CN114713038A - Micro-nano fiber membrane and preparation method and application thereof - Google Patents

Micro-nano fiber membrane and preparation method and application thereof Download PDF

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Publication number
CN114713038A
CN114713038A CN202210334295.0A CN202210334295A CN114713038A CN 114713038 A CN114713038 A CN 114713038A CN 202210334295 A CN202210334295 A CN 202210334295A CN 114713038 A CN114713038 A CN 114713038A
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China
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micro
spinning
membrane
solution
polystyrene
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Chinese (zh)
Inventor
李勃
刘奕博
王峰
张晗
莫宏宇
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Shenzhen Weidu New Material Co ltd
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Shenzhen Weidu New Material Co ltd
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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
    • B01D69/081—Hollow fibre membranes characterised by the fibre diameter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/08—Thickening liquid suspensions by filtration
    • B01D17/085—Thickening liquid suspensions by filtration with membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
    • B01D63/02—Hollow fibre modules
    • 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
    • B01D69/085—Details relating to the spinneret
    • 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
    • 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
    • B01D71/28—Polymers of vinyl aromatic compounds
    • 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
    • B01D71/30—Polyalkenyl halides
    • B01D71/32—Polyalkenyl halides containing fluorine atoms
    • B01D71/34—Polyvinylidene fluoride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/38—Hydrophobic membranes

Abstract

The application discloses micro-nanofiber membrane, micro-nanofiber membrane mainly comprises polymer nanofiber, polymer among the polymer nanofiber includes polyvinylidene fluoride and polystyrene, including nanometer grade fiber and micron order fibre among the micro-nanofiber membrane. The application micro-nano fiber membrane have better hydrophobic oleophylic characteristic, can remove oil to oily water effectively, can also filter the solid particle thing in the oil-water mixture and get rid of. In addition, the application also discloses a preparation method and application of the micro-nano fiber membrane.

