CN112717714A - Preparation method of SMA and PVDF blended hollow fiber membrane - Google Patents
Preparation method of SMA and PVDF blended hollow fiber membrane Download PDFInfo
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- CN112717714A CN112717714A CN202110035803.0A CN202110035803A CN112717714A CN 112717714 A CN112717714 A CN 112717714A CN 202110035803 A CN202110035803 A CN 202110035803A CN 112717714 A CN112717714 A CN 112717714A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
- B01D69/087—Details relating to the spinning process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/12—Specific ratios of components used
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/36—Hydrophilic membranes
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Abstract
A preparation method of a SMA and PVDF blended hollow fiber membrane belongs to the technical field of membrane science. The method comprises the following steps: 1) heating, stirring and dissolving PVDF, SMA, a solvent and a pore-forming agent to form a mixed solution, and carrying out vacuum defoaming on the solution to obtain a spinning solution; 2) and (2) obtaining the hollow fiber membrane by adopting wet spinning, wherein the nascent hollow fiber membrane yarn sequentially passes through an air layer and a coagulation bath, is collected by winding, enters a water tank for further exchange, is fished out after the exchange is finished, and is naturally dried in a cool and ventilated place, and finally the hollow fiber membrane is obtained. The preparation method of the SMA and PVDF blended hollow fiber membrane is simple, the hydrophilicity of the PVDF hollow fiber membrane is gradually increased along with the increase of the addition amount of the SMA, and the anti-pollution performance is gradually enhanced.
Description
The invention belongs to the technical field of membrane science, and particularly relates to a preparation method of a SMA and PVDF blended hollow fiber membrane.
Background
The membrane separation technology is a high and new technology with great development prospect in recent years, and compared with the traditional separation processes of filtration, screening, rectification, extraction, evaporation, recrystallization, sublimation, decoloration, leaching, adsorption, ion exchange and the like, the membrane separation technology has the unique characteristics of strong adaptability, good selectivity, simple preparation process, energy conservation, no phase change, no secondary pollution and the like.
Polymeric membrane materials are widely varied, such as polypropylene, polysulfone, polyethersulfone, cellulose acetate, and the like. Polyvinylidene fluoride (PVDF) has excellent physical and chemical properties, excellent processability, thermal stability, chemical corrosion resistance and the like, and is widely applied to the fields of environmental protection, metallurgy, medicine, food and the like. Since PVDF is a hydrophobic linear crystalline polymer, the surface of the prepared PVDF hollow fiber membrane has strong hydrophobicity, and in the actual use process, the membrane is polluted due to the adsorption effect, so that the use range of the membrane is reduced, the use time of the membrane is shortened, and the service life of the membrane is shortened.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to design and provide a technical scheme of a preparation method of a SMA and PVDF blended hollow fiber membrane, the preparation method is simple, the hydrophilicity of the PVDF hollow fiber membrane is gradually increased along with the increase of the addition amount of SMA, and the anti-pollution performance is gradually enhanced. The method is simple and effective, and has good application prospect in the aspects of expanding the application range and prolonging the service life.
The preparation method of the SMA and PVDF blended hollow fiber membrane is characterized by comprising the following steps:
1) heating and stirring 15-25 parts of polyvinylidene fluoride (PVDF), 15-20 parts of styrene maleic anhydride copolymer (SMA), 40-50 parts of solvent and 15-22 parts of pore-forming agent at 65-75 ℃ to dissolve to form a mixed solution, and carrying out vacuum defoaming on the solution to obtain a spinning solution, wherein the temperature of the spinning solution is 40-80 ℃;
2) and (2) obtaining a hollow fiber membrane by adopting wet spinning, sequentially passing the nascent hollow fiber membrane filaments through an air layer and a coagulating bath, collecting by filament winding, then entering a water tank for further exchange, wherein the exchange time is 60-85h, fishing out the membrane filaments after the exchange is finished, and naturally drying in a cool and ventilated place to finally obtain the hollow fiber membrane.
