CN115025645A - Preparation method of super-hydrophilic and super-oleophobic nanofiber membrane in air - Google Patents

Preparation method of super-hydrophilic and super-oleophobic nanofiber membrane in air Download PDF

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CN115025645A
CN115025645A CN202210958131.5A CN202210958131A CN115025645A CN 115025645 A CN115025645 A CN 115025645A CN 202210958131 A CN202210958131 A CN 202210958131A CN 115025645 A CN115025645 A CN 115025645A
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super
electrostatic spinning
fiber membrane
solvent
air
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李斐然
潘昀路
霍天威
赵学增
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Harbin Institute of Technology
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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
    • B01D71/38—Polyalkenylalcohols; Polyalkenylesters; Polyalkenylethers; Polyalkenylaldehydes; Polyalkenylketones; Polyalkenylacetals; Polyalkenylketals
    • 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
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0081—After-treatment of organic or inorganic membranes
    • 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
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • 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
    • B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
    • B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/39—Electrospinning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/36—Hydrophilic membranes
    • 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
    • Y02A20/20—Controlling water pollution; Waste water treatment
    • Y02A20/204—Keeping clear the surface of open water from oil spills

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nanotechnology (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

The invention relates to the field of preparation of nanofiber membranes, in particular to a preparation method of a super-hydrophilic and super-oleophobic nanofiber membrane in air. S1, adding polyvinyl butyral into a solvent to prepare an electrostatic spinning solution; s2, carrying out electrostatic spinning on the electrostatic spinning solution to obtain a fiber membrane; and S3, removing residual solvent on the surface of the fiber membrane to obtain the super-oleophobic and super-hydrophilic super-infiltrated nano-fiber membrane in the air. The purpose is to provide a nanofiber membrane which can have the characteristics of super-hydrophilicity and super-oleophobicity in air.