Description

Micro-nano fiber membrane and preparation method and application thereof
Technical Field
The application relates to the technical field of filtering materials, in particular to a micro-nanofiber membrane and a preparation method and application of the micro-nanofiber membrane.
Background
The traditional preparation method of the nanofiber membrane is an electrostatic spinning method, polymer solution or melt is sprayed in a strong electric field, liquid drops at a needle head are changed into a Taylor cone from a spherical shape under the action of the electric field, and fiber filaments are obtained by extending from the tip of the cone. The spinning method can produce polymer filaments with nanometer-scale diameters, but has the problems of low efficiency, energy consumption, high pressure danger and the like.
The solution jet spinning technology is a new type of nanometer fiber preparing method, which is to dissolve polymer in solvent to prepare spinning solution, the spinning solution is extruded out of the spinneret orifice and simultaneously blown by surrounding high speed air flow, so that the solution trickle is stretched, and simultaneously the solvent is evaporated to form fiber. The solution jet spinning method has the advantages of high production efficiency, simple process, easy large-scale production and the like.
However, the filtration effect of the nanofiber membrane prepared by the solution jet spinning method on oily substances still needs to be improved.
Disclosure of Invention
In view of this, the present application provides a micro-nanofiber membrane, which aims at improving the filtering effect of the existing micro-nanofiber membrane on oily substances.
The embodiment of the application is realized like this, a micro-nanofiber membrane, micro-nanofiber membrane mainly comprises polymer nanofiber, polymer among the polymer nanofiber includes polyvinylidene fluoride and polystyrene, including nanofiber and micron order fibre in the micro-nanofiber membrane.
Optionally, in some embodiments of the present application, the diameter of the nano-scale fibers is greater than or equal to 800nm and less than 1000nm, and the diameter of the micro-scale fibers is 1 to 2 μm.
Optionally, in some embodiments of the present application, in the micro-nanofiber membrane, a mass ratio of the polystyrene to the polyvinylidene fluoride ranges from (0.025-40): 1.
optionally, in some embodiments of the present application, the micro-nanofiber membrane has an oil absorption multiplying power of 251-346 g/g.
Optionally, in some embodiments of the present application, a water contact angle of the micro-nanofiber membrane is greater than or equal to 137.2 °.
Correspondingly, the embodiment of the application also provides a preparation method of the micro-nanofiber membrane, which comprises the following steps:
dissolving polystyrene in a solvent to obtain a polystyrene solution;
adding polyvinylidene fluoride into the polystyrene solution to obtain spinning solution;
and spinning the spinning solution by adopting a solution jet spinning method, and collecting the spinning by using a collecting device to obtain the micro-nano fiber membrane, wherein the spinning distance is 15-100 cm, the air flow speed is 10-20 slpm, and the jet speed of the spinning solution is 20-30 mu L/min.
Optionally, in some embodiments of the present application, in the spinning solution, the mass concentration of the polyvinylidene fluoride is 1 to 40%, and the mass concentration of the polystyrene solution is 1 to 40%.
Optionally, in some embodiments herein, the solvent is selected from at least one of N, N-dimethylformamide, dimethyl sulfoxide, dimethylacetamide, N-methylpyrrolidone, triethyl phosphate, and acetone.
Optionally, in some embodiments of the present application, after dissolving the polystyrene in the solvent, the method further includes: stirring at the room temperature at the rotating speed of 60-1000 rpm for 0.1-12 h; or
After the polyvinylidene fluoride is added into the polystyrene solution, the method further comprises the following steps: stirring at a temperature of 50-70 ℃ and a rotating speed of 60-1000 rpm for 0.1-12 h.
Correspondingly, this application embodiment still provides an oil strain membrane, the oil strain membrane is above-mentioned micro-nanofiber membrane, perhaps, the oil strain membrane is the micro-nanofiber membrane who makes by above-mentioned preparation method.
Micro-nano fiber membrane have better hydrophobic oleophylic characteristic, can remove oil to oily water effectively, can also filter the solid particle thing of getting rid of in the oil-water mixture.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a flowchart of a method for preparing a micro-nanofiber membrane according to an embodiment of the present disclosure;
fig. 2 is an SEM image of the micro-nanofiber membrane in example 1 of the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. 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 application. Furthermore, it should be understood that the detailed description and specific examples, while indicating exemplary embodiments of the invention, are given by way of illustration and explanation only, and are not intended to limit the scope of the invention.
In the present application, unless indicated to the contrary, the use of the directional terms "upper" and "lower" generally refer to the upper and lower positions of the device in actual use or operation, and more particularly to the orientation of the figures of the drawings; while "inner" and "outer" are with respect to the outline of the device. In addition, in the description of the present application, the term "including" means "including but not limited to". The terms first, second, third and the like are used merely as labels, and do not impose numerical requirements or an established order. The term "plurality" means "two or more".
Various embodiments of the present application may exist in a range of forms; it is to be understood that the description in range format is merely for convenience and brevity and should not be construed as an inflexible limitation on the scope of the application; accordingly, the described range descriptions should be considered to have specifically disclosed all the possible sub-ranges as well as individual numerical values within that range. For example, it is contemplated that the description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the stated range, such as 1, 2, 3, 4, 5, and 6, as applicable regardless of the range. In addition, whenever a numerical range is indicated herein, it is meant to include any number (fractional or integer) recited within the indicated range.
The embodiment of the application provides a micro-nanofiber membrane, the micro-nanofiber membrane mainly comprises polymer nanofibers, and polymers in the polymer nanofibers mainly comprise polyvinylidene fluoride (PVDF) and Polystyrene (PS). In other words, the micro-nano fiber membrane is a PVDF/PS composite fiber membrane.
The micro-nano fiber membrane comprises nano-scale fibers and micron-scale fibers. The diameter range of the nano-scale fibers is more than or equal to 800nm and less than 1000nm, and the diameter range of the micro-scale fibers is 1-2 mu m. Therefore, the micro-nanofiber membrane has excellent hydrophobic and oleophylic properties, can effectively remove oil from oil-containing water, and can also filter and remove solid particles in an oil-water mixture.
In the micro-nano fiber membrane, the mass ratio of the polystyrene to the polyvinylidene fluoride is (0.025-40): 1. the micro-nano fiber membrane has excellent hydrophobic and oleophylic properties, and can effectively remove oil from oil-containing water.
In some embodiments, the micro-nanofiber membrane has an oil absorption multiplying power of 251-346 g/g.
In some embodiments, the micro-nanofiber membrane has a water contact angle of greater than or equal to 137.2 °.
Referring to fig. 1, an embodiment of the present application further provides a method for preparing a micro-nanofiber membrane, including the following steps:
step S01: dissolving polystyrene in a solvent to obtain a polystyrene solution;
step S02: adding polyvinylidene fluoride into the polystyrene solution to obtain spinning solution;