The preparation method of the SMA and PVDF blended hollow fiber membrane is characterized in that in the step 1): 18-22 parts of polyvinylidene fluoride, 16-18 parts of SMA, 45-47 parts of solvent and 19-20 parts of pore-foaming agent.
The preparation method of the SMA and PVDF blended hollow fiber membrane is characterized in that in the step 1): heating to dissolve at 68-72 deg.C, preferably 70-71 deg.C; the temperature of the spinning solution is 50 to 70 ℃, preferably 60 to 65 ℃.
The preparation method of the SMA and PVDF blended hollow fiber membrane is characterized in that the solvent is one or more than one mixed solvent of N-N dimethylformamide, N-N dimethylacetamide, N methylpyrrolidone and dimethyl sulfoxide.
The preparation method of the SMA and PVDF blended hollow fiber membrane is characterized in that the pore-forming agent is one or more of polyethylene glycol, polypropylene glycol, polyvinylpyrrolidone, glycerol, ethylene glycol, water, ethanol, n-butanol, isopropanol, cationic surfactant, anionic surfactant, nonionic surfactant and butanone.
The preparation method of the SMA and PVDF blended hollow fiber membrane is characterized in that in the step 2): the coagulating bath is a mixed solution of a solvent and water, wherein the concentration of the solvent is 10-70 parts; the temperature of the coagulating bath is 20-100 ℃; the solvent is one or more of N-N dimethylformamide, N-N dimethylacetamide, N-methylpyrrolidone and dimethyl sulfoxide.
The preparation method of the SMA and PVDF blended hollow fiber membrane is characterized in that in the step 2): the spinning temperature is 0-90 ℃; the spinning water inlet distance is 0-40 cm; the spinning speed is 1-100 m/min.
The styrene maleic anhydride copolymer (SMA) of the present invention, the simplest form of transparent SMA, is prepared by reacting a styrene monomer with a small amount of maleic anhydride monomer randomly attached to the PS backbone, increasing the glass transition and heat distortion temperature. Typical styrene-maleic anhydride copolymer products have heat distortion temperatures in excess of 260 ° F. The properties of this polymer are quite stable during injection molding even at temperatures in excess of 550 ° F. In the reaction stage, the rubber segment is grafted on the polymer, so that the polymer has good toughness. In many applications, it is desirable to increase the strength and stiffness of styrene-maleic anhydride copolymers through glass fiber reinforcement. Chemical coupling between the chemically treated glass fiber surface and the highly polar maleic anhydride component can be easily performed and is durable. This good adhesion can be fully confirmed by electron microscopy of fractures in the composite. This adhesion allows the strength, modulus, toughness (even after prolonged exposure to harsh environments) to remain unchanged for extended periods of time. The product with stabilized properties has almost no loss of main strength and toughness after 2000hr at a temperature exceeding 235 deg.F.
The preparation method of the SMA and PVDF blended hollow fiber membrane has the following beneficial effects:
1. the polyvinylidene fluoride is used as a membrane material, has the characteristics of excellent processing performance, thermal stability, chemical corrosion resistance and the like, and is widely applied to the fields of environmental protection, metallurgy, medicine, food and the like.
2. The method adopts a blending method to introduce the amphoteric polymer SMA into the PVDF hollow fiber membrane, and is simpler and easier to implement compared with the traditional method of introducing the amphoteric polymer into the PVDF hollow fiber membrane through an ATRP method.
3. The invention adopts a blending method to introduce the amphoteric polymer SMA onto the PVDF hollow fiber membrane to prepare the hollow fiber membrane, improves the hydrophilic performance of the hollow fiber membrane on the basis of ensuring the flux, improves the pollution resistance of the membrane wire, can expand the application range of the hollow fiber membrane and prolong the service life. Has the prospect of industrial application.
The parts referred to in the present invention are parts by weight unless otherwise indicated.
