CN107723815A - A kind of oriented nanofibers and preparation method thereof - Google Patents

A kind of oriented nanofibers and preparation method thereof Download PDF

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Publication number
CN107723815A
CN107723815A CN201710946203.3A CN201710946203A CN107723815A CN 107723815 A CN107723815 A CN 107723815A CN 201710946203 A CN201710946203 A CN 201710946203A CN 107723815 A CN107723815 A CN 107723815A
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CN
China
Prior art keywords
oriented nanofibers
preparation
spinning solution
spinning
solution
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Pending
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CN201710946203.3A
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Chinese (zh)
Inventor
谭睿哲
邹鹏
杨习锋
曾晨光
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Guangzhou Sun Shing Biotech Co ltd
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Guangzhou Sun Shing Biotech Co ltd
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Priority to CN201710946203.3A priority Critical patent/CN107723815A/en
Publication of CN107723815A publication Critical patent/CN107723815A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/12Stretch-spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like

Abstract

The invention discloses a kind of oriented nanofibers and preparation method thereof.The present invention combines by using rotor spinning and magnetic field force, controls the movement locus of spinning solution jet, realizes the production of oriented nanofibers.The present invention simple economy, avoids electrostatic pollution and potential danger caused by high-pressure electrostatic again without high-voltage electrostatic generator, spinning process is more safe and stable, multiple jetses can be produced simultaneously, greatly improve spinning fluency and production efficiency, suitable for industrialized production oriented nanofibers.

