CN114515516B - High-flux corrugated PDMS nanofiber composite membrane and preparation method thereof - Google Patents
High-flux corrugated PDMS nanofiber composite membrane and preparation method thereof Download PDFInfo
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- CN114515516B CN114515516B CN202210098880.5A CN202210098880A CN114515516B CN 114515516 B CN114515516 B CN 114515516B CN 202210098880 A CN202210098880 A CN 202210098880A CN 114515516 B CN114515516 B CN 114515516B
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
- B01D61/362—Pervaporation
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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
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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
- B01D71/70—Polymers having silicon in the main chain, with or without sulfur, nitrogen, oxygen or carbon only
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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
- B01D2325/08—Patterned membranes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a high-flux corrugated PDMS nanofiber composite membrane, which comprises a substrate and a surface layer, wherein the surface layer is a corrugated PDMS membrane, the substrate is a porous nanofiber material with a plurality of strip-shaped protruding structures which are randomly distributed, and the protruding structures are mutually intersected to form a plurality of concave areas. According to the invention, the PDMS casting solution is coated on the electrospun nanofiber substrate to easily manufacture the defect-free and submicron thin PDMS film, wherein the convex structure and the concave area on the surface of the substrate can conduct the structural shape of the bottom layer to the PDMS film, so that the PDMS film is corrugated, and the manufactured corrugated PDMS composite film has the advantages of high flux, no need of a specific substrate die and low transmission resistance, and is simple in preparation process.
Description
Technical Field
The invention belongs to the technical field of fiber composite membranes, and particularly relates to a high-flux corrugated PDMS nanofiber composite membrane and a preparation method thereof.
Background
Polydimethylsiloxane (PDMS) is a standard membrane material for permeation, gas separation and nanofiltration, and has wide application in pervaporation, gas separation and nanofiltration processes. For practical applications, there is always a need for high flux PDMS membranes to improve the efficiency of the separation process. Currently, there are two approaches to control the geometric appearance of membranes in an effort to alter the membrane geometry to increase flux.
The first approach is to make the film as thin as possible, which can produce an ultra thin film of about 100 a nm a thick, but it tends to reduce the selectivity, making the film defective. The second method is to pattern the composite membrane surface, and increase the permeation flux by increasing the membrane surface roughness or the membrane effective area. Reference journal Journal of Membrane Science, "Mass transfer in corrugated membranes", cussler et al, manufactured a high ripple PDMS membrane for pervaporation experiments and validated a modified Thiele model for membrane mass transfer, and found that the ripple membrane structure resulted in a doubling of flux compared to a flat plate membrane, however, no selective permeation was reported in such PDMS membrane, which did not preclude the effect of defects on membrane flux increase. Furthermore, such high flux PDMS membranes are not effective in separating molecular mixtures. Reference journal Journal of Membrane Science, "Fabrication and characterization of micro-patterned PDMS composite membranes for enhanced ethanol recovery," Li Jiding et al, discloses that the high throughput of patterned films is due to the increase in effective film area compared to non-patterned films by preparing a PDMS selective layer using different crosslinkers (p-tolyltriethoxysilane, p-TTES; triethoxyvinylsilane, VTES; tetraethyl orthosilicate, TEOS).
It follows that the fabrication of high throughput PDMS membranes consists in depositing a thinner membrane layer and creating a patterned membrane surface where possible, however, achieving a submicron thin PDMS membrane using a conventional macroporous substrate (e.g., average pore size >100 nm) remains a great challenge, as permeation of the PDMS coating into the substrate macropores often results in excessive transition layer thickness or membrane layer defects, thereby reducing membrane separation performance, and furthermore, current methods of fabricating patterned PDMS membranes are complex or fail to exhibit good separation performance for molecular mixtures. In view of this, it is necessary to study a high-flux corrugated PDMS nanofiber composite membrane and a method of preparing the same.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide the high-flux corrugated PDMS nanofiber composite membrane and the preparation method thereof, and the prepared corrugated PDMS composite membrane has the advantages of high flux, no need of a specific substrate die and low transmission resistance.
In order to achieve the above object, the present invention adopts the following technical scheme:
the high-flux corrugated PDMS nanofiber composite membrane comprises a substrate and a surface layer, wherein the surface layer is a corrugated PDMS membrane, the substrate is a porous nanofiber material with a plurality of strip-shaped protruding structures which are randomly distributed, and the protruding structures are mutually intersected to form a plurality of concave areas.
Preferably, the height of the protruding structures is 230-260 nm, and the average diameter of the recessed areas is 160-280 nm.
Still more preferably, the thickness of the surface layer is 0.5 to 2.5 μm.
