CN101011645A - Method for hydrophilic modification of polypropylene porous membrane surface by using amphipathic molecule - Google Patents
Method for hydrophilic modification of polypropylene porous membrane surface by using amphipathic molecule Download PDFInfo
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- CN101011645A CN101011645A CN 200610161542 CN200610161542A CN101011645A CN 101011645 A CN101011645 A CN 101011645A CN 200610161542 CN200610161542 CN 200610161542 CN 200610161542 A CN200610161542 A CN 200610161542A CN 101011645 A CN101011645 A CN 101011645A
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Abstract
The invention discloses a molecular structure of surface modifier and modifying method, which is characterized by the following: adopting amphipathic molecule with block structure as hydrophilic modifier; immersing porous polypropylene film in the swelling agent with amphipathic molecule and photosensitive initiator; deswelling the surface in the vacuum based on amphipathic molecule with block structure as surface disposer; providing 'anchoring' action for polypropylene molecular chain; conferring hydrophilicity for porous polypropylene film surface.
Description
Technical field
The present invention relates to a kind of method of modifying of polypropylene porous membrane surface, more specifically to the hydrophilic modification method of a kind of amphipathic molecule to polypropylene porous membrane surface.
Background technology
Advantages such as membrane separation technique has low energy consumption, process is simple, separative efficiency is high, free from environmental pollution are the important new and high technologies that solves the energy, resource and the environmental problem in the present age.Membrane separation technique develops rapidly over nearly 20 years, and it uses the fields such as chemical industry, food, medicine, biochemistry, environmental protection of having developed into.Polymer is one of important material of preparing because of its function admirable, inexpensive and workability.The polyvinyl polypropylene (PP) of hemicrystalline, high density polyethylene (HDPE) (HDPE) and polyvinylidene fluoride (PVDF) etc. are as raw material, with methods such as fusion drawn and thermal induction are separated, have been prepared to the high porosity perforated membrane and are applied.But because above-mentioned polyvinyl material is a low pole, the porous film surface that makes has hydrophobicity.Because the relation of surface energy, water is difficult for seeing through the micro channel of hydrophobic film; Because hydrophobic interaction, hydrophobic film also is vulnerable to the pollution and the non-easy cleaning of protein etc., causes the membrane separating property deterioration.These effects limit the application of film in moisture such as biology, food, water treatment exsomatize system.The some effective that overcomes the above problems is that porous film surface is carried out hydrophilic modification.
The hydrophilic modification method of polymer porous film can be divided into physical modification method and chemic modified method, and as material blend, surface-coated, surface chemistry oxidation, surface plasma processing etc., they respectively have characteristics.With blend system films such as hydrophilic polymer and PP, HDPE or PVDF, can give porous film surface lasting hydrophily, shortcoming is to readjust system film parameter, technical process is complicated.Select for use hydrophilic material such as coating, surfactant etc. that porous film surface is applied, method is simple, but coated substance is easily polluted separation system by wash-out.Need when handling with chemical oxidization method with strong oxidizers such as chromate, the hydrophily that the film surface obtains has ageing, the surface texture of simultaneous oxidation effect meeting damage film, and heavy metal ion also can be brought environmental issue.The low-temperature plasma body method is a development in recent years method faster, but a few days ago rest on the basic research stages that the small size film is handled, the uniformity of its processing, to the structure control of handling the film surface, the problems such as treatment effect of fenestra inwall are also needed further research more.The polymer porous film that how to make things convenient for, prepare effectively surface hydrophilicity is the important topic of scientific research circle and industrial circle.