Detailed Description
The present invention will now be described more fully hereinafter with reference to the accompanying specific embodiments, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
heating, stirring and dissolving 15 parts of PVDF, 15 parts of SMA, 48 parts of a solvent (28 parts of N-dimethylacetamide and 20 parts of N-methylpyrrolidone), a pore-forming agent (3 parts of glycerol, 4 parts of ethylene glycol, 3 parts of water, 3 parts of ethanol, 3 parts of N-butanol, 3 parts of isopropanol and 3 parts of cationic surfactant) at 65 ℃ to form a mixed solution, and spinning the solution by adopting a wet spinning process after vacuum defoaming, wherein the temperature of the spinning solution is 40 ℃; extruding the spinning solution from a spinneret orifice, and passing the spinning solution through a coagulating bath formed by mixing N-N dimethylformamide and water, wherein the concentration of a solvent of the coagulating bath is 20wt%, the temperature of the coagulating bath is 30 ℃, and the spinning water-entering distance is 5 cm; the spinning speed was 20 m/min. And collecting by using a wire winding roller, continuously removing the solvent and the pore-forming agent in a water tank, removing after 3 days, and airing to finally obtain the hollow fiber membrane. Testing the hydrophilicity and the anti-pollution performance of the prepared hollow fiber membrane, wherein the pure water contact angle of the hollow fiber membrane is 53.3 degrees; in a BSA solution having a concentration of 3.0g/L, the amount of adsorption of the BSA solution by the hollow fiber membrane was 0.28 mg/mL.
Example 2:
heating and stirring 18 parts of PVDF, 18 parts of SMA, 48 parts of solvent (N-N dimethylacetamide), pore-forming agent (a mixture of 5 parts of polyethylene glycol (PEG), 6 parts of polyvinylpyrrolidone (PVP), 3 parts of deionized water and 2 parts of glycerol) at 70 ℃ to dissolve the mixture to form a mixed solution, and spinning the solution by adopting a wet spinning process after vacuum defoaming, wherein the temperature of the spinning solution is 60 ℃; in order to make the prepared hollow fiber membrane have smooth and compact surface, finger-shaped holes or sponge-shaped structures with larger pore diameter distribution can be formed in the membrane. Extruding the spinning solution from a spinneret orifice, and passing the spinning solution through a coagulating bath formed by mixing DMAC (dimethylacetamide) and water, wherein the concentration of a solvent of the coagulating bath is 60wt%, the temperature of the coagulating bath is 70 ℃, and the spinning water-entering distance is 20 cm; the spinning speed was 50 m/min. And collecting by using a wire winding roller, continuously removing the solvent and the pore-forming agent in a water tank, removing after 3 days, and airing to finally obtain the hollow fiber membrane. Testing the hydrophilicity and the anti-pollution performance of the prepared hollow fiber membrane, wherein the pure water contact angle of the hollow fiber membrane is 48.2 degrees; in a BSA solution having a concentration of 3.0g/L, the amount of adsorption of the BSA solution by the hollow fiber membrane was 0.27 mg/mL.
Example 3:
heating and stirring 20 parts of PVDF, 19 parts of SMA, a solvent (20 parts of N-dimethylacetamide and 23 parts of dimethyl sulfoxide), a pore-forming agent (a mixture of 6 parts of polyethylene glycol (PEG), 7 parts of polyvinylpyrrolidone (PVP), 3 parts of deionized water and 2 parts of glycerol) at 70 ℃ to dissolve the mixture to form a mixed solution, and spinning the solution by adopting a wet spinning process after vacuum defoaming, wherein the temperature of the spinning solution is 55 ℃; the spinning solution was extruded from a spinneret orifice through a die consisting of N-N dimethylformamide in a weight ratio of 1: 2: a coagulation bath formed by mixing dimethyl sulfoxide and water, wherein the concentration of a solvent of the coagulation bath is 55wt%, the temperature of the coagulation bath is 80 ℃, and the spinning water inlet distance is 30 cm; the spinning speed was 70 m/min. And collecting by using a wire winding roller, continuously removing the solvent and the pore-forming agent in a water tank, removing after 3 days, and airing to finally obtain the hollow fiber membrane. Testing the hydrophilicity and the anti-pollution performance of the prepared hollow fiber membrane, wherein the pure water contact angle of the hollow fiber membrane is 45.6 degrees; in a BSA solution having a concentration of 3.0g/L, the amount of adsorption of the BSA solution by the hollow fiber membrane was 0.25 mg/mL.
