micro-filtration membrane, milipore filter and NF membrane as one big type of diffusion barrier according to its pore size.Different according to the macromolecular material source, can divide for by the high-molecular porous film of natural macromolecular material preparation and the high-molecular porous film for preparing by synthetic polymer.Natural macromolecular material is mainly cellulose acetate and derivative thereof, and synthetic polymer then kind is more relatively, mainly comprises polysulfones synthetic polymer, polyamide-based synthetic polymer, polyesters synthetic polymer, TPO synthetic polymer etc.High-molecular porous film is different according to the preparation method, can be divided into be separated perforated membrane and dissolve and cause the perforated membrane that is separated of stretchable porous film, thermic again; Can be divided into dull and stereotyped high-molecular porous film, hollow fiber polymer perforated membrane and tubular high polymer perforated membrane according to profile.Different high-molecular porous films according to differences such as its aperture, materials, has different purposes.
High-molecular porous film in use; Usually can be polluted by the organic or inorganic pollutant in the material; As when handling waste water, the surface that magazines such as the bacterium in the waste water, virus, organic matter and colloid can adsorb, be deposited on high-molecular porous film forms colloid pollution and biological pollution; The permeation flux of high-molecular porous film is descended, and treatment effeciency reduces.Especially when handling high pollution property material, will cause shortening in service life, operating cost increase, the operational efficiency of diffusion barrier to reduce.
Most of high-molecular porous films are slab construction or doughnut structure at present, and have been widely used, still; The high-molecular porous film of flat board or doughnut structure in use; Polluted by material easily, high to the preliminary treatment requirement of material, and be not suitable for processing high pollution fluid.
Summary of the invention
The technical issues that need to address of the present invention just are to overcome the defective of prior art, provide a kind of hydrophilic single skin tubular type high-molecular porous film, and it can improve the antifouling property of high-molecular porous film, prolongs the service life of high-molecular porous film.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides the high-molecular porous film of a kind of hydrophilic single skin tubular type, strengthen the porous tubular support inwall and be compounded with the high-molecular porous layer of one deck, on high-molecular porous layer, one deck hydrophilic crosslinked polymer layer is arranged.
As preferably, the above-mentioned high-molecular porous film of hydrophilic single skin tubular type, described enhancing porous tubular support is a three-decker, comprises inner compact layer nonwoven, middle nylon reinforcements layer and outer nonwoven; Wherein the grammes per square metre of inner compact layer nonwoven is 50-100g/m
2
As preferably, the above-mentioned high-molecular porous film of hydrophilic single skin tubular type, described high-molecular porous layer forms by being coated in the Polymer Solution gel in the aqueous solution that strengthens the porous tubular support inner surface; Wherein Polymer Solution is made up of macromolecular material, solvent and additive, and gel water pH value of solution is 8.0-11.0.
As preferably, the above-mentioned high-molecular porous film of hydrophilic single skin tubular type, described macromolecular material is the polymer poly vinylidene; Or polysulfones; Polyether sulfone, or polyacrylonitrile, or the mixture of polyvinyl chloride and cellulose diacetate, wherein the mass ratio of cellulose diacetate is 0.5-10.0%.
As preferably, the above-mentioned high-molecular porous film of hydrophilic single skin tubular type, described hydrophilic crosslinked polymer layer are to soak in containing the aqueous solution of crosslinking agent through high-molecular porous layer, dry then to make; Wherein crosslinking agent is glutaraldehyde, Polyethylene Glycol Bisglycidyl Ether, sorbierite, inositol or their mixture; The mass concentration of crosslinking agent is 0.01-10.0wt%, and aqueous solution pH is 1.0-7.0, and soak time is 0.5-60 minute, and drying temperature is 20-60 ℃.As more preferably selecting, the mass concentration of described crosslinking agent is 0.05-5.0wt%, and pH value of solution is 1.0-5.0, and soak time is 1.0-30 minute.
The Polymer Solution preparation method is: be dissolved in the polar organic solvent preparation Polymer Solution with the macromolecular material of 10.0-35.0wt% and the additive of 0.5-15.0wt%; Wherein, polar organic solvent is N, N-dimethylacetylamide, or N, dinethylformamide, or N-methyl pyrrolidone, or their mixture; Additive is a PEG400, or PVP, or lithium chloride, or their mixture; Macromolecular material is the polymer poly vinylidene, or polysulfones, or polyether sulfone, or polyacrylonitrile, or polyvinyl chloride, and with the mixture of cellulose diacetate, wherein the mass ratio of cellulose diacetate is 0.5-10.0%.