1991, (Biomaterials, 12,144～153,1991 such as Desai; Macromolecules, 25,226～232,1992) with polyethylene glycol (PEG) as surface conditioning agent, polyester (PET) material has been made performing hydrophilic modification on surface, " surperficial interact network method " process of surface treatment has been proposed.At first with the surface of mixed solvent (trifluoroacetic acid/water) the swelling PET that can control degree of swelling, make PEG in the sweller enter swollen region and with the strand generation winding effect of PET; Carry out deswelling with non-solvent water then and handle, the PEG strand is fixed in rapid contraction of PET strand as a result and embedding.Studies show that it is dark that the PEG strand can be invaded pet sheet face 5～10nm, after the PEG of molecular weight 18500 modification, the contact angle of pet sheet face has dropped to 20 °.Yet since selected for use with the bad PEG of PET compatibility as surface conditioning agent, cause surface treatment effect very responsive to the molecular weight of PEG.The molecular weight of PEG is too little then not enough with the winding of PET strand; The too big then PEG of molecular weight is difficult for entering the surperficial swelling zone of PET.The reliability of this process of surface treatment of Desai is not high simultaneously, and result's reappearance is bad.This is that surface conditioning agent easily is extracted out with sweller because in the deswelling process of non-solvent.But contradiction is for PEG and the bad system of this compatibility of PET, must take the quick deswelling mode of this non-solvent extraction, otherwise owing to phase separation, the PEG strand to be squeezed the surface of PET easily.
This impregnation process technology of Desai is suitable for the surface treatment of this multi-pore structure of polymer porous film, therefore be necessary to redesign the molecular structure of surface modifier, improve process of surface treatment simultaneously, to improve the reliability and the surface modification effect of process of surface treatment, the outer surface and the uniform hydrophily of fenestra inwall of giving polymer porous film.
Summary of the invention
The invention solves deficiency and problem that above-mentioned prior art exists, the molecular structure by the redesign surface modifier improves process of surface treatment simultaneously, and the hydrophilic modification method of a kind of amphipathic molecule to polypropylene porous membrane surface is provided.This method mainly is to carry out embedding and hydrophilic modification with amphiphile, amphiphilic molecule on the surface of polypropylene porous film, and the impregnation technology of employing can be given the outer surface and the uniform hydrophily of fenestra inwall of polypropylene porous film.
The present invention is achieved by the following technical solutions:
Amphipathic molecule of the present invention is to the hydrophilic modification method of polypropylene porous membrane surface, it is characterized in that this method is that amphipathic molecule with block structure is as the hydrophilic modifying agent, earlier polypropylene porous film be impregnated in and carry out surface treatment in the sweller that is dissolved with amphipathic molecule, carry out surperficial deswelling with the method for vacuum extraction sweller at last.For this semicrystalline polymeric of polypropylene, add control to the sweller swelling behavior, can limit the shallow surface of swelling zone in polypropylene material.Because the hydrophobic side and the polyacrylic compatibility of amphipathic molecule are good, the effect of " grappling " easily is provided with the polypropylene molecule chain combination of surperficial swollen region, promptly fixed after the deswelling by embedding.Its water-wet side and polyacrylic compatibility are bad, the result be separated or the effect of orientation etc. under, water-wet side stretches to the outside on film surface, has realized the hydrophilicity-imparting treatment of polypropylene porous membrane surface.The impregnation technology that adopts can make the outer surface of polypropylene screen perforated membrane and fenestra inwall obtain uniform hydrophilic modification.
Amphipathic molecule of the present invention may further comprise the steps the hydrophilic modification method of polypropylene porous membrane surface:
1) uses acetone prerinse polypropylene porous film 24 hours;
2) amphipathic molecule is dissolved in to be made into concentration expressed in percentage by weight in the sweller be 5～10% amphipathic molecule solution;
3) polypropylene porous film being dropped into temperature is to carry out surface treatment in 50～70 ℃ the solution of amphipathic molecule, after 60～720 minutes, takes out polypropylene porous film, vacuum extraction sweller and dry 24～48 hours;
4) take out dried polypropylene porous film, be soaked in water, clean the amphipathic molecule of the simple absorption of polypropylene porous membrane surface.
