CN113957703B - Beaded nanofiber material and preparation method thereof - Google Patents

Beaded nanofiber material and preparation method thereof Download PDF

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CN113957703B
CN113957703B CN202111213693.9A CN202111213693A CN113957703B CN 113957703 B CN113957703 B CN 113957703B CN 202111213693 A CN202111213693 A CN 202111213693A CN 113957703 B CN113957703 B CN 113957703B
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solvent
beaded
nanofiber
polymer solution
polymer
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CN113957703A (en
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唐宁
邵静宜
陈鱼
莫大宝
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Zhejiang Sci Tech University ZSTU
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/08—Organic compounds
    • D06M10/10—Macromolecular compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/22—Polymers or copolymers of halogenated mono-olefins
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
    • D06M2101/28—Acrylonitrile; Methacrylonitrile
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34—Polyamides

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Nonwoven Fabrics (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Artificial Filaments (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The application relates to a beaded nanofiber material and a preparation method thereof, wherein a non-solvent is added into a polymer solution to obtain a microgel polymer solution, an electrostatic spinning fiber membrane is immersed into the microgel polymer solution, the polymer solution is taken out and then is placed into an ultrasonic-assisted non-solvent coagulation bath, and the ultrasonic waves are utilized to increase the Rayleigh instability in the polymer immersion liquid phase separation process, so that the beaded nanofiber membrane is prepared. The average particle diameter of beads in the prepared beaded nanofiber material is 20-1000 nm, the average pore diameter of the material is 200-1000 nm, and the porosity is 80-95%. The method is simple and easy to implement, and the prepared beaded nanofiber has the advantages of multistage coarse structure, large specific surface area, small pore diameter, high porosity and the like, and can obviously improve the filtering separation precision and efficiency of materials.

Description

Beaded nanofiber material and preparation method thereof
Technical Field
The application belongs to the technical field of fiber materials, and relates to a beaded nanofiber material and a preparation method thereof.
Background
The beaded nanofiber material has the advantages of small fiber diameter, multi-level coarse structure, large specific surface area and the like, and has wide application prospect in the fields of adsorption separation, bioengineering and the like. The literature [ the drug release property of electrospun polylactic acid beaded fiber [ J ]. International textile guide ] and the literature [ Superhydrophobic and superoleophillic surface of porous beaded electrospun polystrene and polysytrene-zeolite fiber for crude oil-water separation [ J ]. Physics and Chemistry of the Earth, parts A/B/C,2016,92:7-13 ] respectively disclose a technology for preparing beaded nanofiber materials by using an electrospinning technology. However, the bead particle size of the beaded nanofiber material prepared by the electrostatic spinning method is in the micron level, and the bead with the nanometer level particle size is difficult to obtain, so that the beaded nanofiber material has little effect on increasing the roughness of the material and improving the specific surface area of the material. Patent "preparation method of beaded nanofiber" (CN 103643337B) discloses a technology for preparing beaded nanofiber by electrospinning using an inorganic nanoparticle preparation solution grafted with a polymer, through which a particle size range of less than 1000nm can be obtained, but the technology is complex and the interface bonding of an organic phase and an inorganic phase is not controllable. Therefore, there is an urgent need to develop a new method for simply preparing a nanofiber material of a nanoscale beaded structure.
Disclosure of Invention
The application aims to solve the problems in the prior art and provides a beaded nanofiber material and a preparation method thereof.
In order to achieve the above purpose, the application adopts the following technical scheme: a process for preparing the nano-fibrous material in bead shape includes such steps as preparing the mixture of microgel with polymer, solvent and non-solvent, immersing the chosen electrospun fibrous substrate in the mixture, and ultrasonic-assisted non-solvent induced phase separation. The beaded nanofiber prepared by the application takes electrospun fiber as a base material, and a beaded structure is constructed on the surface of the electrospun fiber by an ultrasonic-assisted non-solvent induced phase separation method.