Example 4:
heating, stirring and dissolving PVDF25 parts, SMA20 parts, solvent 50 (N-N dimethylacetamide DMAC20 parts, N methyl pyrrolidone 10 parts and dimethyl sulfoxide 20 parts), pore-forming agent (a mixture of polypropylene glycol 1 part, ethylene glycol 1 part, anionic surfactant 1 part and glycerol 1 part) at 75 ℃ to form a mixed solution, and spinning the solution by adopting a wet spinning process after vacuum defoaming, wherein the temperature of the spinning solution is 80 ℃; the spinning solution was extruded from a spinneret orifice through a die consisting of N-methylpyrrolidone: a coagulation bath formed by mixing dimethyl sulfoxide and water, wherein the concentration of a solvent of the coagulation bath is 70wt%, the temperature of the coagulation bath is 90 ℃, and the spinning water inlet distance is 40 cm; the spinning speed was 80 m/min. And collecting by using a wire winding roller, continuously removing the solvent and the pore-forming agent in a water tank, removing after 3 days, and airing to finally obtain the hollow fiber membrane. Testing the hydrophilicity and the anti-pollution performance of the prepared hollow fiber membrane, wherein the pure water contact angle of the hollow fiber membrane is 44.1 degrees; in a BSA solution having a concentration of 3.0g/L, the amount of adsorption of the BSA solution by the hollow fiber membrane was 0.25 mg/mL.
The advantageous effects of the present invention are further illustrated by comparative test data below.
Comparative example 1: heating and stirring 18 parts of polyvinylidene fluoride resin (hereinafter abbreviated as PVDF), 63 parts of N-N dimethylacetamide (hereinafter abbreviated as DMAC) and 19 parts of pore-forming agent (a mixture of 6 parts of polyethylene glycol (PEG), 7 parts of polyvinylpyrrolidone (PVP), 4 parts of deionized water and 2 parts of glycerol) at 70 ℃ to dissolve the mixture to form a mixed solution, and spinning the solution by adopting a wet spinning process after vacuum defoaming. In order to make the prepared hollow fiber membrane have smooth and compact surface, finger-shaped holes or sponge-shaped structures with larger pore diameter distribution can be formed in the membrane. The spinning dope is extruded from the spinneret orifices and passed through a coagulation bath formed by mixing DMAC and water. And collecting by using a wire winding roller, continuously removing the solvent and the pore-forming agent in a water tank, removing after 3 days, and airing to finally obtain the hollow fiber membrane. Testing the hydrophilicity and the anti-pollution performance of the prepared hollow fiber membrane, wherein the pure water contact angle of the hollow fiber membrane is 90.4 degrees; in a BSA solution having a concentration of 3.0g/L, the amount of adsorption of the BSA solution by the hollow fiber membrane was 0.54 mg/mL.