Description

A kind of oriented nanofibers and preparation method thereof
Technical field
The present invention relates to the preparation method of nanofiber, and in particular to a kind of oriented nanofibers and preparation method thereof.
Background technology
A diameter of 10nm~1000nm polymer fiber has many special properties, and this kind of polymer fibres layers have Very high filter efficiency, it can be used as the filtering of gas and liquid, retain the barrier material of submicron particles, bacterium and chemicals; As battery separator, composite reinforcement;It is used as pharmaceutical carrier and tissue implants carriers in field of medicaments;Nanowire The high-specific surface area of dimension determines that it has special adsorption property, such as the purposes of the carrier of catalyst.
Nanofiber by the polymer of wide scope, blend polymer and can be gathered by polymer solution processing technology The blend of compound and low molecule additive is made, and because solution viscosity is relatively low, can be obtained by solution process less straight The fiber in footpath.Coulomb force of the solution processing technology in the mechanical force using flowing gaseous medium or electrostatic field, can be divided into Rotor spinning and the class of electrostatic spinning two.
At present, the method and apparatus of rotor spinning have been widely used for the preparation of nanofiber.Polymer solution is noted Enter the spinning head to ring section, then, by means of the mechanism of the air-flow in the ring delivered inside make the solution into Type, producing has 200 nanometers to 3, the fiber of 000 nanometer diameter.
Electrostatic spinning is another common method for preparing nanofiber.Polymer solution is assigned to the milli of internal diameter 0.5 Rice is into 1.5 millimeters of cylindrical spinning-nozzle, and these nozzles are connected to direct voltage source, and effluent solvent is by means of quiet Electric power is attracted to electrode, and this is typically grounded to electrode, while filament is shaped to by means of this power, its Therefore it is split into the fiber of corresponding small diameter.Spinning is from a nozzle either a series of static or mobile nozzle Carry out, so as to improve the production capacity of device.
However, the method and production efficiency ratio of above-mentioned production nanofiber are relatively low, can only produce within a certain period of time seldom The polymeric material of the processing of amount.The diameter of nanofiber prepared by rotor spinning depends particularly on air quality and flows through spinneret The ratio of the polymer solution of head;Electrostatic spinning then must form so-called Taylor cone, process conditions in the throat of spinning head It is it is required that higher.The maximum adjustable intensity of electrostatic field is limited by air insulation intensity, and when being higher than the limit, electrode it Between discharge, potential safety hazard in production process be present.In view of the foregoing and accessible polymer solution spun concentration, The polymer of about 0.1 gram to 1 gram of processing was possible in a spinning head in one hour, while spinning process needs are higher Voltage, produce nanofiber during the problems such as yield is relatively low, and safety coefficient is not high be present.On the other hand, the above method The nanofiber being prepared mostly random alignment, in unordered shape.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of oriented nanofibers and preparation method thereof, Combined by rotor spinning and magnetic field force, control the movement locus of jet, improve nanofiber order;This method need not height Electrostatic generator is pressed, simple economy, spinning process is more safe and stable, and production efficiency is higher, is taken suitable for industrialized production To nanofiber.
To achieve the above object, the technical scheme that the present invention takes is as follows:
A kind of preparation method of oriented nanofibers, it is characterised in that comprise the following steps:
(1) spinning solution is prepared:Magnetic nanoparticle is scattered in macromolecule polymer solution, forms spinning solution;
(2) oriented nanofibers are prepared:Spinning solution made from step (1) is placed in externally-applied magnetic field, to spinning solution Gas is injected, disturbance spinning solution makes it produce jet, jet stretcher strain, is finally formed by curing oriented nanofibers.
Combined in above-mentioned technical proposal by rotor spinning and magnetic field force, control the movement locus of jet, improve Nanowire Tie up order;It is more safe and stable without high-voltage electrostatic generator, simple economy, spinning process, multiply can be produced simultaneously Jet, production efficiency is higher, suitable for industrialized production oriented nanofibers.
As the preferred embodiment of the preparation method of oriented nanofibers of the present invention, the magnetic nanoparticle For γ-Fe2O3、Fe3O4, cobalt, at least one of nickel magnetic nanoparticle.
As the preferred embodiment of the preparation method of oriented nanofibers of the present invention, the magnetic nanoparticle Mass fraction in spinning solution is 5%.
As the preferred embodiment of the preparation method of oriented nanofibers of the present invention, the flow velocity of the gas is 10~200m/s.
As the preferred embodiment of the preparation method of oriented nanofibers of the present invention, the high molecular polymer For PLA, polycaprolactone, poly (glycolide-lactide) or sodium alginate.
As the preferred embodiment of the preparation method of oriented nanofibers of the present invention, the high molecular polymer The concentration of high molecular polymer is 4~15w/v% in solution.
As the preferred embodiment of the preparation method of oriented nanofibers of the present invention, the high molecular polymer Solvent be dichloromethane, dimethyl sulfoxide (DMSO), trifluoroethanol, chloroform or trifluoroacetic acid.
The present invention also provides a kind of oriented nanofibers made from technical scheme in accordance with the above.
Compared with prior art, beneficial effects of the present invention are:
Combined in technical solution of the present invention by rotor spinning and magnetic field force, control the movement locus of jet, improve nanometer Fiber order;For the present invention without high-voltage electrostatic generator, simple economy, spinning process is more safe and stable, can produce simultaneously Raw multiple jetses, greatly improve spinning fluency and production efficiency, suitable for industrialized production oriented nanofibers.
Brief description of the drawings
Fig. 1 is oriented nanofibers scanning electron microscope (SEM) photograph prepared by embodiment 1.
Fig. 2 is oriented nanofibers orientation result prepared by embodiment 1.