The preparation method of the high-flux corrugated PDMS nanofiber composite membrane comprises the following specific steps:
s1, obtaining a substrate;
s2, dissolving PDMS, a catalyst and a cross-linking agent in a solvent, applying the solvent to the surface of a substrate, and performing film forming treatment to obtain the composite film.
Preferably, the aforementioned substrate is prepared by the following method: dissolving a polymer in an organic solvent to obtain a spinning solution; preparing an electrospun nanofiber substrate from the spinning solution by an electrostatic spinning method, and performing hot pressing treatment to obtain a substrate.
Still preferably, the polymer is one of polyvinylidene fluoride, polyethersulfone, polysulfone or polyacrylonitrile, and the organic solvent is one or more of acetone, dichloromethane, N-dimethylformamide or tetrahydrofuran.
More preferably, the organic solvent is N, N-dimethylformamide and acetone in a volume ratio of (4 to 6): and (1-2).
Further preferably, the mass fraction of the polymer in the spinning solution is 8-15 wt%; the injection speed of the injector is kept at 0.1-1 mL/min; the speed of the rotary collector is 300 rpm, the voltage is set to be 5-20 kV, the collector is 10-20 cm away from the metal needle, the temperature of the electrostatic spinning process is 25-50 ℃, and the relative humidity is 40-50%; the hot pressing temperature is 25-80 ℃, and the hot pressing pressure is 1-9 Mpa.
Specifically, the catalyst is one of dibutyl tin dilaurate or dimethyl phthalate, the cross-linking agent is one of tetraethoxysilane, vinyl trimethoxysilane or phenyl triethoxysilane, and the solvent is one or a mixture of more of n-heptane, n-hexane, n-octane, acetone or triethanolamine.
Preferably, the mass ratio of the catalyst, the cross-linking agent and the PDMS is (1-3): (10-16): (100-120).
The invention has the advantages that: according to the invention, a PDMS film casting solution is coated on an electrospun nanofiber substrate to easily manufacture a defect-free and submicron thin PDMS film, wherein the convex structures and the concave areas on the surface of the substrate can conduct the structural shape of the bottom layer to the PDMS film, so that the PDMS film is corrugated, meanwhile, the strip-shaped convex structures on the surface of the substrate are mutually intersected to effectively prevent the PDMS solvent from excessively penetrating into the concave areas of the substrate, and the manufactured corrugated PDMS composite film has the advantages of high flux, no need of a specific substrate die and low transmission resistance, and is simple in preparation process; the corrugated form of the PDMS membrane effectively increases the surface area of the composite membrane, thereby effectively improving the separation performance of the membrane.
Drawings
FIG. 1 is an SEM image of a substrate after heat press post-treatment of S1 to S9 in test 1 of the present invention;
FIG. 2 is a graph of the pervaporation performance test of PDMS composite membranes prepared under the substrate of recessed regions of different average diameters in test 2 of the present invention;
FIG. 3 is an SEM image of (a, c) defect-free PDMS film layer (a, d), a cross-sectional view (b, e) and an elemental EDX map of Si (c, f) formed on a substrate having recessed regions of different average diameters in test 2 of the present invention;
FIG. 4 is an SEM image of the surface (a, c) and cross-section (d, f) of a PDMS nanofiber composite membrane of test 3 of the present invention;
fig. 5 is an AFM image of a smooth PDMS film (a) and a corrugated PDMS film (b, c) in test 3 of the present invention.
Detailed Description
The invention is described in detail below with reference to the drawings and the specific embodiments.
The high-flux corrugated PDMS nanofiber composite membrane comprises a substrate and a surface layer, wherein the surface layer is a corrugated PDMS membrane, the substrate is a porous nanofiber material with a plurality of strip-shaped protruding structures which are randomly distributed, and the protruding structures are mutually intersected to form a plurality of concave areas. The height of the protruding structure is 230-260 nm, the average diameter of the recessed area is 160-280 nm, and the thickness of the surface layer is 0.5-2.5 mu m.
The preparation method of the high-flux corrugated PDMS nanofiber composite membrane comprises the following specific steps:
s1, obtaining a substrate;
s2, dissolving PDMS, a catalyst and a cross-linking agent in a solvent, applying the solvent to the surface of a substrate, and performing film forming treatment to obtain the composite film.
