CN100432307C - Directional magnetic electrical spinning Nano fibers, preparation method and equipment needed - Google Patents

Directional magnetic electrical spinning Nano fibers, preparation method and equipment needed Download PDF

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CN100432307C
CN100432307C CNB2006100895144A CN200610089514A CN100432307C CN 100432307 C CN100432307 C CN 100432307C CN B2006100895144 A CNB2006100895144 A CN B2006100895144A CN 200610089514 A CN200610089514 A CN 200610089514A CN 100432307 C CN100432307 C CN 100432307C
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fiber
fecl
spinning
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CN1873064A (en
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聂俊
杨冬芝
张静
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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Abstract

The present invention provides directional arrangement macromolecule fibers containing paramagnetic Fe3O4 under nanometer scales, a preparation method of the fibers and equipment for preparing the magnetic electric spinning fibers. The method of the present invention comprises the following steps: using Fe3O4 magnetic fluid and macromolecule solution as raw materials; adopting an in-situ composite method; under high voltage electrostatic action, electrically spinning by regulating solution concentration and technological parameters of electric spinning. Because magnetic fields are arranged in a receiving device and macromolecule nanometer fibers containing Fe3O4 are in directional arrangement along the magnetic field direction under the induction of the magnetic fields, the nanometer fibbers with the fiber diameter distribution of 100 to 600 nm are obtained, wherein the nanometer fibers are in directional arrangement along the magnetic field direction. The fibers have the advantages of regular arrangement, consistent directions and capability of generating corresponding performance to external magnetic fields.

Description

Directional magnetic electro spinning nano fiber and preparation method thereof and device therefor
Technical field
The invention belongs to magnetic high-molecular nanofiber and technology of preparing thereof, specifically relate to a kind of paramagnetism Fe that under nanoscale, contains 3O 4The macromolecular fibre of oriented alignment and technology of preparing thereof and device therefor.
Background technology
Along with the development of electrospinning silk technology, the nano particle that people begin to have specific function is doped in the nanofiber, wishes the nanofiber that acquisition has specific function.For example, the Pt nano particle is doped to the nano composite material that can obtain to have high catalytic activity in the nanofiber; The Ag nano particle is doped to the nanofiber that the preparation of polypropylene nitrile has semiconducting behavior.But the preparation method of the nanofiber of magnetic that up to the present, can oriented alignment still is not reported.The magnetic Nano fiber has broad application prospects in fields such as target administration, electronic devices and components, nonlinear optical material, sensor, electromagnetic shielding material and microwave absorptions.At present to prepare the relevant reported in literature of super-paramagnetism nano fiber as follows: M.Wang with electrical spinning method, H.Singh.T.A.Hatton, G.C.Rutledge.Field-responsive super paramagnetic composite nanofibers byelectrospinning.Polymer, 2004:5505-5510 and Song Ting Tan, Joachim H.Wendorff, et al.Biocompatible and Biodegradable polymer nanofibers displaying superparamagnetic properties.ChemPhysChem, 2005, the above-mentioned two pieces of literature research of 6:1461-1465 have the preparation and a characterizing method of super-paramagnetism nano fiber.Above-mentioned bibliographical information all be with magnetic Fe 3O 4Join in the polymer solution, utilize the nanofiber of common electrospinning silk technology preparation, fiber is to be deposited in together in a jumble on gathering-device.If on gathering-device, design magnetic field, the magnetic Nano fiber alignment is arranged, make material in application process, can better produce consistent the response to externally-applied magnetic field, improve practical application.
Summary of the invention
The objective of the invention is: a kind of paramagnetism Fe that contains under nanoscale is provided 3O 4The macromolecular fibre of oriented alignment and technology of preparing thereof provide to prepare the used equipment of this magnetic electrospinning fibre simultaneously.
Mechanism of the present invention is as follows: Fe 3O 4Nano particle is dispersed in the Polymer Solution, and Polymer Solution forms nanofiber under the effect of high-pressure electrostatic.Under the magnetic field effect in receiving system, Fe 3O 4Tend to arrange, thereby prepare the magnetic Nano fiber of oriented alignment along magnetic direction.
