KR101817311B1 - Polyethersulfone-based porous film having high flux property, preparation method and use thereof - Google Patents
Polyethersulfone-based porous film having high flux property, preparation method and use thereof Download PDFInfo
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- KR101817311B1 KR101817311B1 KR1020150053071A KR20150053071A KR101817311B1 KR 101817311 B1 KR101817311 B1 KR 101817311B1 KR 1020150053071 A KR1020150053071 A KR 1020150053071A KR 20150053071 A KR20150053071 A KR 20150053071A KR 101817311 B1 KR101817311 B1 KR 101817311B1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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Abstract
The present invention relates to a polyether sulfone-based porous film having excellent permeation flow characteristics, a method for producing the same, and a use thereof. The production method according to the present invention comprises the steps of (i) selecting the number average molecular weight of polyethylene glycol, The method comprising: selecting a content of the polyethylene glycol and a content of polyethersulfone in a solution, obtaining a polymer solution at a first temperature under the selected conditions, shaping the polymer solution into a film form, 2, and thereby inducing the vapor-induced phase separation and the inverse-induced phase separation to occur at the same time, thereby providing a polyether sulfone-based porous film having excellent pore formation and excellent pore distribution because of its excellent water permeation flow rate.
Description
The present invention relates to a polyether sulfone-based porous film having excellent permeation flow characteristics, a method for producing the same, and uses thereof.
Vapor-induced phase separation (VIPS) is a process in which a shaped polymer solution is exposed to the atmosphere prior to solvent-non-solvent exchange by nonsolvent-induced phase separation (NIPS) And applied to various materials such as PES, PS, PEI and PVDF. Unlike NIPS, the atmospheric air is exposed to air containing a certain concentration of moisture, and thus phase separation is initiated through moisture absorption in the air. The VIPS method has a high porosity and a high permeation flux, but it has a wide pore distribution.
On the other hand, the non-solvent-derived phase separation method is a process in which a polymer solution extracts a solvent by contacting with a non-solvent and causes phase separation, and uses a precipitation of a polymer by exchanging a solvent and a non-solvent in the polymer solution. When a polymer solution prepared by dissolving a polymer in an appropriate solvent is formed and precipitated in a coagulation tank containing a non-solvent, the solvent in the polymer solution is extracted, the polymer forms a matrix, and the solvent is removed to form pores. The non-solvent-based phase separation method has an advantage in that the size of the pores can be freely controlled, but the mechanical strength of the separation membrane is weak and the lifetime of the membrane is shortened because it includes finger-like macrovoids.
Generally, most of the conventionally used separator materials such as polysulfone system and cellulose acetate system are manufactured by vapor induced phase separation method and have a high water permeation flow rate, but they have a wide pore distribution. In addition, polymer separator materials such as nylon, polyethersulfone, cellulose acetate, and fluorine resin generally use a steam-induced phase separation method and a non-solvent-derived phase separation method, and have disadvantages in that porosity and film strength are lowered when they are produced by this method .
It is difficult to fabricate membranes using heat - induced phase separation method for most materials. Particularly, since hydrophilic materials have no crystallinity, there is a problem that pore formation is difficult in the production of a separation membrane by using a heat induction phase separation method. Thus, hydrophilic materials have been prepared using the non-solvent-derived phase separation method. However, when the separator is prepared using the non-solvent-derived phase separation method, the physical properties are poor and the transmittance is also low.
Therefore, it is required to develop a new method for manufacturing a membrane material having macropores and narrow pore size distribution so that a membrane material having a high water permeation flow rate applicable to general water treatment and semiconductor processing can be provided.
An object of the present invention is to provide a polyether sulfone-based porous film having a high water permeation flow rate, a method for producing the same, and a method for using the same.