The substrate is prepared by the following method: dissolving a polymer in an organic solvent to obtain a spinning solution; preparing an electrospun nanofiber substrate from the spinning solution by an electrostatic spinning method, and performing hot pressing treatment to obtain a substrate. Wherein the polymer is one of polyvinylidene fluoride, polyethersulfone, polysulfone or polyacrylonitrile, and the organic solvent is one or a mixture of more of acetone, dichloromethane, N-dimethylformamide or tetrahydrofuran. The organic solvent is N, N-dimethylformamide and acetone according to the volume ratio of (4-6): and (1-2). The mass fraction of the polymer in the spinning solution is 8-15wt%; the injection speed of the injector is kept at 0.1-1 mL/min; the speed of the rotary collector is 300 rpm, the voltage is set to be 5-20 kV, the collector is 10-20 cm away from the metal needle, the temperature of the electrostatic spinning process is 25-50 ℃, and the relative humidity is 40-50%; the hot pressing temperature is 25-80 ℃, and the hot pressing pressure is 1-9 Mpa.
The film forming treatment in the step S2 is followed by drying treatment, the catalyst is one of dibutyl tin dilaurate or dimethyl phthalate, the cross-linking agent is one of tetraethoxysilane, vinyl trimethoxy silane or phenyl triethoxy silane, and the solvent is one or a mixture of more of n-heptane, n-hexane, n-octane, acetone or triethanolamine. The mass ratio of the catalyst to the crosslinking agent to the PDMS is (1-3): (10-16): (100-120).
Performance test
1. Influence of hot pressing conditions on substrate properties
In order to adjust the stripe-shaped protrusion structures and the concave regions of the substrate and improve the mechanical strength, the electrospun nanofiber substrate is subjected to hot pressing treatment under different pressures and temperatures, the performance of the substrate prepared under different hot pressing conditions is detected, and a comparative example C1 is provided, wherein the electrospun nanofiber substrate which is not subjected to hot pressing treatment is selected as the comparative example, and the characteristics and the operation conditions of the substrates in S1-S9 and C1 are shown in Table 1, it can be observed that the increase of the hot pressing pressure and the temperature generates a more compact and rigid substrate structure, the reduction of the average diameter of the concave regions is realized, however, the increase of the transmission resistance is caused, and if the average of the concave regions of the substrate is too large, a defect-free film is difficult to generate on the surface of the substrate. In addition, after hot pressing at different pressures and temperatures, the water contact angle of the substrate is basically unchanged, the surface of the substrate has strong hydrophobicity, the water contact angle is 120 DEG larger, the surface of the substrate can cause nonpolar liquid (such as PDMS/n-heptane coating solution) to be easy to wet, and defect-free film layer is formed, so that the PDMS casting solution can be directly coated on the surface of the substrate to form defect-free and thin PDMS film layer.
The surface morphology of the substrate in S1-S9 is shown in FIG. 1, and it can be seen that the substrate has a plurality of strip-shaped protruding structures, the strip-shaped protruding structures cross and interpenetrate to form a concave area, and no thick skin layer is formed, and the structure of the substrate is beneficial to forming a corrugated polymer coating and low transmission resistance.
TABLE 1 Properties of substrates prepared under different Hot pressing conditions
2. Influence of average diameter of substrate recessed region on characteristics of PDMS nanofiber composite membrane
The pervaporation performance of PDMS composite membranes prepared under substrates using recessed regions of different average diameters was examined, and the results of the examination are shown in FIG. 2, it can be observed that the total flux of these corrugated PDMS composite membranes was 1.9 to 3.9 kg m when 5wt% ethanol/water mixture was separated at a feed temperature of 40 ℃ -2 h -1 The separation coefficient exceeds 7.
PDMS films were prepared on the substrate of S3 in test 1 (the average diameter of the recessed area was 259 nm), and as shown in fig. 3a-c, a defect-free PDMS film layer was formed on the substrate, which was extremely rough and in a corrugated structure from the surface morphology of the composite film. Further increasing the average diameter of the recessed areas of the substrate beyond 300 nm, the PDMS film layer was defective (see fig. 3 d-e), resulting in a significant drop in the separation factor of the ethanol/water solution to 5.83 (see fig. 2), which is lower than the intrinsic selectivity of the PDMS film material, as evidenced by EDX diffraction of the Si element (from PDMS) along the cross-sectional view of the PDMS/PVDF nanofiber composite film (fig. 3c, f), the intrusion of the PDMS coating into the substrate with an average diameter of the recessed areas of about 307 nm was more pronounced than the coating on the substrate with an average diameter of the recessed areas of about 259 nm.
