CN109289540B - Nanofiber porous filter membrane with micropore-nanopore structure and preparation method thereof - Google Patents
Nanofiber porous filter membrane with micropore-nanopore structure and preparation method thereof Download PDFInfo
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- CN109289540B CN109289540B CN201811109395.3A CN201811109395A CN109289540B CN 109289540 B CN109289540 B CN 109289540B CN 201811109395 A CN201811109395 A CN 201811109395A CN 109289540 B CN109289540 B CN 109289540B
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- B01D67/0002—Organic membrane manufacture
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Abstract
The invention discloses a nanofiber porous filter membrane with a micropore-nanopore structure and a preparation method thereof, belonging to the technical field of membrane separation. The preparation method comprises the steps of placing microspheres in a nanofiber suspension, stirring uniformly to obtain a mixed solution, carrying out vacuum filtration on the mixed solution to form a membrane, placing the membrane in a microsphere solution to completely remove the microspheres, and then cleaning and drying to obtain the nanofiber porous filter membrane with a micropore-nanopore structure. The preparation process is simple, the cost is low, the prepared porous filter membrane can be used for water filtration or air filtration without being compounded with a base material, and meanwhile, because the porous filter membrane has a multi-layer micropore and nanopore structure, the initial water flux reaches 1000L/m under the pressure of 0.02MPa in a filtration performance test2h, the retention rate of particles with the particle size of 50 nm-500 nm reaches 99.8 percent.
Description
Technical Field
The invention relates to a nanofiber porous membrane, belongs to the technical field of membrane separation, and particularly relates to a nanofiber porous filter membrane with a micropore-nanopore structure and a preparation method thereof.
Background
The nanofiber membrane is composed of nanofibers, has small pore diameter and high porosity, can effectively intercept particles in water and air, and is widely applied to the fields of biology, medicine, food, industry and the like, particularly to the aspects of water filtration and air filtration. The electrostatic spinning is a common method for preparing the nanofiber membrane, but the nanofiber porous membrane prepared by the method has a single structure and weak mechanical strength.
For example, the Chinese invention patent (No. CN103537198B, No. 2016-06-29) discloses a Kevlar nano fiber porous membrane, a preparation method and an application thereof. Dissolving Kevlar fiber in an organic solvent, adding an auxiliary agent and strong base, heating, stirring and dispersing to obtain a Kevlar nanofiber dispersoid; adding a pore-forming agent into the dispersion, uniformly stirring to form a membrane casting solution, and performing vacuum degassing for later use; coating the casting solution on a glass plate to form a film, evaporating the solvent, putting the film into a gel bath to obtain a gel film, and soaking the gel film in water; carrying out heat treatment on the soaked gel film to obtain a Kevlar nano fiber porous film with high strength, high temperature resistance and solvent resistance; the preparation method is mild, and the prepared nanofiber porous membrane keeps excellent performances of high strength, high modulus and solvent resistance, has a three-dimensional porous structure and is suitable for water treatment work in severe environments. However, the pore-forming agent adopted by the invention leads the finally prepared nano fiber porous membrane to have a single structure, and pores are easy to block in the actual use process.
The microsphere is used as a particle dispersion system, the definition of the microsphere in pharmaceutics refers to that a drug is dissolved or dispersed in a high molecular material to form a micro spherical entity with the particle size range of 1-500 micrometers, the micro spherical entity can be divided into nano microspheres and micro microspheres according to the size, the microsphere is mainly used as a microsphere preparation to be applied to the technical field of targeted drugs, the drug can be released at a required part in vivo, the effective concentration of the drug is improved, the drug concentration of other parts is correspondingly reduced, and the whole toxicity and adverse reaction of the drug are reduced.