The reason why the application uses the electrostatic spinning fiber film as the base material is that: (1) The electrostatic spinning fiber diameter is in nanometer level (less than 1000 nm) which is favorable for the microgel polymer solution with low viscosity to form a nanometer-level beaded structure on the surface, if the material with the fiber diameter of micron level or even tens of microns such as melt-blown or spun-bonded non-woven cloth is used as a base material, the beaded structure can not be formed due to the mismatch between the size of the material and the microsphere size formed on the surface of the microgel polymer solution. (2) The high porosity and the communicating pore canal structure of the electrostatic spinning fiber membrane are beneficial to the mutual diffusion of the solvent and the non-solvent in the ultrasonic auxiliary phase separation process.
The reason for using the polymer solution of the microgel is that the polymer solution of the microgel contains a large number of nucleated polymer microcrystals, which is helpful for forming a bead structure in the phase separation process.
The application adopts ultrasonic-assisted non-solvent induced phase separation technology because the energy of ultrasonic waves can increase the Rayleigh instability in the process of polymer impregnation liquid phase separation, thereby promoting the polymer impregnation liquid of microgel to form a bead structure on the surface of electrospun fiber in the process of phase separation.
The polymer is selected from polyacrylonitrile, polyvinylidene fluoride, polysulfone, polyethersulfone, polyamide, polyurethane and polyetherimide, the electrospun fiber substrate is an electrospun nanofiber membrane, and the preparation of the electrospun nanofiber membrane is a known technology.
The average particle size of the beads in the beaded nanofiber material is 20-1000 nm.
As a preferable technical scheme:
a method for preparing a beaded nanofiber material as described above, the polymer having a weight average molecular weight of 1X 10 4 ～100×10 4 The concentration of the polymer in the microgel polymer solution is 1-5 wt percent, and the viscosity of the microgel polymer solution is 200-2000 mPa.s.
The solvent of the polymer solution is one or more of N, N-dimethylformamide, dimethyl sulfoxide, N-dimethylformamide, N-methylpyrrolidone and formic acid.
According to the preparation method of the beaded nanofiber material, the non-solvent used in the microgel polymer solution is one or more of water, methanol, ethanol, propanol, butanol, isopropanol and acetone, and the amount of the non-solvent is 0.001-0.5 wt%.
The preparation method of the beaded nanofiber material comprises the steps of preparing an electrospun fiber substrate from polyamide electrospun nanofiber membranes, polytetrafluoroethylene electrospun nanofiber membranes, polyethylene terephthalate electrospun nanofiber membranes, polyvinylidene fluoride electrospun nanofiber membranes and polyacrylonitrile electrospun nanofiber membranes. Electrospun fibrous substrates require insolubility in the solvents used in the mixed solution.
The preparation process of the beaded nanometer fiber material with non-solvent soaking amount of 5-30 ul cm -2 。
According to the preparation method of the beaded nanofiber material, the ultrasonic frequency is 20-50 kHz, the ultrasonic power is 50-200W in ultrasonic-assisted non-solvent induced phase separation, the non-solvent is one or more of water, methanol, ethanol, propanol, butanol, isopropanol and acetone or a mixture of the non-solvent and a solvent used by a polymer solution, and the solvent consumption accounts for 0-30wt% of the specific gravity of the coagulating bath.
The application also provides a nanofiber material prepared by the method according to any one of the above, the structure is a bead nanofiber structure, the average pore diameter of the material is 200-1000 nm, and the porosity is 80-95%.
The principle of the application is as follows:
according to the application, a certain proportion of non-solvent is added into the polymer solution, the non-solvent is utilized to enable the homogeneous polymer solution to generate polymer nucleation growth to form a microgel mixed solution containing a large number of polymer microcrystals, and an ultrasonic technology is assisted in a non-solvent induced phase separation process, so that the Rayleigh instability in the microgel solution phase separation process is further increased, and the formation of a bead structure is promoted.
The beneficial effects are that:
(1) Unlike available polymer solution electrostatic spinning process, the present application has bead with average size of 20-1000 nm, and can reduce the pore size of fiber film, raise the surface roughness of the material and raise the specific surface area of the material.
(2) Unlike the beaded nanofiber prepared by electrostatic spinning of inorganic nanoparticles grafted with polymer, the beaded nanofiber material prepared by the application has simple preparation process and good interface compatibility.