A first aspect of the present invention is a polyether sulfone-based porous film having a first side and a second side and having a water permeation flow rate of 1,000 L / m 2 or more at 1 kgf / cm 2, A method for producing a porous film in which spherical particles of ether sulfone are connected to each other to form pores, the method comprising the steps of: (i) selecting a number average molecular weight of polyethylene glycol, which is capable of forming pores by connecting spherical polyether sulfone particles on the surface; ii) a first step of selecting the content of the polyethylene glycol and the content of polyethersulfone in the whole polymer solution; A second step of dissolving the polyethersulfone and the selected polyethylene glycol in a solvent at a first temperature to obtain a polymer solution; A third step of forming the polymer solution into a film form and exposing it to water vapor at a second temperature equal to or higher than the first temperature to effect phase transformation; And a fourth step of immersing the film exposed to the water vapor in a non-solvent. The present invention also provides a method for producing a polyether sulfone porous film.
A second aspect of the present invention is a polyether sulfone-based porous film having a first side and a second side and having a water permeation flow rate of 1,000 L / m 2 or more at 1 kgf / cm 2, There is provided a porous film formed by steam-induced phase separation and inverse-heat-induced phase separation using polyethylene glycol having a molecular weight of 200 to 600 as a pore-forming agent of polyethersulfone, wherein spherical particles of ether sulfone are connected to each other and pores are formed.
A third aspect of the present invention provides a water treatment filter comprising the polyethersulfone porous film according to the second aspect.
A fourth aspect of the present invention provides a water treatment apparatus comprising the water treatment filter according to the third aspect.
A fifth aspect of the present invention provides a method for producing water-treated water, comprising the step of water-treating using the water-treatment filter according to the third aspect.
Hereinafter, the configuration of the present invention will be described in detail.
Generally, a hydrophilic polyether sulfone porous film is prepared by vapor induced phase separation and nonporous phase inductively separating method. When it is produced by this method, formation of macropores is difficult, pore distribution is widened, and porosity is lowered. When the porosity is decreased, the water permeation flow rate is lowered and the application is limited to general water treatment or semiconductor processing.
The present invention provides a method for producing a polyether sulfone based porous film having a first side and a second side and capable of providing a polyether sulfone type porous film having a water permeation flow rate of 1,000 kg / cm < 2 > Phase separation and inductively induced phase separation.
As used herein, the term " inductively induced phase separation method "is a phase separation method distinguished from the existing heat induction phase separation method. Conventional heat induction phase separation method forms a high-temperature polymer solution and phase-separates under a low temperature condition. The inductively induced phase separation method used herein may mean a method of forming a low-temperature polymer solution and phase-separating the polymer solution under the same or higher temperature than the above-mentioned polymer solution.
Further, in the present invention, in order to provide a polyether sulfone-based porous film having a water permeation flow rate of 1,000 L / m 2 or more at 1 kgf / cm 2, spherical polyether sulfone particles are connected to each other on the first surface, Thereby forming a pore, thereby producing a porous film having excellent porosity.
In order to achieve the above object, the present invention provides a method for producing a polyether sulfone spherical particle, comprising the steps of: (i) selecting a number average molecular weight of polyethylene glycol to be connected to spherical particles of polyether sulfone on the surface to form pores; (ii) The polymer solution is formed into a film form at a first temperature under the above-mentioned selected conditions and then exposed to water vapor at a second temperature equal to or higher than the first temperature to form a phase transition It was found that a steam-induced phase separation and a reverse-phase induced phase separation simultaneously occur, thereby making it possible to produce a film having excellent porosity but not a wide pore distribution. The present invention is based on this finding.
That is, when a polyethersulfone-based porous film is produced according to the production method of the present invention, it is possible to produce a porous film having pore control and excellent water permeation flow rate. When a polyethylene glycol having a molecular weight of more than 600 is used, or when the content of the polyethylene glycol is low or other additives other than polyethylene glycol are used, the pores may be uneven and the porosity may be decreased to reduce the flow rate. The present invention is characterized in that the pores are uniform, the difference between the maximum pore and the average pore is small, the porosity is high, and the flow rate is very high. For this, the VIPS method should not be used and the TIPS method should be used.