In addition, the microspheres are also used for preparing a porous structure of a nanofiber material, for example, Chinese patent application (application publication No. CN102505400A, application publication date: 2012-06-20) discloses a preparation method of a porous nanofiber membrane, which comprises the steps of mixing a precursor solution with PS nanospheres to obtain an electrostatic spinning stock solution, carrying out electrostatic spinning on the electrostatic spinning stock solution to obtain a primary nanofiber membrane, putting the nanofiber membrane into a furnace body for calcining, and removing the PS nanospheres to obtain the porous nanofiber membrane. According to the invention, a certain amount of PS nano microspheres are added in the preparation process, so that the size and the diameter of pores in the porous nano fibers can be effectively controlled, however, the porous network structure is prepared on the nano fibers, and the nano fibers of the network structure have better charge transmission performance than nano particles, so that the photoelectric conversion efficiency is favorably improved.
Also for example, the journal ACS nano.voll 6.no.5.4020-4028.2012 discloses a 3D macroporous graphene supercapacitor frame with high energy and power density, and specifically discloses a method for constructing a three-dimensional macroporous structure of graphene by using polystyrene particles as a sacrificial material, wherein the graphene is continuously chemically modified on the basis of the three-dimensional macroporous structure, so that a porous graphene structure with a large area is prepared, and a material with the structure can promote rapid ion transmission in an electrode, and simultaneously keeps good electronic conductivity, and can be used as an energy storage device with high power and energy density.
However, the 2 reports mentioned above are all to improve the internal electron transfer efficiency by establishing a three-dimensional macroporous structure, and do not relate to the technical field of filtration membranes, and there is no report on the application of microspheres to filtration membranes at present.
Disclosure of Invention
In order to solve the technical problems, the invention discloses a nanofiber porous filter membrane which is simple in preparation process and simultaneously has a microporous structure and a nanoporous structure.
In order to achieve the aim, the invention discloses a preparation method of a nanofiber porous filter membrane with a micropore-nanopore structure, which comprises the steps of placing microspheres in a nanofiber suspension, uniformly stirring to obtain a mixed solution, carrying out vacuum filtration on the mixed solution to obtain a fiber membrane, placing the fiber membrane in a microsphere solution to completely remove the microspheres, cleaning and drying to obtain the nanofiber porous filter membrane with the micropore-nanopore structure.
Further, the temperature of the microsphere solution is controlled to be 30-100 ℃, and the microsphere is dissolved for 1-4 hours until the microsphere is completely removed.
Optimally, the temperature of the microsphere solution is controlled to be 30 ℃.
Optimally, the temperature of the microsphere solution is controlled to be 40 ℃.
Optimally, the temperature of the microsphere solution is controlled to be 50 ℃.
Optimally, the temperature of the microsphere solution is controlled to be 60 ℃.
Optimally, the temperature of the microsphere solution is controlled to be 70 ℃.
Optimally, the temperature of the microsphere solution is controlled to be 80 ℃.
Optimally, the temperature of the microsphere solution is controlled to be 90 ℃.
Optimally, the temperature of the microsphere solution is controlled to be 100 ℃.
Further, the microsphere solution is one of acetone, N, N-dimethylformamide, dichloromethane, toluene or chloroform.
Further, the mass ratio of the microspheres to the nanofiber suspension is 1: 10-1: 500.
Optimally, the mass ratio of the microspheres to the nanofiber suspension is 1: 20.
Furthermore, the microsphere is a polymethyl methacrylate sphere or a polystyrene sphere with the particle size of 500 nm-100 um.
Most preferably, the microspheres have a particle size of 10 μm.
Further, the nanofiber suspension is prepared by soaking nanofibers in an organic solvent and performing high-speed shearing and stirring, wherein the nanofibers are one of PVA-co-PE (polyvinyl alcohol ethylene copolymer), PA6 (nylon 6), PTT (polytrimethylene terephthalate), iPP (isotactic polypropylene), PE-co-GMA (polyethylene glycidyl methacrylate copolymer), PET (polyethylene terephthalate), PBT (polybutylene terephthalate), IPET-PEG (polyethylene terephthalate-co-ethylene isophthalate-polyethylene glycol) or POE (polyolefin elastomer), and the organic solvent is one of acetone, ethanol, isopropanol or diethyl ether.
Preferably, the mass ratio of the nano fibers to the organic solvent is controlled to be 0.1: 100-20: 100, the shearing rate is controlled to be 2000-10000 r/min, and the shearing time is controlled to be 10 s-5 min.