Drawings
FIG. 1 is an SEM photograph of a beaded nanofiber material prepared according to example 1.
Detailed Description
The application is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
Example 1
A process for preparing the nano-fibre material in the form of bead includes such steps as choosing the molecular weight of weight-average material 5X 10 4 The polymer solution was prepared from the polymer (polyacrylonitrile) and the solvent (dimethyl sulfoxide), and 0.001wt% of a non-solvent (methanol) was added to the solution to obtain a microgel mixed solution having a concentration of 1wt% and a viscosity of 200 mpa.s. Next, the selected polyamide electrospun nanofiber substrate was placed at an impregnation level of 5ul cm -2 Is immersed in a non-solvent (methanol) coagulation bath with a frequency of 20kHz and a power of 50W, and then is subjected to phase separation to prepare a beaded nanofiber membrane, as shown in FIG. 1.
The average particle diameter of beads in the finally prepared beaded nanofiber material is 50nm, the average pore diameter of the material is 200nm, and the porosity is 80%.
Example 2
A process for preparing the nano-fibre material in the form of bead includes such steps as choosing the molecular weight of 57X 10 4 The polymer solution was prepared from the polymer (polyvinylidene fluoride) and the solvent (N, N-dimethylformamide) in g/mol, and 0.01wt% of a non-solvent (water) was added to the solution to obtain a microgel mixed solution having a concentration of 2wt% and a viscosity of 800 mPa.s. Next, the selected polytetrafluoroethylene electrospun nanofiber substrate was placed at an impregnation level of 10ul cm -2 Is immersed in a coagulation bath of ultrasonic-assisted non-solvent (a mixture of water and N, N-dimethylformamide) with a frequency of 20kHz and a power of 100W, and is subjected to phase separation, wherein the amount of N, N-dimethylformamide accounts for 2wt% of the specific gravity of the coagulation bath, to prepare the beaded nanofiber membrane.
The average particle diameter of beads in the finally prepared beaded nanofiber material is 50nm, the hydrophobic angle of the filter membrane is 150 degrees, the rolling angle is 3 degrees, the average pore diameter of the filter membrane material is 300nm, and the porosity is 85%.
Example 3
A process for preparing the nano-fibre material in the form of bead includes such steps as choosing the molecular weight of 20X 10 4 Preparing a polymer solution from g/mol polymer (polysulfone) and solvent (N, N-dimethylformamide), and adding 0.15wt% of non-solvent (ethanol) to the solution to obtain a concentration of 3wtAnd a microgel mixed solution with a viscosity of 800 mPa.s. Next, the selected polyethylene terephthalate electrospun nanofiber substrate was placed in an impregnation amount of 15ul cm -2 Is immersed in a non-solvent (ethanol) coagulation bath with a frequency of 30kHz and a power of 120W, and then is subjected to phase separation to prepare the beaded nanofiber membrane.
The average particle diameter of beads in the finally prepared beaded nanofiber material is 1000nm, the average pore diameter of the material is 600nm, and the porosity is 90%.
Example 4
A process for preparing the nano-fibre material in the form of bead includes such steps as choosing the molecular weight of 30X 10 4 The polymer solution was prepared from the polymer (polyethersulfone) and the solvent (N-methylpyrrolidone), and 0.2wt% of a non-solvent (water) was added to the solution to obtain a microgel mixed solution having a concentration of 2wt% and a viscosity of 1000 mPa.s. The selected polyamide electrospun fibrous substrate was then brought to an impregnation level of 25ul cm -2 After being taken out, the mixture was placed in a coagulation bath (a mixture of water and propanol) with a frequency of 30kHz and a power of 200W, in which the propanol was used in an amount of 20wt% based on the specific gravity of the coagulation bath, to perform phase separation, to prepare a beaded nanofiber membrane.
The average particle size of beads in the finally prepared beaded nanofiber material is 300nm, the average pore size of the material is 300nm, and the porosity is 93%.