In the hydrophilic modification method of above-mentioned amphipathic molecule to polypropylene porous membrane surface, described amphipathic molecule is that molecular weight is 400～2000 18 pure polyglycol ethers, polyvinyl alcohol graft copolymerized polypropylene wax or Tissuemat E, polyacrylic acid grafted polypropylene wax or Tissuemat E, and the degree of polymerization of preferred polyalkylene glycol moiety is 8 18 pure polyglycol ethers.
In the hydrophilic modification method of above-mentioned amphipathic molecule to polypropylene porous membrane surface, its described sweller is a carbon tetrachloride, 1,2-dichloroethanes, dimethylbenzene/cyclohexanone mixed solvent or naphthane, preferred its weight proportion of wherein said dimethylbenzene/cyclohexanone mixed solvent is 90/10～60/40.
Amphipathic molecule of the present invention is to the hydrophilic modification method of polypropylene porous membrane surface, and its used polypropylene porous film is preferably polypropylene hollow fiber membrane.
The present invention has following beneficial effect:
1) employing has the close and distant water amphipathic molecule of block structure as surface conditioning agent, wherein hydrophobic segment and polyacrylic compatibility are better, the effect of " grappling " easily is provided with the polypropylene molecule chain combination of surperficial swollen region, hydrophilic segment is owing to being separated or the outside on film surface is stretched in the orientation effect, and gives the hydrophily of polypropylene porous membrane surface.
2) because the compatibility of the hydrophobic section of amphipathic molecule and carrier polymer is good, the two is difficult for being separated, therefore less demanding to deswelling speed, so can adopt vacuum drying as the deswelling means, the surface modifier of having avoided non-solvent deswelling method easily to cause is extracted out, causes the unsettled shortcoming of modified effect.
3) because polypropylene is a semicrystalline polymeric, unformed area is easily by solvation and crystal region is difficult for, again by regulating conditions such as sweller composition, swelling temperature, swelling time, can make swelling action only be confined to the shallow surf zone of polypropylene material, therefore destroy faint the pore structure of polypropylene porous film.
4) dipping method of the present invention is particularly suitable for the surface modification of this porous structure material of diffusion barrier, and sweller can go deep into the fenestra depths, makes the outer surface of perforated membrane and fenestra inwall all can access uniform hydrophilic modification.
5) processing method of the present invention and technology are simple, and treatment effect is reliable, need not complex apparatus, are suitable for the plant-scale surface treatment of polymer porous film.
The specific embodiment
Further specify the present invention by the following examples:
Embodiment 1
1) uses acetone prerinse polypropylene hollow fiber membrane 24 hours;
2) be that 8 18 pure polyglycol ethers are dissolved in the carbon tetrachloride with the polyethylene glycol section degree of polymerization, be made into concentration expressed in percentage by weight and be 5% amphipathic molecule swelling solution;
3) swelling solution constant temperature drops into and carries out surface treatment through the pretreated polypropylene hollow fiber membrane of step 1 at 50 ℃, after 60 minutes, takes out polypropylene hollow fiber membrane, blots the solution of surface absorption, vacuum extraction sweller also dry 24 hours;
4) take out dried polypropylene hollow fiber membrane, be soaked in water and clean the amphipathic molecule of the simple absorption in polypropylene screen surface.The performance of the polypropylene hollow fiber membrane of surface modification sees the following form 1.
Embodiment 2
1) uses acetone prerinse polypropylene hollow fiber membrane 24 hours;
2) be that 8 18 pure polyglycol ethers are dissolved in the carbon tetrachloride with the polyethylene glycol section degree of polymerization, be made into concentration expressed in percentage by weight and be 10% amphipathic molecule swelling solution;
3) swelling solution constant temperature drops into and carries out surface treatment through the pretreated polypropylene hollow fiber membrane of step 1 at 65 ℃, after 360 minutes, takes out polypropylene hollow fiber membrane, blots the solution of surface absorption, vacuum extraction sweller also dry 48 hours;
4) take out dried polypropylene hollow fiber membrane, be soaked in water and clean the amphipathic molecule of the simple absorption in polypropylene screen surface.The performance of the polypropylene hollow fiber membrane of surface modification sees the following form 1.