Further, the relative vacuum degree is controlled to be 0.01MPa to 1MPa during vacuum filtration, the filtration time is 30s to 30min, and after the vacuum filtration is finished, the air is dried at room temperature for 1 to 2 days to ensure that the organic solvent is completely removed.
In order to better realize the technical purpose of the invention, the invention also discloses the nanofiber porous filter membrane with the micropore-nanopore structure prepared by the preparation method.
Furthermore, the aperture of the micropores in the nanofiber porous filter membrane is 1-100 μm, and the aperture of the nanopores is 50-500 nm.
Most preferably, the pore diameter of the micropores in the nanofiber porous filter membrane is 10 μm, and the pore diameter of the nanopores is 120 nm.
Further, the thickness of the nanofiber porous filter membrane is 50-5000 microns.
Further, the initial water flux of the nanofiber porous filter membrane reaches 1000L/m under the pressure of 0.02MPa2h, the retention rate of particles with the particle size of 50 nm-500 nm is less than or equal to 99.8 percent.
The beneficial effects of the invention are mainly embodied in the following aspects:
1. the preparation method provided by the invention comprises the steps of uniformly dispersing microspheres in a nanofiber suspension, filtering in vacuum to obtain a fibrous membrane filled with microspheres inside, and removing the microspheres through simple chemical dissolution to obtain a filtering membrane filled with multiple layers of micropores and nano-pore structures inside;
2. the preparation method designed by the invention is simple in process operation, and the filtering performance of the nanofiber porous filter membrane can be regulated and controlled by controlling the particle size and the number of the microspheres;
3. the nanofiber porous filter membrane with the micropore-nanopore structure provided by the invention has a multilayer three-dimensional nanopore and micropore structure, can realize effective filtration without blocking internal gaps, has high mechanical performance strength, is not required to be compounded with a base material, can be directly used as a filter membrane, and has good application prospects in the aspects of water filtration, air filtration and the like.
4. The initial water flux of the nano-fiber porous filter membrane with the micropore-nanopore structure reaches 1000L/m under the pressure of 0.02MPa2h, the retention rate of particles with the particle size of 50 nm-500 nm is less than or equal to 99.8 percent.
Drawings
FIG. 1 is a sectional electron microscope image of a nanofiber porous membrane having a micro-pore-nano-pore structure according to example 1 of the present invention;
FIG. 2 is a surface electron microscope image of the nanofiber porous filter membrane of FIG. 1;
FIG. 3 is a pore size distribution diagram of the nanofiber porous filter membrane of FIG. 1;
FIG. 4 is a load-displacement test chart of the nanofiber porous filter membrane of FIG. 1;
FIG. 5 is a contact angle test chart of the nanofiber porous filter membrane of FIG. 1;
FIG. 6 is a schematic representation of the nanofiber porous filter membrane of FIG. 1.
Detailed Description
In order to better explain the invention, the following further illustrate the main content of the invention in connection with specific examples, but the content of the invention is not limited to the following examples.
Example 1
1) Soaking a PVA-co-PE nanofiber bundle (preferably prepared by a melt spinning technology) in isopropanol, wherein the mass ratio of the PVA-co-PE nanofiber bundle to the isopropanol is 0.1:100, shearing and stirring at a high speed to prepare a nanofiber suspension, and controlling the shearing rate to be 2000r/min and the shearing time to be 3 min;
2) adding polymethyl methacrylate (PMMA) soluble microspheres with the particle size of 20-100 microns and the average particle size of 60 microns into the nanofiber suspension prepared in the step 1), and uniformly mixing by magnetic stirring, wherein the mass ratio of the polymethyl methacrylate soluble microspheres to the nanofiber suspension is 1:500, the stirring time is 30min, and the stirring speed is 50r/min, so as to obtain a mixed solution;
3) performing vacuum filtration under the pressure of 0.03MPa, performing suction filtration on the mixed solution prepared in the step 2) to form a membrane, wherein the diameter of a suction filtration funnel is 5cm, the volume of the mixed solution is 25mL, and drying the membrane at room temperature for 24h after the suction filtration is completed to obtain a fiber membrane;
4) and (3) placing the fiber membrane prepared in the step 3) into an acetone solution, heating to remove the polymethyl methacrylate soluble microspheres, taking out, cleaning and drying, wherein the dissolving temperature is 30 ℃, and the dissolving time is 2 hours, thus obtaining the PVA-co-PE nanofiber porous filter membrane with the multilayer micropore-nanopore structure.