Description

Preparation method of super-hydrophilic and super-oleophobic nanofiber membrane in air
Technical Field
The invention relates to the field of preparation of nanofiber membranes, in particular to a preparation method of a super-hydrophilic and super-oleophobic nanofiber membrane in air.
Background
In recent years marine oil spill accidents and the discharge of industrial oily waste water have put increasing pressure on the ecological environment. Compared with the traditional oil-water separation technology, the selective super-infiltration membrane is more and more favored by people to separate the oil-water mixture.
The selective super-wetting membrane has opposite wetting characteristics to oil and water, and can intercept one phase and enable the other phase to pass through smoothly, so that oil-water separation is realized. The super-wetting membrane for realizing the mode of water and oil passing resistance has super-hydrophilic underwater super-oleophobic membrane and super-oleophobic membrane in super-hydrophilic air, and compared with the defects that the underwater super-oleophobic membrane needs to be pre-wetted and is easy to be polluted after a water membrane is broken, the super-oleophobic membrane in air has the characteristics of simple use condition and more stable dirt resistance. The immiscible oil-water mixture and the emulsion can be stably separated. Therefore, the development of the nanofiber membrane with super-hydrophilicity and super-lipophobicity in the air is of great significance.
Disclosure of Invention
The invention provides a preparation method of a nano-fiber membrane with super-hydrophilicity and super-lipophobicity in air, and aims to provide a nano-fiber membrane with the characteristics of super-hydrophilicity and super-lipophobicity in air.
The above purpose is realized by the following technical scheme:
the preparation method of the nano-fiber membrane with super-hydrophilicity and super-lipophobicity in the air comprises the following steps:
s1, adding polyvinyl butyral into a solvent to prepare an electrostatic spinning solution;
s2, placing the electrostatic spinning solution in an injector, and performing electrostatic spinning in a single-needle spinning mode or a double-needle parallel spinning mode, wherein a receiver adopts a barrel aluminum foil receiver to obtain a fiber membrane;
wherein the electrostatic spinning voltage is 21kV, the distance between the medical syringe needle and the barrel is 15cm, the flow rate of the electrostatic spinning solution is controlled to be 1ml/h, and the rotating speed of the barrel is 100 revolutions per minute;
s3, removing the fiber membrane from the cylindrical aluminum foil receiver, and removing residual solvent on the surface of the fiber membrane by a heating and drying mode, wherein the fiber membrane is taken and placed in an oven to be dried for 5-6 hours at 60 ℃, and the super-hydrophilic and super-oleophobic nanofiber membrane in the air is obtained.
In S1: the solvent is a mixed solution of a fluorine-containing anionic surfactant, absolute ethyl alcohol and P25 TiO2 particles; or the solvent is a mixed solution of NaOH aqueous solution, perfluorooctanoic acid, absolute ethyl alcohol and P25 TiO2 particles.
Drawings
FIGS. 1 to 4 are flow charts of the preparation method of the invention for the super-hydrophilic and super-oleophobic nano-fiber membrane in air;
FIG. 5 is a schematic SEM view;
FIG. 6 is a schematic representation of the wettability behaviour of water and oil on a nanofiber membrane;
fig. 7 is a schematic view of contact angle images of water and oil in air on nanofiber membranes.
Detailed Description
The first embodiment is as follows: the preparation method of the air super-hydrophilic and super-oleophobic nanofiber membrane based on PVB and fluorine-containing anionic surfactant comprises the following steps:
step one, taking 10ml of fluorine-containing anionic surfactant, taking 50ml of absolute ethyl alcohol, placing the absolute ethyl alcohol in a beaker with the specification of 100ml, performing magnetic stirring hydrolysis for 10min at normal temperature, then adding 1g to 2g of P25 TiO2 into the solution, and performing magnetic stirring for 30min at normal temperature to obtain a solvent, wherein the type of the fluorine-containing anionic surfactant is FS-50.
And step two, weighing 3g of PVB powder, adding the PVB powder into the solution, wherein the mass ratio of the PVB to the absolute ethyl alcohol is 1: 13.2, continuously and violently stirring for about 1 hour at normal temperature until the PVB and the absolute ethyl alcohol are completely dissolved to obtain a homogeneous electrostatic spinning solution, wherein the content of P25 TiO2 in the electrostatic spinning solution is 1.9% -3.6% by mass percentage.
Step three, putting the electrostatic spinning solution obtained in the step two into a 5ml medical injector for electrostatic spinning, wherein the injector is provided with a stainless steel needle with the diameter of 0.5mm, and a single-needle spinning mode or a double-needle parallel spinning mode is adopted; the electrostatic spinning voltage is 21kV, the distance between a medical syringe needle and a drum aluminum foil on a drum aluminum foil receiver is 15cm, the flow rate of an electrostatic spinning solution is controlled to be 1ml/h, the drum aluminum foil receiver adopts a metal cylinder which rotates at a high speed and has the diameter of 10cm and the height of 23cm, the rotating speed is 100 revolutions per minute, absolute ethyl alcohol volatilizes in the spinning process, a nanofiber membrane is left on the surface of the aluminum foil at the terminal of a roller, and the fiber membrane is taken off and then heated to dry the residual solvent on the surface, so that the super-oleophobic and super-hydrophilic super-infiltrated nanofiber membrane in the air of a target object is obtained.
The super-oleophobic and super-hydrophilic super-wetting nanofiber membrane in the air has the super-hydrophilic and super-oleophobic characteristics in the air, the water contact angle WCA is equal to 0 degree, the oil contact angle OCA is larger than 150 degrees, the membrane is covered on the membrane by taking a stainless steel net as a support, and layered oil-water mixtures can be directly separated in a water-passing and oil-blocking mode.