step S03: and spinning the spinning solution by adopting a solution jet spinning method, and collecting the spinning by using a collecting device to obtain the micro-nano fiber membrane, wherein the spinning interval is 15-100 cm, the air flow speed is 10-20 slpm, and the jet speed of the spinning solution is 20-30 mu L/min.
In step S01:
the solvent may be selected from, but not limited to, at least one of N, N-Dimethylformamide (DMF), dimethyl sulfoxide (DMSO), Dimethylacetamide (DMAC), N-methylpyrrolidone (NMP), triethyl phosphate (TEP), and acetone.
In some embodiments, said dissolving the polystyrene in the solvent further comprises: stirring at the room temperature at the rotating speed of 60-1000 rpm for 0.1-12 h. In this way, the polystyrene can be dissolved in the solvent sufficiently rapidly.
In the step S02:
in the spinning solution, the mass concentration of the polyvinylidene fluoride is 1-40%, and the mass concentration of the polystyrene solution is 1-40%. Above the range, a solution cannot be prepared. It is understood that the mass concentration refers to the mass of solute divided by the mass of the spinning solution.
In some embodiments, said adding polyvinylidene fluoride to said polystyrene solution further comprises: stirring at a temperature of 50-70 ℃ and a rotating speed of 60-1000 rpm for 0.1-12 h. In this way, the polyvinylidene fluoride can be sufficiently and rapidly dissolved in the solvent.
In at least one preferred embodiment, the mixture is stirred at a rotation speed of 60-1000 rpm for 0.1-12 h at a temperature of 60 ℃. At the temperature of 60 ℃, the polyvinylidene fluoride can be quickly dissolved in the solvent, and the solvent volatilization caused by overhigh temperature can be avoided.
In step S03:
the collecting device is a device known in the art for collecting the spun filaments and forming the filaments into a film. In at least one embodiment, the collection device is a drum.
It is understood that the spinning solution is ejected from the spinning nozzle, and the spinning distance is the distance between the spinning nozzle and the collecting device.
The embodiment of the application also provides an application of the micro-nano fiber membrane as an oil filter membrane.
The present application will be described in detail with reference to specific examples, which are intended to be part of the present application and are not intended to limit the present application.
Example 1
Dissolving 0.5g of polystyrene in a mixed solution of 3g of acetone and 7g of DMF, and stirring at room temperature at the rotating speed of 800rpm for 1h to obtain a polystyrene solution;
adding 1g of polyvinylidene fluoride into the polystyrene solution, and stirring at the rotating speed of 800rpm at 60 ℃ for 6 hours to obtain spinning solution;
and spinning the spinning solution by adopting a solution jet spinning method, and collecting the spinning by using a roller to obtain the micro-nano fiber membrane, wherein the spinning space is 30cm, the air flow speed is 15slpm, and the jet speed of the spinning solution is 20 mu L/min.
Example 2
Dissolving 0.5g of polystyrene in a mixed solution of 2g of acetone and 8g of DMF, and stirring at the room temperature at the rotating speed of 850rpm for 1.5h to obtain a polystyrene solution;
adding 1g of polyvinylidene fluoride into the polystyrene solution, and stirring at the rotating speed of 850rpm at 60 ℃ for 6.5 hours to obtain spinning solution;
and spinning the spinning solution by adopting a solution jet spinning method, and collecting the spinning by using a collecting device to obtain the micro-nano fiber membrane, wherein the spinning space is 25cm, the air flow speed is 15slpm, and the jet speed of the spinning solution is 20 muL/min.
Example 3
Dissolving 0.5g of polystyrene in a mixed solution of 1g of acetone and 9g of DMF, and stirring at the room temperature at the rotating speed of 750rpm for 1h to obtain a polystyrene solution;
adding 1g of polyvinylidene fluoride into the polystyrene solution, and stirring at the rotating speed of 850rpm at 60 ℃ for 6 hours to obtain spinning solution;
and spinning the spinning solution by adopting a solution jet spinning method, and collecting the spinning by using a collecting device to obtain the micro-nano fiber membrane, wherein the spinning space is 30cm, the air flow speed is 20slpm, and the jet speed of the spinning solution is 30 muL/min.
Example 4
Dissolving 0.5g of polystyrene in a mixed solution of 10g of DMF, and stirring at the room temperature at the rotating speed of 900rpm for 2 hours to obtain a polystyrene solution;
adding 1g of polyvinylidene fluoride into the polystyrene solution, and stirring at the rotating speed of 800rpm at 60 ℃ for 6.5 hours to obtain spinning solution;
and spinning the spinning solution by adopting a solution jet spinning method, and collecting the spinning by using a collecting device to obtain the micro-nano fiber membrane, wherein the spinning space is 25cm, the air flow speed is 15slpm, and the jet speed of the spinning solution is 20 muL/min.
Example 5
This example is substantially the same as example 1 except that the spinning pitch of this example is 40 cm.
Example 6
This example is substantially the same as example 1 except that the spinning pitch of this example is 55 cm.
Example 7
This example is substantially the same as example 1 except that the spinning pitch of this example is 70 cm.
Example 8
This example is substantially the same as example 1 except that the gas flow rate in this example is 10 slpm.
Example 9
This embodiment is substantially the same as embodiment 1 except that the gas flow rate of this embodiment is 15 slpm.
Example 10
This embodiment is substantially the same as embodiment 1 except that the gas flow rate of this embodiment is 20 slpm.
Example 11
This example is substantially the same as example 1 except that the spinning liquid jet speed of this example was 20. mu.L/min.
Example 12
This example is substantially the same as example 1 except that the spinning liquid jet speed of this example was 25. mu.L/min.
Example 13
This example is substantially the same as example 1 except that the spinning liquid jet speed of this example was 30. mu.L/min.
Comparative example
The fiber membrane of the present comparative example was a micron-sized carbon fiber membrane prepared by a solution jet spinning method.
Referring to fig. 2, the micro-nano fiber film of example 1 is scanned by SEM electron microscope to obtain an SEM image. As can be seen from fig. 2, the micro-nanofibers in the micro-nanofiber membrane of embodiment 1 are uniformly distributed, and include both the nano-fibers and the micro-fibers.
And (3) respectively detecting the water contact angle and the oil absorption multiplying power of the micro-nano fiber film of the embodiment 1-3 and the micron-sized carbon fiber film of the comparative example. Wherein, the water contact angle is detected by a water contact angle measuring instrument; the method for detecting the oil absorption multiplying power comprises the steps of fully soaking a certain mass of fiber membrane in a beaker filled with an oily substance solution for 12 hours, taking out the fiber membrane and standing for 5 min. The oil absorption multiplying power Q is calculated using the following formula: q ═ mt-m0)/m0In the formula, m0Is the initial mass of the fibrous membrane in g; m istThe mass of the fiber membrane after absorbing oil for 12 hours is g; the unit of Q is g/g. The detection results are shown in the first table.
Table one:
oil absorption multiplying power Water contact angle
Example 1 292 137.2°
Example 2 346 141.3°
Example 3 251 139.1°
Comparative example 192 N/A
From table one, it can be seen that: compared with the micron-sized carbon fiber film of the comparative example, the micro-nanofiber films of examples 1-3 have higher oil absorption multiplying power and larger water contact angle, and therefore the micro-nanofiber film has better hydrophobic and oleophilic characteristics and can effectively remove oil from oil-containing water.
The micro-nano fiber membrane and the preparation method thereof provided by the embodiment of the application are described in detail, a specific example is applied in the description to explain the principle and the implementation mode of the application, and the description of the embodiment is only used for helping to understand the method and the core idea of the application; meanwhile, for those skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.