Comparative example 2: heating, stirring and dissolving 18 parts of PVDF, 61 parts of DMAC, 19 parts of pore-forming agent (a mixture of 6 parts of polyethylene glycol (PEG), 7 parts of polyvinylpyrrolidone (PVP), 4 parts of deionized water and 2 parts of glycerol) and 2 parts of SMA at 70 ℃ to form a mixed solution, and spinning the solution by adopting a wet spinning process after vacuum defoaming. In order to make the prepared hollow fiber membrane have smooth and compact surface, finger-shaped holes or sponge-shaped structures with larger pore diameter distribution can be formed in the membrane. The spinning dope is extruded from the spinneret orifices and passed through a coagulation bath formed by mixing DMAC and water. And collecting by using a wire winding roller, continuously removing the solvent and the pore-forming agent in a water tank, removing after 3 days, and airing to finally obtain the hollow fiber membrane. Testing the hydrophilicity and the anti-pollution performance of the prepared hollow fiber membrane, wherein the pure water contact angle of the hollow fiber membrane is 68.5 degrees; in a BSA solution having a concentration of 3.0g/L, the amount of adsorption of the BSA solution by the hollow fiber membrane was 0.52 mg/mL.
Comparative example 3: heating, stirring and dissolving 18 parts of PVDF, 57 parts of DMAC, 19 parts of pore-forming agent (a mixture of 6 parts of polyethylene glycol (PEG), 7 parts of polyvinylpyrrolidone (PVP), 4 parts of deionized water and 2 parts of glycerol) and 6 parts of SMA at 70 ℃ to form a mixed solution, and spinning the solution by adopting a wet spinning process after vacuum defoaming. In order to make the prepared hollow fiber membrane have smooth and compact surface, finger-shaped holes or sponge-shaped structures with larger pore diameter distribution can be formed in the membrane. The spinning dope is extruded from the spinneret orifices and passed through a coagulation bath formed by mixing DMAC and water. And collecting by using a wire winding roller, continuously removing the solvent and the pore-forming agent in a water tank, removing after 3 days, and airing to finally obtain the hollow fiber membrane. Testing the hydrophilicity and the anti-pollution performance of the prepared hollow fiber membrane, wherein the pure water contact angle of the hollow fiber membrane is 65.1 degrees; in a BSA solution having a concentration of 3.0g/L, the amount of adsorption of the BSA solution by the hollow fiber membrane was 0.45 mg/mL.
Comparative example 4: heating, stirring and dissolving 18 parts of PVDF, 53 parts of DMAC, 19 parts of pore-forming agent (a mixture of 6 parts of polyethylene glycol (PEG), 7 parts of polyvinylpyrrolidone (PVP), 4 parts of deionized water and 2 parts of glycerol) and 10 parts of SMA at 70 ℃ to form a mixed solution, and spinning the solution by adopting a wet spinning process after vacuum defoaming. In order to make the prepared hollow fiber membrane have smooth and compact surface, finger-shaped holes or sponge-shaped structures with larger pore diameter distribution can be formed in the membrane. The spinning dope is extruded from the spinneret orifices and passed through a coagulation bath formed by mixing DMAC and water. And collecting by using a wire winding roller, continuously removing the solvent and the pore-forming agent in a water tank, removing after 3 days, and airing to finally obtain the hollow fiber membrane. Testing the hydrophilicity and the anti-pollution performance of the prepared hollow fiber membrane, wherein the pure water contact angle of the hollow fiber membrane is 64.3 degrees; in a BSA solution having a concentration of 3.0g/L, the amount of adsorption of the BSA solution by the hollow fiber membrane was 0.48 mg/mL.
The results of inventive examples 1-4 and comparative examples 1-4 show that: the prepared hollow fiber membrane is tested for hydrophilicity and anti-pollution performance, and the pure water contact angle of the hollow fiber membrane is 44.1-53.3 degrees; in BSA solution with the concentration of 3.0g/L, the adsorption capacity of the hollow fiber membrane is 0.24-0.29 mg/mL. The hollow fiber membranes obtained in comparative examples 1 to 4 had a contact angle of pure water of 64.3 to 90.4 ℃ and an adsorption amount of 0.48 to 0.54mg/mL in a BSA solution having a concentration of 3.0 g/L.