Said hydrophilic single skin tubular porous membrane preparation method is: adopt the synchronous forming technology; When preparation contains the enhancing porous tubular support of three-decker of inner compact layer nonwoven, middle nylon reinforcements layer and outer nonwoven, the Polymer Solution of preparation evenly is coated to the inner surface that strengthens antipriming pipe; The above-mentioned enhancing porous tubular support that scribbles Polymer Solution stops 30-300s in air after, be immersed in the aqueous solution that pH is 8.0-11.0, in the aqueous solution, stop after 30-60 minute, remove and use the pure water rinsing; Then, the pbz polymer porous layer that above-mentioned gel is obtained be immersed in contain the 0.01-10.0wt% crosslinking agent, pH is in the aqueous solution of 1.0-7.0, soak time is 0.5-60 minute; At last, under 20-60 ℃, dry, can obtain hydrophilic single skin tubular porous membrane.Wherein crosslinking agent is a glutaraldehyde, or Polyethylene Glycol Bisglycidyl Ether, or sorbierite, or inositol, or their mixture.
The high-molecular porous film of tubular type then has advantages such as excellent, the easy cleaning of the stifled performance of anti-soil.In addition, through hydrophily and the optimization membrane structure that improves high-molecular porous membrane material, can further improve the separation and the serviceability of macromolecule tubular type perforated membrane.
Thereby, the invention has the beneficial effects as follows:
The present invention is through being hydrolyzed and crosslinked immersion treatment to the high-molecular porous film that contains cellulose diacetate; Not only make the hydrophilicity of high-molecular porous film be greatly enhanced; Has good antifouling property; Form the single skin structure on high-molecular porous film surface simultaneously, make high-molecular porous film have the stifled performance of better anti-soil.The separating property of the high-molecular porous film of hydrophilic single skin tubular type of the present invention is not less than existing high-molecular porous film, and the preparation method is also simpler.
The specific embodiment
The Polymer Solution preparation:
The present invention is that the additive with the macromolecular material of 10.0-35.0wt% and 0.5-15.0wt% is dissolved in the polar organic solvent, the preparation Polymer Solution.Wherein, polar organic solvent is N, N-dimethylacetylamide, or N, dinethylformamide, or N-methyl pyrrolidone, or their mixture; Additive is a PEG400, or PVP, or lithium chloride, or their mixture; Macromolecular material is the polymer poly vinylidene, or polysulfones, or polyether sulfone, or polyacrylonitrile, or polyvinyl chloride, and with the mixture of cellulose diacetate, wherein the mass ratio of cellulose diacetate is 0.5-10.0%.
Hydrophilic single skin tubular porous membrane preparation:
Employing synchronous forming technology when preparation contains the enhancing porous tubular support of three-decker of inner compact layer nonwoven, middle nylon reinforcements layer and outer nonwoven, evenly is coated to the inner surface that strengthens antipriming pipe with the Polymer Solution of above-mentioned preparation; The above-mentioned enhancing porous tubular support that scribbles Polymer Solution stops 30-300s in air after, be immersed in the aqueous solution that pH is 8.0-11.0, in the aqueous solution, stop after 30-60 minute, remove and use the pure water rinsing; Then, the pbz polymer porous layer that above-mentioned gel is obtained be immersed in contain the 0.01-10.0wt% crosslinking agent, pH is in the aqueous solution of 1.0-7.0, soak time is 0.5-60 minute; At last, under 20-60 ℃, dry, can obtain hydrophilic single skin tubular porous membrane.Wherein crosslinking agent is a glutaraldehyde, or Polyethylene Glycol Bisglycidyl Ether, or sorbierite, or inositol, or their mixture.
The perforated membrane performance test:
The molecular cut off (MWCO) of the pure water permeation flux of the main evaluated for film of tubular porous membrane performance test and film.