As can be seen from fig. 1, 2 and 6, the microporous structure and the nanoporous structure in the nanofiber porous filter membrane prepared by the present invention are distributed in a cross manner, and the distribution of each pore is uniform; as can be seen from FIG. 3, each well exhibited a normal distribution.
As can be seen from the figure 4, the PVA-co-PE nanofiber porous filter membrane prepared by the method has better mechanical strength and tensile property.
As can be seen from FIG. 5, the PVA-co-PE nanofiber porous filter membrane prepared by the method has a contact angle of 85 degrees and has certain hydrophilicity.
And, the filter membrane prepared above was subjected to filtration performance test: under the pressure of 0.02MPa, the initial water flux reaches 1000L/m2h, the retention rate of particles with the particle size of 50 nm-500 nm reaches 99.8 percent.
Example 2
The embodiment discloses a preparation method of a nanofiber porous filter membrane with a micropore-nanopore structure, which comprises the following preparation steps:
1) soaking a PA6 nanofiber bundle (preferably prepared by a melt spinning technology) in isopropanol, wherein the mass ratio of the PA6 nanofiber bundle to the isopropanol is 0.5:100, carrying out high-speed shearing and stirring to prepare a nanofiber suspension, and controlling the shearing rate to be 5000r/min and the shearing time to be 1 min;
2) adding Polystyrene (PS) soluble microspheres with the particle size of 500 micrometers into the nanofiber suspension prepared in the step 1), and uniformly mixing by magnetic stirring, wherein the mass ratio of the PS soluble microspheres to the nanofiber suspension is 2:500, the stirring time is 30min, and the stirring speed is 30r/min, so as to obtain a mixed solution;
3) performing vacuum filtration under the pressure of 0.05MPa, performing suction filtration on the mixed solution prepared in the step 2) to form a membrane, wherein the diameter of a suction filtration funnel is 5cm, the volume of the mixed solution is 30mL, and drying the membrane at room temperature for 24h after the suction filtration is completed to obtain a fiber membrane;
4) and (3) placing the fiber membrane prepared in the step 3) into a toluene solution, heating to remove the polystyrene soluble microspheres, wherein the dissolving temperature is 30 ℃, the dissolving time is 3 hours, taking out, cleaning and drying to obtain the PA6 nano fiber porous filter membrane with the multilayer micropore-nanopore structure.
Example 3
The embodiment discloses a preparation method of a nanofiber porous filter membrane with a micropore-nanopore structure, which comprises the following preparation steps:
1) soaking a PET-co-GMA nano fiber bundle (preferably prepared by a melt spinning technology) in isopropanol, wherein the mass ratio of the PET-co-GMA nano fiber bundle to the isopropanol is 2:100, carrying out high-speed shearing and stirring to prepare a nano fiber suspension, and controlling the shearing rate to be 8000r/min and the shearing time to be 1 min;
2) adding Polystyrene (PS) soluble microspheres with the particle size of 200 mu m into the nanofiber suspension prepared in the step 1), and uniformly mixing by magnetic stirring, wherein the mass ratio of the PS soluble microspheres to the nanofiber suspension is 3:500, the stirring time is 10min, and the stirring speed is 25r/min, so as to obtain a mixed solution;
3) performing vacuum filtration under the pressure of 0.045MPa, performing suction filtration on the mixed solution prepared in the step 2) to form a membrane, wherein the diameter of a suction filtration funnel is 10cm, the volume of the mixed solution is 50mL, and drying the membrane at room temperature for 24h after the suction filtration is completed to obtain a fiber membrane;
4) and (3) placing the fiber membrane prepared in the step 3) into a toluene solution, heating to remove the polystyrene soluble microspheres, taking out, cleaning and drying, wherein the dissolving temperature is 50 ℃, and the dissolving time is 2 hours, thus obtaining the PET-co-GMA nano fiber porous filter membrane with the multilayer micropore-nanopore structure.