Fig. 3 is oriented nanofibers scanning electron microscope (SEM) photograph prepared by embodiment 4.
Fig. 4 is oriented nanofibers orientation result prepared by embodiment 4.
Embodiment
For the object, technical solutions and advantages of the present invention are better described, below in conjunction with the drawings and specific embodiments pair The present invention further illustrates.It will be appreciated by those skilled in the art that specific embodiment described herein is only explaining this hair It is bright, it is not intended to limit the present invention.
Embodiment 1
A kind of embodiment of the preparation method of oriented nanofibers of the present invention, the system of oriented nanofibers described in the present embodiment Preparation Method is:
PLA is dissolved in dichloromethane, PLA concentration is 4w/v% in gained PLA solution;By Fe3O4Nanometer Grain is added in the PLA solution for preparing, using high-shear homogenizer by Fe3O4It is dispersed in PLA solution, is formed and spun Silk solution, Fe3O4Nano particle is 5% in the mass fraction of spinning solution;Spinning solution is placed in externally-applied magnetic field, and spun Gas is injected in silk solution, the flow velocity of gas is 10m/s, and disturbance spinning solution makes it produce bubble, in externally-applied magnetic field, bubble Rupture and produce jet, jet stretcher strain, the dichloromethane volatilization of residual, be formed by curing oriented nanofibers;Vacuum drying 48h obtains final oriented nanofibers.
Embodiment 2
A kind of embodiment of the preparation method of oriented nanofibers of the present invention, the system of oriented nanofibers described in the present embodiment Preparation Method is:
Polycaprolactone is dissolved in dimethyl sulfoxide (DMSO), polycaprolactone concentration is 8w/v% in gained polycaprolactone solution;By γ- Fe2O3Nano particle is added in the polycaprolactone solution for preparing, using high-shear homogenizer by γ-Fe2O3Nano particle uniformly divides Dissipate in polycaprolactone solution, form spinning solution, γ-Fe2O3Nano particle is 5% in the mass fraction of spinning solution;It will spin Silk solution is placed in externally-applied magnetic field, and gas is injected in spinning solution, and the flow velocity of gas is 50m/s, and disturbance spinning solution makes It produces bubble, in externally-applied magnetic field, bubbles burst and produces jet, jet stretcher strain, the dimethyl sulfoxide (DMSO) volatilization of residual, It is formed by curing oriented nanofibers;Vacuum drying 48h obtains final oriented nanofibers.
Embodiment 3
A kind of embodiment of the preparation method of oriented nanofibers of the present invention, the system of oriented nanofibers described in the present embodiment Preparation Method is:
Poly (glycolide-lactide) is dissolved in trifluoroethanol, poly (glycolide-lactide) concentration is 12w/v% in gained poly (glycolide-lactide) solution; Nano nickel particles are added in the poly (glycolide-lactide) solution prepared, uniformly divided nickel magnetic nanoparticle using high-shear homogenizer Dissipate in poly (glycolide-lactide) solution, form spinning solution, nickel magnetic nanoparticle is 5% in the mass fraction of spinning solution;Will Spinning solution is placed in externally-applied magnetic field, and gas is injected in spinning solution, and the flow velocity of gas is 100m/s, disturbs spinning solution It is set to produce bubble, in externally-applied magnetic field, bubbles burst and produce jet, jet stretcher strain, the trifluoroethanol volatilization of residual, It is formed by curing oriented nanofibers;Vacuum drying 48h obtains final oriented nanofibers.
Embodiment 4
A kind of embodiment of the preparation method of oriented nanofibers of the present invention, the system of oriented nanofibers described in the present embodiment Preparation Method is:
Sodium alginate is dissolved in chloroform, sodium alginate concentration is 4w/v% in gained sodium alginate soln;Cobalt magnetic is received Rice grain is added in the sodium alginate soln prepared in spinning solution, is being spun cobalt magnetic nanoparticle using high-shear homogenizer Silk solution is dispersed in sodium alginate soln, forms spinning solution, quality point of the cobalt magnetic nanoparticle in spinning solution Number is 5%;Spinning solution is placed in externally-applied magnetic field, and gas is injected in spinning solution, the flow velocity of gas is 150m/s, is disturbed Dynamic spinning solution makes it produce bubble, in externally-applied magnetic field, bubbles burst and produce jet, jet stretcher strain, the chlorine of residual Imitative volatilization, is formed by curing oriented nanofibers;Vacuum drying 48h obtains final oriented nanofibers.
Embodiment 5
A kind of embodiment of the preparation method of oriented nanofibers of the present invention, the system of oriented nanofibers described in the present embodiment Preparation Method is:
PLA is dissolved in trifluoroacetic acid, PLA concentration is 15w/v% in gained PLA solution;Cobalt nickel magnetic is received Rice grain is added in the PLA solution prepared, and cobalt nickel magnetic nanoparticle is dispersed in into poly- breast using high-shear homogenizer In acid solution, spinning solution is formed, cobalt nickel magnetic nanoparticle is 5% in the mass fraction of spinning solution;Spinning solution is put In externally-applied magnetic field, and gas is injected in spinning solution, the flow velocity of gas is 200m/s, and disturbance spinning solution makes it produce gas Bubble, in externally-applied magnetic field, bubbles burst and produce jet, jet stretcher strain, residual trifluoroacetic acid volatilization, be formed by curing and take To nanofiber;Vacuum drying 48h obtains final oriented nanofibers.
Oriented nanofibers prepared by embodiment 1 and embodiment 4 are scanned with electron microscopic observation and degree of orientation test.Figure 1 and Fig. 2 is respectively the scanning electron microscopic picture and degree of orientation result of the oriented nanofibers prepared by embodiment 1, and embodiment 1 is made Standby oriented nanofibers surface is smooth, arranges very well ordered, is arranged mainly along the axial direction of fiber.Fig. 3 and Fig. 4 is respectively real The scanning electron microscopic picture and degree of orientation result of the oriented nanofibers prepared by example 4 are applied, the nanofiber tool prepared by embodiment 4 There is certain orientation.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than the present invention is protected The limitation of scope is protected, although being explained in detail with reference to preferred embodiment to the present invention, one of ordinary skill in the art should Understand, technical scheme can be modified or equivalent substitution, without departing from the essence of technical solution of the present invention And scope.