Adopt the cross-flow permeability test, as charging, under 25 ℃, 0.1MPa, see through the volume (V) of the water of elementary membrane area (A) in the analytical unit time (t) with pure water, can obtain the pure water permeation flux (F) of tubular porous membrane, its unit is l/m
2.h, concrete computing formula is following:
Employing cross-flow test is charging with different molecular weight polyethylene glycol (PEG) aqueous solution of 50mg/l, under 25 ℃, 0.1MPa, measures the rejection (R) of film to the PEG of different molecular weight, rejection be defined as feeding liquid PEG concentration (C
f) with penetrating fluid in PEG concentration (C
p) poor, again divided by feeding liquid PEG concentration.Concrete computing formula is following:
The film rejection is the molecular cut off that 90% pairing PEG molecular weight is film, and unit is g/mol.
Embodiment 1-5
With lithium chloride and PEG400 (PEG400) is additive, and with N, the N-dimethylacetylamide is a solvent; Adopting different polymer (is Kynoar; Or polysulfones, or polyether sulfone, or polyacrylonitrile; Or polyvinyl chloride) with the mixture (mass ratio of cellulose diacetate is 5.0%) of cellulose diacetate as macromolecular material, the preparation Polymer Solution; Wherein, the content of macromolecular material is that 20.0wt%, lithium chloride content are that 0.5wt%, PEG400 content are 10.0wt% in the Polymer Solution.
Employing synchronous forming technology, preparation contains the enhancing porous tubular support of the three-decker of inner compact layer nonwoven, middle nylon reinforcements layer and outer nonwoven, the Polymer Solution of above-mentioned preparation evenly is coated to the inner surface of enhancing antipriming pipe; The above-mentioned enhancing porous tubular support that scribbles Polymer Solution stops 120s in air after, be immersed in pH and be in 10.0 the aqueous solution, gel was removed and is also used the pure water rinsing after 60 minutes in the aqueous solution; Then, the pbz polymer porous layer that above-mentioned gel is obtained is that soak time is 20 minutes in 4.5 the aqueous solution containing 0.1wt% glutaraldehyde, pH; Under 30 ℃, dry at last, can obtain hydrophilic single skin tubular porous membrane.Measure the pure water flux and the molecular cut off (MWCO) of the prepared high-molecular porous film of tubular type, the result sees table 1.These several embodiment are performances of investigating the prepared tubular membrane of macromolecular material that various polymerization thing and cellulose diacetate form.
Table 1: embodiment 1-5
Embodiment 6-10
Except being used for preparing the mass ratio difference of the used macromolecular material cellulose diacetate of Polymer Solution; Adopt and prepare the high-molecular porous film of tubular type with embodiment 1 identical method; Measure the pure water flux and the molecular cut off of the prepared high-molecular porous film of tubular type, the result sees table 2.These several embodiment are performances of investigating the prepared tubular membrane of different cellulose diacetate mass ratios.
Table 2: embodiment 6-10
Above-mentioned instance shows: have the forward proportionate relationship between cellulose diacetate mass ratio and membrane flux and the molecular cut off.
Embodiment 11-13
Except the pH difference of Polymer Solution gel solution, adopt to prepare the high-molecular porous film of tubular type with embodiment 1 identical method, measure the pure water flux and the molecular cut off of the prepared high-molecular porous film of tubular type, the result sees table 3.These several embodiment investigate to adopt the different pH aqueous solution Polymer Solution to be carried out the performance of the high-molecular porous film of gel gained tubular type.
Table 3: embodiment 11-13
Above-mentioned instance shows: have the forward proportionate relationship between gel solution pH and membrane flux and the molecular cut off.
Embodiment 14-18
In the aqueous solution that high-molecular porous layer is carried out after-treatment the contained crosslinking agent difference; Adopt and prepare the high-molecular porous film of tubular type with embodiment 3 identical methods; Measure the pure water flux and the molecular cut off of the prepared high-molecular porous film of tubular type, the result sees table 4.These several embodiment investigate to adopt different crosslinking agents high-molecular porous layer to be carried out the performance of the high-molecular porous film of after-treatment gained tubular type.
Table 4: embodiment 14-18
Embodiment 19-23
In the aqueous solution that high-molecular porous layer is carried out after-treatment the glutaraldehyde concentration difference; Adopt and prepare the high-molecular porous film of tubular type with embodiment 3 identical methods; Measure the pure water flux and the molecular cut off of the prepared high-molecular porous film of tubular type, the result sees table 5.These several embodiment investigate to adopt the glutaraldehyde water solution that contains variable concentrations high-molecular porous layer to be carried out the performance of the high-molecular porous film of after-treatment gained tubular type.