Example 4
The embodiment discloses a preparation method of a nanofiber porous filter membrane with a micropore-nanopore structure, which comprises the following preparation steps:
1) soaking a POE nano fiber bundle (preferably prepared by a melt spinning technology) in ether, wherein the mass ratio of the POE nano fiber bundle to isopropanol is 5:100, shearing and stirring at a high speed to prepare a nano fiber suspension, and controlling the shearing rate to be 10000r/min and the shearing time to be 30 s;
2) adding Polystyrene (PS) soluble microspheres with the particle size of 300 microns into the nanofiber suspension prepared in the step 1), and uniformly mixing by magnetic stirring, wherein the mass ratio of the PS soluble microspheres to the nanofiber suspension is 20:500, the stirring time is 60min, and the stirring speed is 50r/min, so as to obtain a mixed solution;
3) performing vacuum filtration under the pressure of 0.02MPa, performing suction filtration on the mixed solution prepared in the step 2) to form a membrane, wherein the diameter of a suction filtration funnel is 20cm, the volume of the mixed solution is 50mL, and drying the membrane at room temperature for 24h after the suction filtration is completed to obtain a fiber membrane;
4) and (3) placing the fiber membrane prepared in the step 3) into a chloroform solution, heating to remove the polystyrene soluble microspheres, wherein the dissolving temperature is 40 ℃, the dissolving time is 2 hours, taking out, cleaning and drying to obtain the POE nano fiber porous filter membrane with the multilayer micropore-nanopore structure.
Example 5
The embodiment discloses a preparation method of a nanofiber porous filter membrane with a micropore-nanopore structure, which comprises the following preparation steps:
1) the preparation method comprises the following steps of (1) soaking a PTT nano fiber bundle (preferably prepared by a melt spinning technology) in isopropanol, wherein the mass ratio of the PTT nano fiber bundle to the isopropanol is 10:100, carrying out high-speed shearing and stirring to prepare a nano fiber suspension, controlling the shearing rate to be 5000r/min, and controlling the shearing time to be 5 min;
2) adding Polystyrene (PS) soluble microspheres with the particle size of 600 microns into the nanofiber suspension prepared in the step 1), and uniformly mixing by magnetic stirring, wherein the mass ratio of the PS soluble microspheres to the nanofiber suspension is 30:500, the stirring time is 60min, and the stirring speed is 50r/min, so as to obtain a mixed solution;
3) performing vacuum filtration under the pressure of 0.08MPa, performing suction filtration on the mixed solution prepared in the step 2) to form a membrane, wherein the diameter of a suction filtration funnel is 5cm, the volume of the mixed solution is 30mL, and drying the membrane at room temperature for 24h after the suction filtration is completed to obtain a fiber membrane;
4) and (3) placing the fiber membrane prepared in the step 3) in a tetrachloroethane solution, heating to remove the polystyrene soluble microspheres, wherein the dissolving temperature is 50 ℃, the dissolving time is 2 hours, taking out, cleaning and drying to obtain the PTT nano fiber porous filter membrane with the multilayer micropore-nanopore structure.