Example two: the preparation method of the air super-hydrophilic and super-oleophobic nanofiber membrane based on PVB and sodium perfluorooctanoate (PFOA-Na) comprises the following steps:
step one, 50ml of absolute ethyl alcohol is placed in a beaker with the specification of 100ml, 10g of NaOH aqueous solution with the mass fraction of 3wt% and 3g of perfluorooctanoic acid (PFOA) are added into the absolute ethyl alcohol, the mass ratio of the NaOH to the perfluorooctanoic acid is 1 to 10, the mass ratio of the perfluorooctanoic acid to the absolute ethyl alcohol is 1 to 13.2, and the mixture is magnetically stirred for 10min at normal temperature for hydrolysis. Then, 1g to 2g of P25 TiO2 was added to this solution, and magnetically stirred at normal temperature for 30min to obtain a solvent.
Step two, weighing 3g of PVB powder, adding the PVB powder into a solvent, continuously and violently stirring the PVB powder and absolute ethyl alcohol for about 1 hour at normal temperature until the PVB powder and the absolute ethyl alcohol are completely dissolved to obtain a homogeneous electrostatic spinning solution, wherein the content of P25 TiO2 in the electrostatic spinning solution is 1.7-3.5% in percentage by mass.
And step three, putting the electrostatic spinning solution obtained in the step two into a 5ml medical injector for electrostatic spinning, wherein the specific process of electrostatic spinning is consistent with the step three in the embodiment one.
The super-oleophobic and super-hydrophilic super-infiltrated nanofiber membrane in the air also has the super-hydrophilic and super-oleophobic characteristics in the air, the water contact angle WCA is equal to 0 degree, the oil contact angle OCA is larger than 150 degrees, the membrane is covered on a stainless steel net serving as a support, and layered oil-water mixtures can be directly separated in a water-through and oil-blocking mode. The film formation form was compared with example one: the film formed by the scheme of the first embodiment is more fluffy and tough and is easy to pick; the embodiment of the second embodiment is thinner and compact.
Example three: a preparation method of a Polyacrylonitrile (PAN) and fluorine-containing anionic surfactant based super-hydrophilic and super-oleophobic nanofiber membrane in air comprises the following steps:
step one, fluoridizing TiO 2 Preparation of the particles: putting 50ml of absolute ethyl alcohol into a beaker, measuring 10ml of fluorine-containing anionic surfactant, adding the 10ml of fluorine-containing anionic surfactant into the absolute ethyl alcohol, magnetically stirring for 10min for hydrolysis, wherein the volume ratio of the absolute ethyl alcohol to the fluorine-containing anionic surfactant is 1:5, then adding 10g of P25 TiO2 particles into the solution under the condition of magnetic stirring, wherein the mass ratio of the P25 TiO2 particles to the fluorine-containing anionic surfactant is 1:5.15, continuously stirring for 1 hour at normal temperature to obtain a liquid I, then putting the liquid I into an evaporation dish, putting the evaporation dish into an oven, heating for about 1 hour at 90 ℃, taking out until the solvent is completely volatilized, and obtaining a dried solid TiO particle block, wherein the solid TiO block is obtained 2 -a fluorine-containing anionic surfactant, and drying the solid mass of particles to form a TiO mass 2 Grinding the fluorine-containing anionic surfactant in a grinding bowl to obtain fluorinated TiO 2 Granules or powder for later use;
step two, preparing an electrostatic spinning solution: weighing 2.2g of Polyacrylonitrile (PAN) powder and 1g of perfluorooctanoic acid (PFOA) and adding the mixture into 17.8g of N, N-Dimethylformamide (DMF) solvent, and magnetically stirring for about 1 hour until the mixture is completely dissolved to obtain a solution II, wherein the mass fraction of PAN in the DMF solution II is 11 wt%. Then taking the prepared fluorinated TiO 2 And adding 1-2 g of powder into the PAN electrostatic spinning solution gradually in small amount by times under magnetic stirring, and performing magnetic stirring for more than 2 hours at normal temperature to form an electrostatic spinning solution. At this time, the TiO in the electrostatic spinning solution is calculated by mass percentage 2 -the anionic fluorinated surfactant content is 4.8wt% to 9.1 wt%.
Step three, preparation of the super-wetting fiber membrane: placing the electrostatic spinning solution obtained in the step two into a 5ml medical injector for electrostatic spinning; the process of electrospinning was identical to that of step three of example one or two, and N, N-Dimethylformamide (DMF) volatilized during the spinning process, leaving a nanofiber film on the aluminum foil at the end of the drum. And (3) removing the nanofiber membrane, and heating and drying the residual solvent on the surface to obtain the super-hydrophilic and oleophobic nanofiber membrane in the air of the target object.
The nanofiber membrane has super-hydrophilic and oleophobic properties in air, the water contact angle is 0 degree, the oil contact angle is about 140 degrees, the membrane is covered on the membrane by taking a stainless steel net as a support, and a layered oil-water mixture can be directly separated in a 'water and oil resistance' mode.
The preparation method has the characteristics of simple operation, high separation rate, environmental friendliness and the like. Selects the PVB material with low cost and environmental protection, the PAN material with excellent chemical stability and film forming rate, and the modified material containing fluorine anion surfactant, sodium perfluorooctanoate and TiO 2 Particles are prepared into the super-hydrophilic and super-oleophobic nanofiber membrane in the air through three solutions of electrostatic spinning, and the super-hydrophilic and super-oleophobic nanofiber membrane is applied to oil-water separation.
The PVB material, PAN material and perfluorooctanoic acid are purchased from Shanghai Aladdin Biotechnology Inc., P25 TiO2 is purchased from Tianjin Baima technology Inc., and N, N-Dimethylformamide (DMF), absolute ethyl alcohol, sodium hydroxide NaOH, vegetable oil and dichloroethane are purchased from local Baida laboratory instruments and the market place. The SEM pictures shot by the method are obtained by a Scios2 scanning electron microscope provided by Sammerfoil.