Table 5: embodiment 19-23
Above-mentioned instance shows: best with glutaraldehyde content resulting high-molecular porous film properties between 0.05-5.0wt%.
Embodiment 24-27
Except the pH difference of the glutaraldehyde water solution that high-molecular porous layer carried out after-treatment; Adopt and prepare the high-molecular porous film of tubular type with embodiment 5 identical methods; Measure the pure water flux and the molecular cut off of the prepared high-molecular porous film of tubular type, the result sees table 6.These several embodiment investigate to adopt the glutaraldehyde water solution that contains variable concentrations high-molecular porous layer to be carried out the performance of the high-molecular porous film of after-treatment gained tubular type.
Table 6: embodiment 24-27
Above-mentioned instance shows: best with glutaraldehyde water solution pH resulting high-molecular porous film properties between 1.0-5.0.
Embodiment 28-34
Except high-molecular porous layer is carried out the asynchronism(-nization) of glutaraldehyde water solution immersion treatment; Adopt and prepare the high-molecular porous film of tubular type with embodiment 2 identical methods; Measure the pure water flux and the molecular cut off of the prepared high-molecular porous film of tubular type, the result sees table 7.These several embodiment investigate to adopt the glutaraldehyde water solution that contains variable concentrations high-molecular porous layer to be carried out the performance of the high-molecular porous film of after-treatment gained tubular type.
Table 7: embodiment 28-34
Above-mentioned instance shows: best with glutaraldehyde water solution immersion treatment time resulting high-molecular porous film properties between 1.0-30.0 minute.
What should explain at last is: obviously, the foregoing description only be for clearly the present invention is described and is done for example, and be not qualification to embodiment.For the those of ordinary skill in affiliated field, on the basis of above-mentioned explanation, can also make other multi-form variation or change.Here need not also can't give exhaustive to all embodiments.And conspicuous variation of being amplified out thus or change still are among protection scope of the present invention.
Claims (8)
1. high-molecular porous film of hydrophilic single skin tubular type; It is characterized in that; The high-molecular porous film of said hydrophilic single skin tubular type comprises the enhancing porous tubular support, strengthens the porous tubular support inwall and is compounded with the high-molecular porous layer of one deck, on high-molecular porous layer, one deck hydrophilic crosslinked polymer layer is arranged.
2. the high-molecular porous film of a kind of hydrophilic single skin tubular type as claimed in claim 1, it is characterized in that: described enhancing porous tubular support is a three-decker, comprises inner compact layer nonwoven, middle nylon reinforcements layer and outer nonwoven; Wherein, the proportion of inner compact layer nonwoven is 50-100g/m
2
3. the high-molecular porous film of a kind of hydrophilic single skin tubular type as claimed in claim 1 is characterized in that: described high-molecular porous layer forms by being coated in the Polymer Solution gel in the aqueous solution that strengthens the porous tubular support inner surface; Wherein Polymer Solution is made up of macromolecular material, solvent and additive; Gel water pH value of solution is 8.0-11.0.
4. the high-molecular porous film of a kind of hydrophilic single skin tubular type as claimed in claim 3; It is characterized in that: described macromolecular material is the polymer poly vinylidene; Or polysulfones, or polyether sulfone, or polyacrylonitrile; Or the mixture of polyvinyl chloride and cellulose diacetate, wherein the mass ratio of cellulose diacetate is 0.5-10.0%.
5. the high-molecular porous film of a kind of hydrophilic single skin tubular type as claimed in claim 1 is characterized in that: described hydrophilic crosslinked polymer layer is to soak in containing the aqueous solution of crosslinking agent through high-molecular porous layer, dries then to make; Wherein crosslinking agent is glutaraldehyde, Polyethylene Glycol Bisglycidyl Ether, sorbierite, inositol or their mixture; The mass concentration of crosslinking agent is 0.01-10.0wt%, and aqueous solution pH is 1.0-7.0, and soak time is 0.5-60 minute, and drying temperature is 20-60 ℃.
6. the high-molecular porous film of a kind of hydrophilic single skin tubular type as claimed in claim 5, it is characterized in that: the mass concentration of described crosslinking agent is 0.05-5.0wt%, and pH value of solution is 1.0-5.0, and soak time is 1.0-30 minute.