The present invention is with Fe 3O 4Magnetic fluid, Polymer Solution are raw material, adopt in-situ compositing, by regulator solution concentration, and the technological parameter of electrospinning silk, under the high-pressure electrostatic effect, carry out the electrospinning silk, owing to be provided with magnetic field, under the induction in magnetic field, make and contain Fe at the receiving system place 3O 4High polymer nanometer fiber along the magnetic direction oriented alignment, thereby obtain being the magnetic high-molecular nanofiber of oriented alignment.This fiber alignment rule, direction are consistent, can produce consistent correspondence to externally-applied magnetic field.
Preparation process of the present invention is as follows:
A. respectively with FeCl 2.4H 2O, FeCl 3.6H 2O is dissolved in the FeCl that the distilled water compound concentration is 0.1～2molL 2Solution and concentration are the FeCl of 0.1～2molL 3Solution; Install additional in the reactor of strong magnet, in band stirring and bottom FeCl 3Solution and FeCl 2Solution is according to mol ratio Fe 3+: Fe 2+=1～2: 1 mixed is evenly prepared mixed liquor, feeds nitrogen to remove the oxygen in the mixed solution; The control reacting liquid temperature to mixed solution and dripping ammoniacal liquor, is 6.5～7 until the pH of solution value at 50～90 ℃, behind reaction 15～30min, continues slow dropping ammonia in solution, is 9～10 until the pH value, continues to stop reaction behind the reaction 30min; Take out supernatant liquid,, be neutral,, obtain Fe the product freeze drying until washing lotion with distilled water cyclic washing product 3O 4Nano particle;
At FeCl 3.6H 2O and FeCl 2.4H 2In the solution mixed process of O, Fe 3+With Fe 2+Preferred molar ratio be 1.5～1.75: 1.
B. with the Fe of drying 3O 4Nanoparticulate dispersed is prepared mass percent in the aqueous solution be 5～30% Fe 3O 4Suspension adds the quality percentage composition and is 0.1～1% surfactant again in solution, adopt ultrasonic dispersing;
Surfactant is a kind of in dodecyl sodium sulfate, lauryl sodium sulfate, Tween 80 (polysorbate), ammonium oleate, the alkyl quaternary ammonium salts.
C. get above-mentioned Fe 3O 4Suspension joins in the electrospinning silk Polymer Solution and disposes spinning solution, Fe 3O 4With high molecular mass ratio be 5～40: 100, and carry out the supersonic oscillations of 1～12h; But the macromolecular material that is used for the electrospinning silk can be a kind of of all spinning macromolecular materials such as polyvinyl alcohol, Merlon, poly butyric ester, shitosan, gelatin, polyoxyethylene.
D. above-mentioned spinning solution is added storage tank, under pump pressure or gravity effect, spinning solution is sprayed from shower nozzle, because the repulsive interaction of Polymer Solution surface charge, drop stretches and is the taylor cone shape, under effect of electric field, be drawn into fiber, repeatedly splitting took place in fiber before reaching dash receiver, on the dash receiver in band magnetic field, collect distribution of fiber diameters and be 100～600nm and along the nanofiber of magnetic direction oriented alignment.
Electric spinning device of the present invention comprises:
A high direct voltage electrostatic generator, a storage tank, connect a syringe pump on the storage tank, the storage tank bottom connects one group of metal shower nozzle, shower nozzle links to each other with HV generator is anodal, a metal dash receiver that links to each other with negative pole (or ground connection) is provided with two N utmost points that face and S utmost point magnet on the dash receiver; Electrostatic generator voltage is 10～60KV, and two magnet distance is 10～30cm, and the magnet surface magnetic intensity is 200～2000 Gausses, metal dash receiver conventional aluminium foil plate, and it is 10～30cm apart from shower nozzle.Metal shower nozzle internal diameter is 0.4～1.4mm.Also can produce magnetic field by place conductive coil on the metal dash receiver, distance is 5～10cm between conductive coil, and the magnetic field intensity that coil produces is 200～2000 Gausses.