The preparation method limits the proportion of PVDF, SMA, solvent and pore-forming agent, the heating and stirring temperature, the temperature of spinning solution, the temperature, time and concentration of a coagulation bath, the water inlet distance of spinning and the spinning speed. According to the invention, with the increase of the addition amount of SMA, the hydrophilicity of the PVDF hollow fiber membrane is gradually increased, and the anti-pollution performance is gradually enhanced.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A preparation method of a SMA and PVDF blended hollow fiber membrane is characterized by comprising the following steps:
1) heating and stirring 15-25 parts of polyvinylidene fluoride (PVDF), 15-20 parts of styrene maleic anhydride copolymer (SMA), 40-50 parts of solvent and 15-22 parts of pore-forming agent at 65-75 ℃ to dissolve to form a mixed solution, and carrying out vacuum defoaming on the solution to obtain a spinning solution, wherein the temperature of the spinning solution is 40-80 ℃;
2) and (2) obtaining a hollow fiber membrane by adopting wet spinning, sequentially passing the nascent hollow fiber membrane filaments through an air layer and a coagulating bath, collecting by filament winding, then entering a water tank for further exchange, wherein the exchange time is 60-85h, fishing out the membrane filaments after the exchange is finished, and naturally drying in a cool and ventilated place to finally obtain the hollow fiber membrane.
2. The method for preparing the SMA and PVDF blended hollow fiber membrane as claimed in claim 1, wherein in step 1): 18-22 parts of polyvinylidene fluoride, 16-18 parts of SMA, 45-47 parts of solvent and 19-20 parts of pore-foaming agent.
3. The method for preparing the SMA and PVDF blended hollow fiber membrane as claimed in claim 1, wherein in step 1): heating to dissolve at 68-72 deg.C, preferably 70-71 deg.C; the temperature of the spinning solution is 50 to 70 ℃, preferably 60 to 65 ℃.
4. The method for preparing the SMA and PVDF blended hollow fiber membrane as claimed in claim 1, wherein the solvent is one or more of N-N dimethylformamide, N-N dimethylacetamide, N methylpyrrolidone and dimethyl sulfoxide.
5. The method for preparing SMA and PVDF blended hollow fiber membrane according to claim 1, wherein the pore-forming agent is one or more of polyethylene glycol, polypropylene glycol, polyvinylpyrrolidone, glycerol, ethylene glycol, water, ethanol, n-butanol, isopropanol, cationic surfactant, anionic surfactant, nonionic surfactant, and butanone.
6. The method for preparing the SMA and PVDF blended hollow fiber membrane as claimed in claim 1, wherein in step 2): the coagulating bath is a mixed solution of a solvent and water, wherein the concentration of the solvent is 10-70 wt%; the temperature of the coagulating bath is 20-100 ℃; the solvent is one or more of N-N dimethylformamide, N-N dimethylacetamide, N-methylpyrrolidone and dimethyl sulfoxide.
7. The method for preparing the SMA and PVDF blended hollow fiber membrane as claimed in claim 1, wherein in step 2): the spinning temperature is 0-90 ℃; the spinning water inlet distance is 0-40 cm; the spinning speed is 1-100 m/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116712870A (en) * | 2023-08-10 | 2023-09-08 | 世韩(天津)节能环保科技有限公司 | Hydrophilic modification method for polypropylene film |
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| CN101264428A (en) * | 2008-04-25 | 2008-09-17 | 浙江大学 | Method for modifying polyvinylidene fluoride ultrafiltration membrane by amphiphilic co-polymer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101264428A (en) * | 2008-04-25 | 2008-09-17 | 浙江大学 | Method for modifying polyvinylidene fluoride ultrafiltration membrane by amphiphilic co-polymer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116712870A (en) * | 2023-08-10 | 2023-09-08 | 世韩(天津)节能环保科技有限公司 | Hydrophilic modification method for polypropylene film |
| CN116712870B (en) * | 2023-08-10 | 2024-04-26 | 世韩(天津)节能环保科技有限公司 | Hydrophilic modification method for polypropylene film |
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