The term " polyethersulfone (PES) "used in the present invention is an amber transparent amorphous resin containing a unit represented by the following formula (1). PES is excellent in heat resistance and creep resistance at a glass transition temperature of 225 ° C because of low temperature dependency of physical properties and excellent processability. Therefore, transparent substrates for LCDs, injection molded products for automobiles, structural materials for aircraft, And is widely used as a material for polymer membranes, particularly hollow membranes.
[Chemical Formula 1]
In Formula 1,
and n is an integer of 100 to 200.
In the polyether sulfone-based porous film produced by the production method of the present invention, the spherical polyether sulfone particles on the first surface, the second surface, or both are connected to each other to form pores, thereby forming macropores and narrowing the pore distribution, Lt; RTI ID = 0.0 > L / m2hr. ≪ / RTI >
A polyether sulfone-based porous film having a first side and a second side according to the present invention and having a water permeation flow rate of 1,000 L / m 2 or more at 1 kgf / cm 2, wherein the polyether sulfone- A method of manufacturing a porous film in which particles are connected to each other and a pore is formed may include the following steps.
(I) the number average molecular weight of the polyethylene glycol is selected, and (ii) the content of the polyethylene glycol and the content of the polyether sulfone in the whole polymer solution A first step of selecting;
A second step of dissolving the polyethersulfone and the selected polyethylene glycol in a solvent at a first temperature to obtain a polymer solution;
A third step of forming the polymer solution into a film form and exposing it to water vapor at a second temperature equal to or higher than the first temperature to effect phase transformation; And
And a fourth step of immersing the film exposed to the water vapor in the non-solvent.
In the present invention, the first surface may refer to a film surface exposed to water vapor, and the second surface may refer to a back surface of the first surface.
The water permeation flow rate of the polyethersulfone porous film produced by the method according to the present invention may be 1,000 to 5,000 L / m 2 hr at 1 kgf / cm 2 (Table 1).
The first step is a condition in which the polyether sulfone spherical particles are connected to each other to form pores on the surface of the film, wherein (i) the number average molecular weight of the polyethylene glycol is selected, (ii) the polyethylene glycol And the content of polyethersulfone is selected.
Preferably, the number average molecular weight of the polyethylene glycol selected in the first step may be from 200 to 600.
Specifically, in the examples of the present invention, it was confirmed that when the number average molecular weight of the polyethylene glycol exceeds 600, the water permeation flow rate is drastically decreased (comparison between Example 1 and Comparative Examples 3 and 4).
Preferably, the content of polyethersulfone in the entire polymer solution selected in the first step is 10 to 25% by weight, and the content of polyethylene glycol is 25 to 70% by weight. More preferably, the content of the polyethersulfone in the entire polymer solution selected in the first step is 15 to 20% by weight, and the content of polyethylene glycol is 50 to 70% by weight.
Specifically, in the embodiment of the present invention, when the content of polyethersulfone in the whole polymer solution is adjusted to 10 to 25 wt% and the content of polyethylene glycol is adjusted to 25 to 70 wt%, the water permeation flow rate is 1 kgf / It is confirmed that it can be over 1,000 L / ㎡ hr. Particularly, the content of polyethersulfone in the whole polymer solution is adjusted to 15 to 20% by weight (comparison of Examples 1 and 5 and Example 6), the content of polyethylene glycol is controlled to 50 to 70% by weight 1, 7 and 8 and Example 9), it was confirmed that the water permeation flow rate could be 2,000 L / m 2 hr or more, specifically 2100 to 4300 L / m 2 hr at 1 kgf / cm 2.
The second step is a step of dissolving polyethersulfone in a solvent at a first temperature in a selected content together with the polyethylene glycol selected in the first step to obtain a polymer solution for film forming.
The term " polyethylene glycol (PEG) "used in the present invention may mean a polymer compound represented by the following formula (2).