The technological process of electrospinning silk is: the macromolecule spinning solution for preparing is added storage tank 2, under the pump pressure of syringe pump 5 or gravity effect, make spinning solution from shower nozzle 3 ejections, because surface tension, just the drop of ejection is spheroidal, because the repulsive interaction of Polymer Solution surface charge, drop stretches and is the taylor cone shape, and further under the electric field action that high direct voltage electrostatic generator 1 produces, be drawn into fiber, repeatedly splitting took place in fiber before reaching dash receiver, on the dash receiver 4 in band magnetic field, collect diameter at micron and nanometer tunica fibrosa along the magnetic direction oriented alignment.
Fe with preparation 3O 4Particle and fiber carry out signs such as SEM, TEM, the results are shown in Figure 2-4.As seen from Figure 2, Fe 3O 4Particle is evenly distributed in the polyvinyl alcohol nano.
Can be found out when the machine direction that receives during no magnetic field in the received field by Fig. 3, Fig. 4 to be random, when in the received field magnetic field being set, the nanofiber that receives is along the magnetic direction oriented alignment.
The present invention is successfully with Fe 3O 4Nano particle is dispersed in the high polymer nanometer fiber, and utilizes externally-applied magnetic field that fiber alignment is arranged, and it is simple to have preparation technology, and easy operating and advantage such as repeat is easy to be extended and applied.
Description of drawings:
Fig. 1 is electric spinning device figure, and 1 is the dash receiver in high direct voltage static power supply 2 storage tanks 3 shower nozzles 4 band magnetic fields, and 5 is syringe pump.
Fig. 2 for the present invention preparation contain Fe 3O 4The polyvinyl alcohol nano of nano particle.
Fig. 3 contains Fe in the polyvinyl alcohol nano 3O 4The transmission electron microscope photo of nano particle.
Fig. 4 is the magnetic response curve of polyvinyl alcohol nano film.
The specific embodiment:
Embodiment 1:
A. in the 100mL volumetric flask, with distilled water respectively compound concentration be the FeCl of 0.1molL 2With FeCl 3Solution; In being added with churned mechanically round-bottomed flask, with 35mL 0.1molL FeCl 3Solution and 20mL 0.1molL FeCl 2Solution mixes, and liquid level feeds nitrogen down, to remove the oxygen in anhydrating.Reaction unit is warmed up to 80 ℃, begins slow dropping ammonia in solution, is 6.5 until the pH of solution value, behind the reaction 15min, continues slow dropping ammonia in solution, is 9.5 until the pH value, and continuation stops reaction after reacting 30min; Hold drag with strong magnet, the supernatant liquid that inclines with distilled water cyclic washing product, is neutral until washing lotion; With product Fe 3O 4Freeze drying;
B. with the Fe of drying 3O 4Nanoparticulate dispersed adds 0.1% surfactant dodecyl sodium sulfate in the solution in the aqueous solution, adopt ultrasonic dispersing;
C. get above-mentioned Fe 3O 4It is in 10% the polyvinyl alcohol water solution that suspension joins concentration, and Fe 3O 4Addition and polyvinyl alcohol mass ratio be 30%, and carry out the supersonic oscillations of 1h;
D. in electric field, above-mentioned solution is joined in the syringe 2, shower nozzle 3 is the 10# syringe needle, and syringe needle links to each other 1 with the positive level of HV generator, and as negative electrode dash receiver 4, the aluminium foil plate is 10cm apart from syringe needle with the aluminium foil plate; Place two N utmost points that face and S utmost point magnet on the aluminium foil plate, Surface field is 1200 Gausses, and absorption affinity is 6kg, and two magnet distance is 10cm, apply 20KV voltage and carry out the electrospinning silk,
Embodiment 2:
Fe 3O 4With the mass ratio of polyvinyl alcohol be 1: 100, the amount of all the other experiment conditions and reactive material is with embodiment 1, obtains distribution of fiber diameters and be 100～600nm and along the nanofiber of magnetic direction oriented alignment.