Influence of PDMS film layer thickness on PDMS nanofiber composite Membrane Properties
Defect-free PDMS film layers of different thicknesses of 2.5 μm, 1.5 μm and 0.5 μm were successfully prepared on the S3 substrate in test 1, and at least three film samples were observed through fig. 4, and if the film thickness was less than 0.5 μm, defects were more easily formed, and in addition, the reproducibility of film fabrication was lower and the mechanical stability was reduced. From fig. 4a-c, it can be seen that the ripple morphology of the PDMS film layer gradually emerges as the thickness of the PDMS film layer gradually decreases, and further monitoring the surface morphology of these PDMS composite films by AFM, see fig. 5, can confirm that the strip-shaped raised structures and recessed areas of the substrate create a ripple film surface, which effectively increases the film surface area by a factor of 2-3 as the thickness of the PDMS film layer decreases.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be appreciated by persons skilled in the art that the above embodiments are not intended to limit the invention in any way, and that all technical solutions obtained by means of equivalent substitutions or equivalent transformations fall within the scope of the invention.
Claims (4)
1. The application of the high-flux corrugated PDMS nanofiber composite membrane in ethanol/water solution separation is characterized in that the high-flux corrugated PDMS nanofiber composite membrane comprises a substrate and a surface layer, wherein the surface layer is a corrugated PDMS membrane, the substrate is a porous nanofiber material with a plurality of strip-shaped protruding structures which are randomly distributed, and the strip-shaped protruding structures are mutually intersected to form a plurality of concave areas;
the height of the convex structure is 230-260 nm, and the average diameter of the concave region is 160-280 nm;
the thickness of the surface layer is 0.5-2.5 mu m;
the preparation method of the high-flux corrugated PDMS nanofiber composite membrane comprises the following specific steps:
s1, obtaining a substrate;
s2, dissolving PDMS, a catalyst and a cross-linking agent in a solvent, applying the solvent to the surface of a substrate, and obtaining a composite film after film forming treatment;
the substrate is prepared by the following steps: dissolving a polymer in an organic solvent to obtain a spinning solution; preparing an electrospun nanofiber substrate from a spinning solution by an electrostatic spinning method, and performing hot pressing treatment to obtain a substrate; the mass ratio of the catalyst to the crosslinking agent to the PDMS is (1-3): (10-16): (100-120);
the mass fraction of the polymer in the spinning solution is 8-15wt%; the injection speed of the injector is kept at 0.1-1 mL/min; the speed of the rotary collector is 300 rpm, the voltage is set to be 5-20 kV, the collector is 10-20 cm away from the metal needle, the temperature of the electrostatic spinning process is 25-50 ℃, and the relative humidity is 40-50%; the hot pressing temperature is 25-80 ℃, and the hot pressing pressure is 1-9 MPa.
2. The use according to claim 1, wherein the polymer is one of polyvinylidene fluoride, polyethersulfone, polysulfone or polyacrylonitrile, and the organic solvent is one or a mixture of several of acetone, dichloromethane, N-dimethylformamide or tetrahydrofuran.
3. The use according to claim 2, wherein the organic solvent is N, N-dimethylformamide and acetone in a volume ratio (4-6): and (1-2).
4. The use according to claim 1, wherein the catalyst is dibutyltin dilaurate, the cross-linking agent is one of ethyl orthosilicate, vinyl trimethoxysilane or phenyl triethoxysilane, and the solvent is one or a mixture of several of n-heptane, n-hexane, n-octane, acetone or triethanolamine.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1655927A (en) * | 2002-05-27 | 2005-08-17 | 帝人杜邦菲林日本株式会社 | Releasing film |
| CN101530010A (en) * | 2006-10-18 | 2009-09-09 | 3M创新有限公司 | Methods of patterning a material on polymeric substrates |
| CN105731364A (en) * | 2016-02-29 | 2016-07-06 | 天津大学 | PDMS elastomer micro-nano processing method based on surface oxidation control transfer printing |
| CN110033900A (en) * | 2019-04-09 | 2019-07-19 | 深圳市华星光电技术有限公司 | Flexible conductive film and preparation method thereof, display panel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US10589216B2 (en) * | 2014-11-13 | 2020-03-17 | Ohio State Innovation Foundation | Membranes for fluid separation |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1655927A (en) * | 2002-05-27 | 2005-08-17 | 帝人杜邦菲林日本株式会社 | Releasing film |
| CN101530010A (en) * | 2006-10-18 | 2009-09-09 | 3M创新有限公司 | Methods of patterning a material on polymeric substrates |
| CN105731364A (en) * | 2016-02-29 | 2016-07-06 | 天津大学 | PDMS elastomer micro-nano processing method based on surface oxidation control transfer printing |
| CN110033900A (en) * | 2019-04-09 | 2019-07-19 | 深圳市华星光电技术有限公司 | Flexible conductive film and preparation method thereof, display panel |
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