(2)
H- (O-CH 2 -CH 2 ) m -OH
In Formula 2, m is the number of ethylene glycol repeating units (O-CH 2 -CH 2 ), and may be appropriately changed according to the molecular weight of the selected polyethylene glycol.
In the present invention, the polyethylene glycol may serve as a pore-forming agent for polyethersulfone. That is, the polyethylene glycol is removed from the surface of the film when the polyethersulfone-containing polymer solution is simultaneously inductively induced and phase-separated at the temperature of the polymer solution, that is, at a second temperature higher than or equal to the first temperature, Polyethersulfone Forms spherical particles to form pores.
The term "solvent " used in the present invention is a solvent capable of dissolving at least 5 parts by weight of polymer at a temperature of about 60 DEG C or lower, and examples of the solvent of polyethersulfone include dimethylacetamide, dimethylformamide, dimethylsulfoxide Ketones such as acetone, methyl ethyl ketone, cyclic ketones such as N-methylpyrrolidone (NMP) and r-butyrolactone, and the like can be used.
In the present invention, the polymer solution obtained under the first temperature condition in the second step is then formed into a film form in the third step and is exposed to water vapor having a second temperature equal to or higher than the first temperature, And inductively induced phase separation are simultaneously performed. Thus, the pores are uniform, and the difference between the maximum pore and the average pore is small and the porosity is high, so that a film having a very high flow rate can be formed.
In the present invention, the molding in the third step may be performed by knife casting or tape casting, but not limited thereto, and any method capable of forming a film can be used. The knife casting or tape casting can be performed by molding the polymer solution into a plate shape such as a film using a knife or a tape, respectively.
In the present invention, the water vapor in the third step may have a relative humidity of 40 to 99%. If the relative humidity is less than 40%, there is a disadvantage that the pore formation is not performed well and the permeation flow rate becomes small.
In the present invention, the water vapor in the third step may have a temperature equal to or lower than the first temperature in the second step. Specifically, when the polymer solution is prepared at room temperature (20 ° C) in the second step, the water vapor in the third step may have a temperature of 30 to 60 ° C.
In the present invention, the water vapor exposure time in the third step is preferably 0.1 minute to 10 minutes, more preferably 1 minute to 5 minutes.
The fourth step is a step of immersing the film exposed to the water vapor in the non-solvent and solidifying the film.
The term " non-solvent " used in the present invention refers to a solvent that does not dissolve or swell the polymer until the melting point of the polymer or the boiling point of the liquid. Examples of the solvent include water, alcohol, ether, and hexane You can use water.
In the present invention, the fourth step may be carried out under a temperature condition of 5 to 30 占 폚.
In the present invention, the immersion time in the fourth step may be 5 minutes to 24 hours.
The present invention also provides a polyether sulfone-based porous film having a first side and a second side and having a water permeation flow rate of 1,000 L / m 2 or more at 1 kgf / cm 2,
Induced phase separation using a polyethylene glycol having a molecular weight of 200 to 600 as a pore-forming agent of polyethersulfone, wherein the spherical particles of polyethersulfone are connected to each other on the first surface, the second surface or both, To provide a porous film.
The polyether sulfone based porous film according to the present invention can be produced by the process according to the first aspect of the present invention.
The polyether sulfone based porous film according to the present invention may have a micro pore structure with a maximum pore size of 0.1 to 0.5 m and an average pore size of 0.1 to 0.4 m.
The polyether sulfone based porous film according to the present invention has a micro pore structure and has a water permeation flow rate of 1,000 L / m 2 or more at 1 kgf / cm 2, and can be used for manufacturing a water treatment filter, Treatment or ultrapure water purification, and the like. In addition, the polyether sulfone-based porous film according to the present invention can be widely used for manufacturing water treatment filters such as wastewater and water treatment, and can be used for various purposes known in the art depending on the type of polymer and physical properties, etc. .
Further, the present invention can provide a water treatment apparatus including the water treatment filter.