Claims (8)

1. a kind of preparation method of oriented nanofibers, it is characterised in that comprise the following steps:
(1) spinning solution is prepared:Magnetic nanoparticle is scattered in macromolecule polymer solution, forms spinning solution;
(2) oriented nanofibers are prepared:Spinning solution made from step (1) is placed in externally-applied magnetic field, injected to spinning solution Gas, disturbance spinning solution make it produce jet, jet stretcher strain, are finally formed by curing oriented nanofibers.
2. the preparation method of oriented nanofibers according to claim 1, it is characterised in that the magnetic nanoparticle is γ-Fe2O3、Fe3O4, cobalt, at least one of nickel magnetic nanoparticle.
3. the preparation method of oriented nanofibers according to claim 1, it is characterised in that the magnetic nanoparticle exists Mass fraction in spinning solution is 5%.
4. the preparation method of oriented nanofibers according to claim 1, it is characterised in that the flow velocity of the gas is 10 ~200m/s.
5. the preparation method of oriented nanofibers according to claim 1, it is characterised in that the high molecular polymer is PLA, polycaprolactone, poly (glycolide-lactide) or sodium alginate.
6. the preparation method of oriented nanofibers according to claim 1, it is characterised in that the high molecular polymer is molten The concentration of high molecular polymer is 4~15w/v% in liquid.
7. the preparation method of oriented nanofibers according to claim 1, it is characterised in that the high molecular polymer Solvent is dichloromethane, dimethyl sulfoxide (DMSO), trifluoroethanol, chloroform or trifluoroacetic acid.
8. oriented nanofibers made from the preparation method of the oriented nanofibers according to any one of claim 1~7.
CN201710946203.3A 2017-10-11 2017-10-11 A kind of oriented nanofibers and preparation method thereof Pending CN107723815A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110656402A (en) * 2019-01-21 2020-01-07 深圳维度新材料有限公司 Preparation method and equipment of inorganic nano-fiber
CN112369661A (en) * 2020-01-16 2021-02-19 湖北中烟工业有限责任公司 Cooling filter rod and low-temperature cigarette with same
CN114959924A (en) * 2022-06-28 2022-08-30 衢州学院 High-intensity magnetic field system for orientation arrangement of nano chitin fibers

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102965744A (en) * 2012-12-17 2013-03-13 苏州大学 Composite bubble electrostatic spinning device
CN104862799A (en) * 2015-05-26 2015-08-26 青岛大学 Method for preparing graphene/polymer orderly micro-nanometer composite fiber through magnetic spinning
CN104878455A (en) * 2015-05-26 2015-09-02 青岛大学 Melt magnetism spinning device and micro-nanofiber preparing method by utilizing melt magnetism spinning device
CN105350088A (en) * 2015-11-13 2016-02-24 广东工业大学 Ultrasonic porous bubble electro-spinning equipment

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102965744A (en) * 2012-12-17 2013-03-13 苏州大学 Composite bubble electrostatic spinning device
CN104862799A (en) * 2015-05-26 2015-08-26 青岛大学 Method for preparing graphene/polymer orderly micro-nanometer composite fiber through magnetic spinning
CN104878455A (en) * 2015-05-26 2015-09-02 青岛大学 Melt magnetism spinning device and micro-nanofiber preparing method by utilizing melt magnetism spinning device
CN105350088A (en) * 2015-11-13 2016-02-24 广东工业大学 Ultrasonic porous bubble electro-spinning equipment

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110656402A (en) * 2019-01-21 2020-01-07 深圳维度新材料有限公司 Preparation method and equipment of inorganic nano-fiber
CN112369661A (en) * 2020-01-16 2021-02-19 湖北中烟工业有限责任公司 Cooling filter rod and low-temperature cigarette with same
CN114959924A (en) * 2022-06-28 2022-08-30 衢州学院 High-intensity magnetic field system for orientation arrangement of nano chitin fibers

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Application publication date: 20180223