Embodiment 3
1) uses acetone prerinse polypropylene hollow fiber membrane 24 hours;
2) be that 8 18 pure polyglycol ethers are dissolved in the carbon tetrachloride with the polyethylene glycol section degree of polymerization, be made into concentration expressed in percentage by weight and be 10% amphipathic molecule swelling solution;
3) swelling solution constant temperature drops into and carries out surface treatment through the pretreated polypropylene hollow fiber membrane of step 1 at 70 ℃, after 720 minutes, takes out polypropylene hollow fiber membrane, blots the solution of surface absorption, vacuum extraction sweller also dry 48 hours;
4) take out dried polypropylene hollow fiber membrane, be soaked in water and clean the amphipathic molecule of the simple absorption in polypropylene screen surface.The performance of the polypropylene hollow fiber membrane of surface modification sees the following form 1.
Embodiment 4
1) uses acetone prerinse polypropylene hollow fiber membrane 24 hours;
2) with the polyethylene glycol section degree of polymerization be 8 18 pure polyglycol ethers be dissolved in dimethylbenzene/cyclohexanone (80/20, in mixed solvent wt%), be made into concentration expressed in percentage by weight and be 5% amphipathic molecule swelling solution;
3) swelling solution constant temperature drops into and carries out surface treatment through the pretreated polypropylene hollow fiber membrane of step 1 at 70 ℃, after 360 minutes, takes out polypropylene hollow fiber membrane, blots the solution of surface absorption, vacuum extraction sweller also dry 48 hours;
4) take out dried polypropylene hollow fiber membrane, be soaked in water and clean the amphipathic molecule of the simple absorption in polypropylene screen surface.The performance of the polypropylene hollow fiber membrane of surface modification sees the following form 1.
Embodiment 5
1) uses acetone prerinse polypropylene hollow fiber membrane 24 hours;
2) be that 8 18 pure polyglycol ethers are dissolved in 1 with the polyethylene glycol section degree of polymerization, in the 2-dichloroethanes, be made into concentration expressed in percentage by weight and be 5% amphipathic molecule swelling solution;
3) swelling solution constant temperature drops into and carries out surface treatment through the pretreated polypropylene hollow fiber membrane of step 1 at 60 ℃, after 360 minutes, takes out polypropylene hollow fiber membrane, blots the solution of surface absorption, vacuum extraction sweller also dry 24 hours;
4) take out dried polypropylene hollow fiber membrane, be soaked in water and clean the amphipathic molecule of the simple absorption in polypropylene screen surface.The performance of the polypropylene hollow fiber membrane of surface modification sees the following form 1.
Comparative Examples 1
1) uses acetone prerinse polypropylene hollow fiber membrane 24 hours;
2) with the polyethylene glycol section degree of polymerization be 8 18 pure polyglycol ethers be dissolved in dimethylbenzene/cyclohexanone (80/20, in mixed solvent wt%), be made into concentration expressed in percentage by weight and be 5% amphipathic molecule solution;
3) at ambient temperature, to immerse in the amphipathic molecule solution of step 2 through the pretreated polypropylene hollow fiber membrane of step 1,, take out after 15 minutes at the surface-coated amphipathic molecule of polypropylene hollow fiber membrane, blot the solution of surface absorption, vacuum drying 48 hours;
4) take out dried polypropylene hollow fiber membrane, be soaked in water and clean the amphipathic molecule of the simple absorption in polypropylene screen surface.The performance of the polypropylene hollow fiber membrane of surface modification sees the following form 1.