In the present invention, the water treatment apparatus may be, for example, a wastewater treatment apparatus for semiconductor processing, an ultrapure water purification apparatus for semiconductor processing, a water purifier, a pretreatment apparatus for seawater desalination, a water softener, a water treatment apparatus, a wastewater treatment apparatus or a food purification apparatus.
In addition, the present invention can provide a method for producing water-treated water including a step of water-treating using the water-treatment filter.
In the present invention, the water used for the water treatment may be ultrapure water, wastewater or seawater.
In the present invention, the water treated water may be ultrapure water, purified water, drinking water, or the like.
The production method of the present invention is characterized in that (i) the number average molecular weight of the polyethylene glycol is selected, (ii) the content of the polyethylene glycol and the content of the polyether sulfone in the whole polymer solution are selected, The polymer solution is formed into a film form and exposed to water vapor at a second temperature equal to or higher than the first temperature to induce phase transition so that steam induced phase separation and inverse heat induced phase separation coexist simultaneously, A polyether sulfone based porous film excellent in water permeation flow rate can be provided because the pore distribution is not wide and thus the film thus prepared is applicable to general water treatment and semiconductor processing.
FIG. 1 is a result of observation of a front surface (first surface) surface of a film produced according to an embodiment of the present invention with an electron microscope.
2 is a result obtained by observing the surface of the back surface (second surface) of the film produced according to an embodiment of the present invention with an electron microscope.
FIG. 3 shows the result of observation of the surface of the front surface (first surface) of the film produced according to the comparative example with an electron microscope.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
Example One: Polyethersulfone Porous film production
A solution having 15% by weight of polyethersulfone, 35% by weight of dimethylacetamide and 50% by weight of polyethylene glycol 200 was uniformly prepared at 20 캜. The film was uniformly coated on a glass plate with a casting knife having a thickness of 200 microns, exposed to air in a relative humidity of 80% at 40 DEG C in air for 3 minutes, immersed in distilled water at room temperature for coagulation, Respectively.
As a result, the permeation flow rate of the film was 3200 L / m 2 hr at 1 kgf / cm 2, and the maximum pore was 0.40 μm and the average pore was 0.35 μm (Table 1).
As a result of observing the surface state of the film by an electron microscope, it was found that the film was found to be poly (poly) film in the front face (first face) (FIG. 1) in contact with water vapor and the reverse face It was confirmed that spherical particles of ether sulfone were connected to each other to form pores, and the degree of pore formation was more prominent on the front face of the film.
Example 2: Polyethersulfone Porous film production
A polyethersulfone porous film was prepared in the same manner as in Example 1, except that the air humidity was 40%.
Example 3: Polyethersulfone Porous film production
A polyethersulfone porous film was prepared in the same manner as in Example 1, except that the temperature at the time of air exposure was 20 占 폚.
Example 4: Polyethersulfone Porous film production
A polyethersulfone porous film was prepared in the same manner as in Example 1, except that the coagulation bath was immersed in distilled water at 60 占 폚.
Comparative Example One: Polyethersulfone Porous film production
A polyethersulfone porous film was prepared in the same manner as in Example 1, except that a polymer solution having a composition of 15 wt% of polyethersulfone and 85 wt% of dimethylacetamide was used.
Example 5: Different concentration of polymer Polyethersulfone Porous film production
A polyethersulfone porous film was prepared in the same manner as in Example 1, except that the composition of the polymer solution was 20 wt% of polyethersulfone, 30 wt% of dimethylacetamide, and 50 wt% of polyethylene glycol 200.
Example 6: Different concentration of polymer Polyethersulfone Porous film production
A polyethersulfone porous film was prepared in the same manner as in Example 1, except that the composition of the polymer solution was 24 wt% of polyethersulfone, 26 wt% of dimethylacetamide, and 50 wt% of polyethylene glycol 200.
Example 7: Different additive concentrations Polyethersulfone Porous film production
A polyethersulfone porous film was prepared in the same manner as in Example 1 except that the composition of the polymer solution was 15 wt% of polyethersulfone, 25 wt% of dimethylacetamide, and 60 wt% of polyethylene glycol 200.