Claims (10)

1. A micro-nano fiber membrane is characterized in that: the micro-nanofiber membrane mainly comprises polymer nanofibers, polymers in the polymer nanofibers comprise polyvinylidene fluoride and polystyrene, and the micro-nanofiber membrane comprises nano-scale fibers and micron-scale fibers.
2. The micro-nanofiber membrane of claim 1, wherein: the diameter range of the nano-scale fibers is more than or equal to 800nm and less than 1000nm, and the diameter range of the micro-scale fibers is 1-2 mu m.
3. The micro-nanofiber membrane of claim 1, wherein: in the micro-nano fiber membrane, the mass ratio of the polystyrene to the polyvinylidene fluoride is (0.025-40): 1.
4. the micro-nanofiber membrane of claim 1, wherein: the oil absorption multiplying power of the micro-nano fiber film is 251-346 g/g.
5. The micro-nanofiber membrane of claim 1, wherein: the water contact angle of the micro-nanofiber membrane is more than or equal to 137.2 degrees.
6. A preparation method of a micro-nanofiber membrane is characterized by comprising the following steps:
dissolving polystyrene in a solvent to obtain a polystyrene solution;
adding polyvinylidene fluoride into the polystyrene solution to obtain spinning solution;
spinning the spinning solution by adopting a solution jet spinning method, and collecting the spinning by using a collecting device to obtain the micro-nano fiber membrane, wherein the spinning distance is 15-100 cm, the air flow speed is 10-20 slpm, and the jet speed of the spinning solution is 20-30 mu L/min.
7. The method of claim 6, wherein: in the spinning solution, the mass concentration of the polyvinylidene fluoride is 1-40%, and the mass concentration of the polystyrene solution is 1-40%.
8. The method of claim 6, wherein: the solvent is at least one selected from N, N-dimethylformamide, dimethyl sulfoxide, dimethylacetamide, N-methylpyrrolidone, triethyl phosphate and acetone.
9. The method of claim 6, wherein: the method also comprises the following steps after the polystyrene is dissolved in the solvent: stirring at the rotating speed of 60-1000 rpm for 0.1-12 h at room temperature; or
After the polyvinylidene fluoride is added into the polystyrene solution, the method further comprises the following steps: stirring at a temperature of 50-70 ℃ and a rotating speed of 60-1000 rpm for 0.1-12 h.
10. An oil filter membrane is characterized in that: the oil filter membrane is the micro-nano fiber membrane according to any one of claims 1 to 5, or the oil filter membrane is the micro-nano fiber membrane prepared by the preparation method according to any one of claims 6 to 9.
CN202210334295.0A 2022-03-30 2022-03-30 Micro-nano fiber membrane and preparation method and application thereof Pending CN114713038A (en)

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