Table 1
| Embodiment | Sweller | Processing time (min) | Contact angle (°) | Water flux a (kg/h m 2) | BSA adsorbance b (mg/g) | |
| Advancing angle | Receding angle | |||||
| Embodiment 1 | Carbon tetrachloride | 60 | 82.8 | 17.9 | 24.5 | 0.071 |
| Embodiment 2 | Carbon tetrachloride | 360 | 41.5 | 3.1 | 27.3 | 0.032 |
| Embodiment 3 | Carbon tetrachloride | 720 | 40.0 | 0 | 18.1 | 0.024 |
| Embodiment 4 | Dimethylbenzene/cyclohexanone (80/20, wt%) | 360 | 55.6 | 6.0 | 13.7 | 0.035 |
| Embodiment 5 | 1, the 2-dichloroethanes | 360 | 65.5 | 14.9 | 27.0 | 0.040 |
| Comparative Examples 1 | Dimethylbenzene/cyclohexanone (80/20, wt%) | 15 | 119.0 | 89.6 | 0 | 0.118 |
| Original membrane | 121.5 | 92.2 | 0 | 0.131 | ||
Annotate: a. film pressure at both sides 0.02MPa; B. PROTEIN B SA initial concentration 0.8mg/mL soaked 24 hours.
As can be seen from the above table, compare with not surface treated original membrane, after the surface modification of embodiment 1～5, the contact angle of polypropylene porous membrane surface all has decline in various degree, the water flux of film is improved, the film surface descends to the adsorbance of PROTEIN B SA simultaneously, and is wherein better with the hydrophilicity on embodiment 2～5 Modified Membrane surfaces.Because the treatment temperature of Comparative Examples 1 is a room temperature, not by embedding, the simple amphipathic molecule that applies in this surface is easily washed by water amphipathic molecule, so the surface of film does not obtain effective hydrophilic modification on the surface of membrane material.
Claims (7)
1, a kind of amphipathic molecule is to the hydrophilic modification method of polypropylene porous membrane surface, it is characterized in that this method is that amphipathic molecule with block structure is as the hydrophilic modifying agent, earlier polypropylene porous film be impregnated in and carry out surface treatment in the sweller that is dissolved with amphipathic molecule, carry out surperficial deswelling with the method for vacuum extraction sweller at last.
2, amphipathic molecule according to claim 1 is characterized in that may further comprise the steps to the hydrophilic modification method of polypropylene porous membrane surface:
1) uses acetone prerinse polypropylene porous film 24 hours;
2) amphipathic molecule is dissolved in to be made into concentration expressed in percentage by weight in the sweller be 5～10% amphipathic molecule solution;
3) polypropylene porous film being dropped into temperature is to carry out surface treatment in 50～70 ℃ the solution of amphipathic molecule, after 60～720 minutes, takes out polypropylene porous film, vacuum extraction sweller and dry 24～48 hours;
4) take out dried polypropylene porous film, be soaked in water, clean the amphipathic molecule of the simple absorption of polypropylene porous membrane surface.
3, amphipathic molecule according to claim 1 and 2 is to the hydrophilic modification method of polypropylene porous membrane surface, and described amphipathic molecule is that molecular weight is 400～2000 18 pure polyglycol ethers, polyvinyl alcohol graft copolymerized polypropylene wax or Tissuemat E, polyacrylic acid grafted polypropylene wax or Tissuemat E.
4, amphipathic molecule according to claim 3 is to the hydrophilic modification method of polypropylene porous membrane surface, it is characterized in that described amphipathic molecule is that the degree of polymerization of polyalkylene glycol moiety is 8 18 pure polyglycol ethers.
5, amphipathic molecule according to claim 1 and 2 is characterized in that described sweller is a carbon tetrachloride, 1,2-dichloroethanes, dimethylbenzene/cyclohexanone mixed solvent or naphthane to the hydrophilic modification method of polypropylene porous membrane surface.
6, amphipathic molecule according to claim 1 and 2 is characterized in that to the hydrophilic modification method of polypropylene porous membrane surface described dimethylbenzene/its weight proportion of cyclohexanone mixed solvent is 90/10～60/40.
7, amphipathic molecule according to claim 1 and 2 is characterized in that to the hydrophilic modification method of polypropylene porous membrane surface described polypropylene porous film is a polypropylene hollow fiber membrane.
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