Claims (3)

1. The preparation method of the nano-fiber membrane with super-hydrophilicity and super-lipophobicity in the air is characterized by comprising the following steps:
s1, adding polyvinyl butyral into a solvent to prepare an electrostatic spinning solution;
s2, carrying out electrostatic spinning on the electrostatic spinning solution to obtain a fiber membrane;
s3, removing residual solvent on the surface of the fiber membrane to obtain the super-oleophobic and super-hydrophilic super-infiltrated nano-fiber membrane in the air;
in the step S2, the electrostatic spinning solution is placed in an injector for electrostatic spinning, and a receiver adopts a barrel aluminum foil receiver;
adopting a single-needle spinning mode or a double-needle parallel spinning mode, wherein the electrostatic spinning voltage is 21kV, the distance between the needle of the medical injector and the barrel is 15cm, the flow rate of the electrostatic spinning solution is controlled to be 1ml/h, and the rotating speed of the barrel is 100 revolutions per minute;
in the step S3, removing residual solvent on the surface of the fiber membrane by a heating and drying mode;
in the step S3, the fiber membrane is firstly peeled off from the barrel aluminum foil receiver and then the residual solvent on the surface is heated and dried;
in S3, the heating and drying step: placing the fiber membrane in an oven to be dried for 5-6 hours at 60 ℃ to obtain a super-hydrophilic and super-oleophobic nanofiber membrane in the air;
the solvent is a mixed solution of a fluorine-containing anionic surfactant, absolute ethyl alcohol and P25 TiO2 particles, or the solvent is a mixed solution of NaOH aqueous solution, perfluorooctanoic acid, absolute ethyl alcohol and P25 TiO2 particles.
2. The preparation method according to claim 1, wherein the solvent is a mixed solution of a fluorine-containing anionic surfactant, absolute ethyl alcohol and P25 TiO2 particles: adding fluorine-containing anionic surfactant into anhydrous ethanol, stirring and hydrolyzing for 10min at a volume ratio of 1:5, adding P25 TiO2 particles under magnetic stirring, and continuously stirring at room temperature for 30 min.
3. The method according to claim 1, wherein the solvent is a mixed solution of NaOH aqueous solution, perfluorooctanoic acid, absolute ethanol and P25 TiO2 particles, and the method comprises the following steps: dissolving 3wt% of NaOH aqueous solution and perfluorooctanoic acid in absolute ethyl alcohol, wherein the mass ratio of NaOH to perfluorooctanoic acid is 1 to 10, the mass ratio of perfluorooctanoic acid to absolute ethyl alcohol is 1 to 13.2, carrying out magnetic stirring hydrolysis for 10min, adding P25 TiO2 particles under the condition of magnetic stirring, and continuously stirring for 30min at normal temperature.
CN202210958131.5A 2022-08-11 2022-08-11 Preparation method of super-hydrophilic and super-oleophobic nanofiber membrane in air Pending CN115025645A (en)

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CN113896282A (en) * 2021-11-10 2022-01-07 哈尔滨工业大学 Underwater oil stain removing equipment based on super-oleophobic and super-hydrophilic net film
CN114210208A (en) * 2021-12-15 2022-03-22 哈尔滨工业大学 Preparation method of ultraviolet light driven nanofiber membrane capable of converting wettability
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Publication number Priority date Publication date Assignee Title
US20120000853A1 (en) * 2010-06-14 2012-01-05 The United States Air Force Superhydrophilic and oleophobic porous materials and methods for making and using the same
US20140065906A1 (en) * 2012-09-05 2014-03-06 Samsung Electro-Mechanics Co., Ltd. Super hydrophobic membrane and method of manufacturing the same
CN103601826A (en) * 2013-10-17 2014-02-26 华南理工大学 Hydrophilic oleophobic polymer and preparation method thereof, and application thereof in humidity response oil and water separating membrane
KR20160055505A (en) * 2014-11-10 2016-05-18 주식회사 아모그린텍 Membrane having hydrophilicity and oleophobicity, and method of manufacturing the same
CN107638817A (en) * 2017-10-13 2018-01-30 中国科学院生态环境研究中心 A kind of hydrophilic and oleophobic films of compound PTFE/PAN and preparation method thereof
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CN109825179A (en) * 2019-02-01 2019-05-31 东南大学 A kind of aqueous superhydrophilic superoleophobic coating and its preparation method and application
US20210379539A1 (en) * 2020-06-09 2021-12-09 Board Of Trustees Of The University Of Arkansas Bilayer electrospun membranes for treating fracking wastewater via membrane distillation
CN112717710A (en) * 2020-12-11 2021-04-30 武汉理工大学 Air super-oleophobic and super-hydrophilic film and preparation method and application thereof
CN113842676A (en) * 2021-10-20 2021-12-28 同济大学 Super-hydrophilic-super-oleophobic particle for oily sewage treatment and preparation method and application thereof
CN113896282A (en) * 2021-11-10 2022-01-07 哈尔滨工业大学 Underwater oil stain removing equipment based on super-oleophobic and super-hydrophilic net film
CN114210208A (en) * 2021-12-15 2022-03-22 哈尔滨工业大学 Preparation method of ultraviolet light driven nanofiber membrane capable of converting wettability
CN114522550A (en) * 2022-02-22 2022-05-24 华南理工大学 Super-hydrophilic/underwater super-oleophobic nanofiber membrane as well as preparation method and application thereof

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Application publication date: 20220909