7. like the high-molecular porous film of arbitrary described a kind of hydrophilic single skin tubular type of claim 1-6, it is characterized in that the Polymer Solution preparation method is:
Be dissolved in the polar organic solvent preparation Polymer Solution with the macromolecular material of 10.0-35.0wt% and the additive of 0.5-15.0wt%; Wherein, polar organic solvent is N, N-dimethylacetylamide, or N, dinethylformamide, or N-methyl pyrrolidone, or their mixture; Additive is a PEG400, or PVP, or lithium chloride, or their mixture; Macromolecular material is the polymer poly vinylidene, or polysulfones, or polyether sulfone, or polyacrylonitrile, or polyvinyl chloride, and with the mixture of cellulose diacetate, wherein the mass ratio of cellulose diacetate is 0.5-10.0%.
8. the high-molecular porous film of a kind of hydrophilic single skin tubular type as claimed in claim 7 is characterized in that, said hydrophilic single skin tubular porous membrane preparation method is:
Employing synchronous forming technology when preparation contains the enhancing porous tubular support of three-decker of inner compact layer nonwoven, middle nylon reinforcements layer and outer nonwoven, evenly is coated to the inner surface that strengthens antipriming pipe with the Polymer Solution of preparation; The above-mentioned enhancing porous tubular support that scribbles Polymer Solution stops 30-300s in air after, be immersed in the aqueous solution that pH is 8.0-11.0, in the aqueous solution, stop after 30-60 minute, remove and use the pure water rinsing; Then, the pbz polymer porous layer that above-mentioned gel is obtained be immersed in contain the 0.01-10.0wt% crosslinking agent, pH is in the aqueous solution of 1.0-7.0, soak time is 0.5-60 minute; At last, under 20-60 ℃, dry, can obtain hydrophilic single skin tubular porous membrane.Wherein crosslinking agent is a glutaraldehyde, or Polyethylene Glycol Bisglycidyl Ether, or sorbierite, or inositol, or their mixture.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103551054A (en) * | 2013-11-14 | 2014-02-05 | 中科瑞阳膜技术（北京）有限公司 | Ultrafiltration membrane and preparation method thereof |
| CN104689729A (en) * | 2015-03-24 | 2015-06-10 | 广州市恩德氏医疗制品实业有限公司 | Polysulfon group and cellulose acetate blended hollow fiber membrane fluid, preparing method thereof and hollow fiber membrane made from the same |
| CN108698819A (en) * | 2016-01-05 | 2018-10-23 | myFC 股份公司 | Distribution of the reactant solution in fuel cassette |
| CN110080006A (en) * | 2019-05-31 | 2019-08-02 | 南通东屹高新纤维科技有限公司 | The preparation method of waterproof composite fabric |
| CN110158324A (en) * | 2019-05-31 | 2019-08-23 | 南通东屹高新纤维科技有限公司 | Super-hydrophobic linen-cotton textile fabric |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103551054A (en) * | 2013-11-14 | 2014-02-05 | 中科瑞阳膜技术（北京）有限公司 | Ultrafiltration membrane and preparation method thereof |
| CN103551054B (en) * | 2013-11-14 | 2015-11-25 | 中科瑞阳膜技术（北京）有限公司 | A kind of milipore filter and preparation method thereof |
| CN104689729A (en) * | 2015-03-24 | 2015-06-10 | 广州市恩德氏医疗制品实业有限公司 | Polysulfon group and cellulose acetate blended hollow fiber membrane fluid, preparing method thereof and hollow fiber membrane made from the same |
| CN104689729B (en) * | 2015-03-24 | 2017-01-11 | 广州市恩德氏医疗制品实业有限公司 | Polysulfon group and cellulose acetate blended hollow fiber membrane fluid, preparing method thereof and hollow fiber membrane made from the same |
| CN108698819A (en) * | 2016-01-05 | 2018-10-23 | myFC 股份公司 | Distribution of the reactant solution in fuel cassette |
| CN110080006A (en) * | 2019-05-31 | 2019-08-02 | 南通东屹高新纤维科技有限公司 | The preparation method of waterproof composite fabric |
| CN110158324A (en) * | 2019-05-31 | 2019-08-23 | 南通东屹高新纤维科技有限公司 | Super-hydrophobic linen-cotton textile fabric |
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Application publication date: 20120718 |