Example 6
The embodiment discloses a preparation method of a nanofiber porous filter membrane with a micropore-nanopore structure, which comprises the following preparation steps:
1) soaking an IPET-PEG nano fiber bundle (preferably prepared by a melt spinning technology) in ethanol, wherein the mass ratio of the IPET-PEG nano fiber bundle to the ethanol is 20:100, carrying out high-speed shearing and stirring to prepare a nano fiber suspension, and controlling the shearing rate to be 5000r/min and the shearing time to be 3 min;
2) adding Polystyrene (PS) soluble microspheres with the particle size of 800 microns into the nanofiber suspension prepared in the step 1), and uniformly mixing by magnetic stirring, wherein the mass ratio of the PS soluble microspheres to the nanofiber suspension is 50:500, the stirring time is 60min, and the stirring speed is 50r/min, so as to obtain a mixed solution;
3) performing vacuum filtration under the pressure of 0.9MPa, performing suction filtration on the mixed solution prepared in the step 2) to form a membrane, wherein the diameter of a suction filtration funnel is 5cm, the volume of the mixed solution is 30mL, and drying the membrane at room temperature for 24h after the suction filtration is completed to obtain a fiber membrane;
4) placing the fiber membrane prepared in the step 3) in a styrene solution, heating to remove the polystyrene soluble microspheres, wherein the dissolving temperature is 40 ℃, the dissolving time is 2 hours, taking out, cleaning and drying to obtain the IPET-PEG nano fiber porous filter membrane with the multilayer micropore-nanopore structure.
The embodiment shows that the nanofiber porous filter membrane with the micropore-nanopore structure is prepared, the porous filter membrane simultaneously has multiple layers of three-dimensional nanopores and micropore structures, effective filtration can be realized, internal gaps are not blocked, the nanofiber porous filter membrane has high mechanical performance strength, the nanofiber porous filter membrane is not required to be compounded with a base material, the nanofiber porous filter membrane can be directly used as a filter membrane, and the nanofiber porous filter membrane has good application prospects in the aspects of water filtration, air filtration and the like.
The above examples are merely preferred examples and are not intended to limit the embodiments of the present invention. In addition to the above embodiments, the present invention has other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (9)
1. A preparation method of a nanofiber porous filter membrane with a micropore-nanopore structure is characterized by comprising the following steps: the preparation method comprises the steps of placing microspheres in a nanofiber suspension, stirring uniformly to obtain a mixed solution, carrying out vacuum filtration on the mixed solution to obtain a fibrous membrane, placing the fibrous membrane in a microsphere dissolving solution to dissolve and remove the microspheres, and cleaning and drying to obtain the nanofiber porous filter membrane with a micropore-nanopore structure.
2. The method of claim 1, wherein the step of preparing the nanofiber porous membrane having a micro-nano pore structure comprises: and controlling the temperature of the microsphere solution to be 30-100 ℃, and dissolving for 1-4 hours until the microspheres are completely removed.
3. The method for preparing a nanofiber porous membrane having a micro-nano pore structure as set forth in claim 1 or 2, wherein: the microsphere solution is one of acetone, N, N-dimethylformamide, dichloromethane, toluene or chloroform.
4. The method for preparing a nanofiber porous membrane having a micro-nano pore structure as set forth in claim 1 or 2, wherein: the mass ratio of the microspheres to the nanofiber suspension is 1: 10-1: 500.
5. The method of claim 4, wherein the step of preparing the nanofiber porous membrane having a micro-nano pore structure comprises: the microsphere is a polymethyl methacrylate sphere or a polystyrene sphere with the particle size controlled between 500nm and 100 mu m.
6. The method of claim 4, wherein the step of preparing the nanofiber porous membrane having a micro-nano pore structure comprises: the nanofiber suspension is prepared by soaking nanofibers in an organic solvent and carrying out high-speed shearing and stirring, wherein the nanofibers are one of PVA-co-PE, PA6, PTT, iPP, PE-co-GMA, PET, PBT, IPET-PEG or POE, and the organic solvent is one of acetone, ethanol, isopropanol or diethyl ether.
7. A nanofiber porous filter membrane having a micro-nano pore structure, comprising: the catalyst is prepared by the preparation method of any one of claims 1 to 6.
8. The nanofiber porous membrane having a micro-nano pore structure as set forth in claim 7, wherein: the pore diameter of the micropores in the nanofiber membrane is 0.5-100 mu m, and the pore diameter of the nanopores is 50-300 nm.
9. The nanofiber porous membrane having a micro-nano pore structure as set forth in claim 7, wherein: the initial water flux of the nanofiber porous filter membrane reaches 1000L/m under the pressure of 0.02MPa2h, the retention rate of particles with the particle size of 50 nm-500 nm is less than or equal to 99.8 percent.
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