Example 8: Different additive concentrations Polyethersulfone Porous film production
A polyethersulfone porous film was prepared in the same manner as in Example 1, except that the composition of the polymer solution was 15 wt% of polyethersulfone, 15 wt% of dimethylacetamide, and 70 wt% of polyethylene glycol 200.
Example 9: Different additive concentrations Polyethersulfone Porous film production
A polyethersulfone porous film was prepared in the same manner as in Example 1, except that the composition of the polymer solution was 15 wt% of polyether sulfone, 60 wt% of dimethylacetamide, and 25 wt% of polyethylene glycol 200.
Comparative Example 2: Additive Different molecular weight Polyethersulfone Porous film production
A polyethersulfone porous film was prepared in the same manner as in Example 1, except that the composition of the polymer solution was 15 wt% of polyethersulfone, 60 wt% of dimethylacetamide, and 25 wt% of polyethylene glycol 2000.
FIG. 3 shows the result of observation of the front surface (first surface) in contact with water vapor on the surface of the prepared film by an electron microscope. 3, it was confirmed that the degree of pore formation of the film was lower than that of Example 1. [
Comparative Example 3: Additive Different molecular weight Polyethersulfone Porous film production
A polyethersulfone porous film was prepared in the same manner as in Example 1, except that the composition of the polymer solution was 15 wt% of polyethersulfone, 60 wt% of dimethylacetamide, and 25 wt% of polyethylene glycol 20000.
Experimental Example
1: Evaluation of membrane performance
The permeation fluxes of the membranes prepared in Examples 1 to 9 and Comparative Examples 1 to 3 were measured using ultrapure water. The membrane performance is shown in Table 1 below (measured pressure, 1 kgf / cm 2). The pore size was measured using a PMI Bubble Point Tester and the results are shown in Table 1.
From Table 1, it can be seen that the water permeation flow rate is drastically lowered in Comparative Examples 3 and 4 in which the molecular weight of polyethylene glycol is 2000 or more, and in particular, the water permeation flow rate is lower than that of Comparative Example 1 in which polyethylene glycol is not used . Therefore, it is understood that the molecular weight of the polyethylene glycol is required to be controlled in view of the water permeation flow rate.
Also, it can be seen from Table 1 that the content of polyethersulfone in the whole polymer solution is controlled to 10 to 25 wt% and the content of polyethylene glycol is controlled to 25 to 70 wt%, the water permeation flow rate is 1 L / / M < 2 > hr or more. Particularly, the content of polyethersulfone in the whole polymer solution is controlled to 15 to 20% by weight (comparison of Examples 1 and 5 and Example 6), and the content of polyethylene glycol is 50 to 70% by weight It can be confirmed that the water permeation flow rate can be 2,000 L / m 2 hr or more, specifically 2100 to 4300 L / m 2 hr at 1 kgf / cm 2 in the case of adjusting (comparison of Examples 1, 7 and 8 with Example 9) .
Claims (16)
(I) polyethylene glycol having a number average molecular weight of 200 is selected, and (ii) 50 to 70% by weight of the polyethylene glycol in the whole polymer solution is added to the polyether sulfone spherical particles, And a content of polyethersulfone of 15 to 20% by weight;
A second step of dissolving the polyethersulfone and the selected polyethylene glycol in a solvent at a first temperature to obtain a polymer solution;
A third step of forming the polymer solution into a film form and exposing the polymer solution to steam at a second temperature equal to or higher than the first temperature and a relative humidity of 40 to 99% And
And a fourth step of immersing the film exposed to the water vapor in the non-solvent.
The polyether sulfone spherical particles are connected to each other on the first surface, the second surface or both to form pores, and the polyethylene glycol having a molecular weight of 200 is formed by steam-induced phase separation and inverse heat induced phase separation using as a pore forming agent of polyethersulfone And,
9. A porous film produced by the method of any one of claims 1 to 8.
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