Example 5
A process for preparing the nano-fibre material in the form of bead includes such steps as choosing the molecular weight of 100X 10 4 The polymer solution was prepared from g/mol of the polymer (polyetherimide) and a solvent (N, N-dimethylformamide, dimethyl sulfoxide), wherein the ratio of N, N-dimethylformamide to dimethyl sulfoxide was 3/7, and 0.005wt% of a non-solvent (water) was added to the solution to obtain a microgel mixed solution having a concentration of 1wt% and a viscosity of 2000mPa.s. Next, the selected polyamide electrospun nanofiber substrate was placed at an impregnation level of 20ul cm -2 Immersing in the mixed solution of (B) and then placing it in ultrasonic wave with frequency of 50kHz and power of 150WPhase separation is carried out in a non-solvent (water) coagulation bath to prepare the beaded nanofiber membrane.
The average particle diameter of beads in the finally prepared beaded nanofiber material is 500nm, the average pore diameter of the material is 350nm, and the porosity is 85%.
Example 6
A process for preparing the nano-fibre material in the form of bead includes such steps as choosing the molecular weight of 20X 10 4 The polymer solution was prepared from g/mol of the polymer (polyurethane) and a solvent (N, N-dimethylacetamide and N-methylpyrrolidone) in a ratio of 5/5, and 0.3% by weight of a non-solvent (water) was added to the solution to obtain a microgel mixed solution having a concentration of 2% by weight and a viscosity of 1200 mpa.s. Next, the selected polytetrafluoroethylene electrospun nanofiber substrate was placed at an impregnation level of 15ul cm -2 Is immersed in a non-solvent (water) coagulation bath with a frequency of 40kHz and a power of 125W, and then is subjected to phase separation to prepare the beaded nanofiber membrane.
The average particle diameter of beads in the finally prepared beaded nanofiber material is 700nm, the average pore diameter of the material is 600nm, and the porosity is 89%.
Example 7
A process for preparing the nano-fibre material in the form of bead includes such steps as choosing the molecular weight of 9X 10 4 The polymer solution was prepared from the polymer (polyacrylonitrile) and the solvent (dimethyl sulfoxide), and 0.003wt% of a non-solvent (methanol) was added to the solution to obtain a microgel mixed solution having a concentration of 1.5wt% and a viscosity of 800 mpa.s. Next, the selected polyethylene terephthalate electrospun nanofiber membrane substrate was placed at an impregnation level of 30ul cm -2 Is immersed in a non-solvent (water) coagulation bath with a frequency of 50kHz and a power of 100W, and then is subjected to phase separation to prepare the beaded nanofiber membrane.
The average particle diameter of beads in the finally prepared beaded nanofiber material is 600nm, the average pore diameter of the material is 1000nm, and the porosity is 95%.
Example 8
A process for preparing the nano-fibre material in the form of bead includes such steps as choosing the molecular weight of 1.8×10 4 The polymer solution was prepared from the polymer (polyamide) and the solvent (formic acid), and 0.002wt% of a non-solvent (water) was added to the solution to obtain a microgel mixed solution having a concentration of 1.5wt% and a viscosity of 300 mpa.s. Next, the selected polyvinylidene fluoride electrospun nanofiber substrate was placed at an impregnation level of 30ul cm -2 Is immersed in a non-solvent (water) coagulation bath with a frequency of 50kHz and a power of 100W, and then is subjected to phase separation to prepare the beaded nanofiber membrane.
The average particle diameter of beads in the finally prepared beaded nanofiber material is 400nm, the average pore diameter of the material is 500nm, and the porosity is 90%.
Example 9
A process for preparing the nano-fibre material in the form of bead includes such steps as choosing the molecular weight of weight-average material (1X 10) 4 The polymer solution was prepared from the polymer (polyamide) and the solvent (formic acid), and 0.003wt% of a non-solvent (methanol) was added to the solution to obtain a microgel mixed solution having a concentration of 3wt% and a viscosity of 700 mpa.s. Next, the selected polyacrylonitrile electrospun fibrous substrate was placed at an impregnation level of 25ul cm -2 Is immersed in a non-solvent (water) coagulation bath with a frequency of 30kHz and a power of 200W, and then is subjected to phase separation to prepare the beaded nanofiber membrane.
The average particle diameter of beads in the finally prepared beaded nanofiber material is 500nm, the average pore diameter of the material is 600nm, and the porosity is 92%.
Example 10
A process for preparing the nano-fibre material in the form of bead includes such steps as choosing the molecular weight of 68X 10 4 The polymer solution was prepared from the polymer (polyvinylidene fluoride) and the solvent (N, N-dimethylformamide) in g/mol, and 0.1wt% of a non-solvent (water) was added to the solution to obtain a microgel mixed solution having a concentration of 2wt% and a viscosity of 1500 mpa.s. The selected polyamide electrospun nanofiber substrate was then placed at an impregnation level of 30ul cm -2 In a mixed solution of (2)Dipping, taking out, and then placing the mixture into an ultrasonic-assisted nonsolvent (water) coagulation bath with the frequency of 50kHz and the power of 200W for phase separation to prepare the beaded nanofiber membrane.
The average particle diameter of beads in the finally prepared beaded nanofiber material is 400nm, the average pore diameter of the material is 200nm, and the porosity is 93%.

Claims (8)

1. A preparation method of a beaded nanofiber material is characterized by comprising the following steps: firstly, selecting a polymer and a solvent, adding a non-solvent to obtain a microgel polymer solution, then, immersing an electrospun fiber membrane in the microgel polymer solution, taking out, and then, placing the microgel membrane in an ultrasonic-assisted non-solvent coagulation bath, and increasing the Rayleigh instability of the polymer in the process of polymer immersion liquid phase separation by utilizing ultrasonic waves, thereby preparing a beaded nanofiber membrane;
the polymer is selected from polyacrylonitrile, polyvinylidene fluoride, polysulfone, polyethersulfone, polyamide and polyetherimide; the electrostatic spinning fiber substrate is an electrostatic spinning nanofiber membrane;
the solvent of the polymer solution is selected fromN, NDimethylformamide, dimethyl sulfoxide,N-one or more of methyl pyrrolidone and formic acid;
the non-solvent used in the microgel polymer solution is more than one of water, methanol, ethanol, propanol, butanol, isopropanol and acetone;
the non-solvent used for ultrasonic assistance is one or more of water, methanol, ethanol, propanol, butanol, isopropanol and acetone or a mixture of one or more of water, methanol, ethanol, propanol, butanol, isopropanol and acetone and the solvent used for the polymer solution.
2. The method for preparing a beaded nanofiber material according to claim 1, wherein the average particle size of beads in the beaded nanofiber is 20-1000 nm.
3. A process for preparing a beaded nanofiber material as defined in claim 1, which is characterized byCharacterized in that the weight average molecular weight of the polymer is 1X 10 4 ~100×10 4 The concentration of the polymer in the microgel polymer solution is 1-5 wt%, and the viscosity of the microgel polymer solution is 200-2000 mPa.s.
4. The method of claim 1, wherein the non-solvent is 0.001-0.5 wt% of the microgel polymer solution.
5. The method of preparing a beaded nanofiber material according to claim 4, wherein the electrospun fibrous substrate is selected from the group consisting of polyamide electrospun nanofiber membranes, polytetrafluoroethylene electrospun nanofiber membranes, polyethylene terephthalate electrospun nanofiber membranes, polyvinylidene fluoride electrospun nanofiber membranes, and polyacrylonitrile electrospun nanofiber membranes.
6. The method for preparing a beaded nanofiber material according to claim 5, wherein the amount of the microgel polymer solution impregnated into the electrospun fiber substrate is 5 to 30ul cm -2 。
7. The method for preparing a beaded nanofiber material according to claim 1, wherein the ultrasonic frequency used for ultrasonic-assisted non-solvent-induced phase separation is 20-50 kHz, the ultrasonic power is 50-200W, and the solvent consumption accounts for 0-30wt% of the coagulation bath.
8. A beaded nanofiber material prepared by the method according to any one of claims 1-7, characterized in that: the average pore diameter of the material is 200-1000 nm, and the porosity is 80-95%.
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