Embodiment 3:
Fe 3O 4With the mass ratio of polyvinyl alcohol be 50: 100, the amount of all the other experiment conditions and reactive material is with embodiment 1, obtains distribution of fiber diameters and be 100～600nm and along the nanofiber of magnetic direction oriented alignment.
Embodiment 4:
The macromolecule that participates in the electrospinning silk is a polyoxyethylene, and the amount of all the other experiment conditions and reactive material is with embodiment 1, obtains distribution of fiber diameters and be 100～600nm and along the nanofiber of magnetic direction oriented alignment.
Embodiment 5:
The macromolecule that participates in the electrospinning silk is a Merlon, adopts chloroform as solvent, and solution concentration still is 10%, and the amount of all the other experiment conditions and reactive material is with embodiment 1, obtains distribution of fiber diameters and be 100～600nm and along the nanofiber of magnetic direction oriented alignment.
Embodiment 6:
The N utmost point at receiving system place and S utmost point magnet surface magnetic field are 1300 Gausses, and absorption affinity is 0.6kg.The amount of all the other experiment conditions and reactive material is with embodiment 1, obtains distribution of fiber diameters and be 100～600nm and along the nanofiber of magnetic direction oriented alignment.
Embodiment 7:
Employed surfactant is an ammonium oleate in the experiment, and the amount of all the other experiment conditions and reactive material is with embodiment 1, obtains distribution of fiber diameters and be 100～600nm and along the nanofiber of magnetic direction oriented alignment.
Embodiment 8:
Employed surfactant is a Tween 80 in the experiment, and the amount of all the other experiment conditions and reactive material is with embodiment 1, obtains distribution of fiber diameters and be 100～600nm and along the nanofiber of magnetic direction oriented alignment.
Embodiment 9:
Employed surfactant is an alkyl quaternary ammonium salts in the experiment, and the amount of all the other experiment conditions and reactive material is with embodiment 1, obtains distribution of fiber diameters and be 100～600nm and along the nanofiber of magnetic direction oriented alignment.
Embodiment 10:
The macromolecule that participates in the electrospinning silk is a gelatin, and the amount of all the other experiment conditions and reactive material is with embodiment 1, obtains distribution of fiber diameters and be 100～600nm and along the nanofiber of magnetic direction oriented alignment.
Embodiment 11:
In the 100mL volumetric flask, with distilled water respectively compound concentration be the FeCl of 2molL 2With FeCl 3Solution; In being added with churned mechanically round-bottomed flask, with 35mL 2molL FeCl 3Solution and 20mL 2molL FeCl 2Solution mixes, and liquid level feeds nitrogen down, to remove the oxygen in anhydrating.Reaction unit is warmed up to 80 ℃, begins slow dropping ammonia in solution, is 6.5 until the pH of solution value, behind the reaction 15min, continues slow dropping ammonia in solution, is 9.5 until the pH value, and continuation stops reaction after reacting 30min; Hold drag with strong magnet, the supernatant liquid that inclines with distilled water cyclic washing product, is neutral until washing lotion; With product Fe 3O 4Freeze drying; Fe with drying 3O 4Nanoparticulate dispersed adds 0.1% surfactant dodecyl sodium sulfate in the solution in the aqueous solution, adopt ultrasonic dispersing; Get above-mentioned Fe 3O 4Suspension joins (concentration is 10%) in poly butyric ester-chloroformic solution, and Fe 3O 4Addition and poly butyric ester mass ratio be 30%, and carry out the supersonic oscillations of 1h;
Above-mentioned solution is joined in the syringe, and syringe needle is selected the 10# syringe needle, and syringe needle links to each other with the positive level of HV generator, makes the negative electrode dash receiver with the aluminium foil plate, and the aluminium foil plate is 10cm apart from syringe needle; Place two N utmost points that face and S utmost point magnet on the aluminium foil plate, Surface field is 1200 Gausses, and two magnet distance is 10cm.Apply 20KV voltage and carry out the electrospinning silk, can get Fe 3O 4About particle diameter 30nm, distribution of fiber diameters is the nanofiber along the magnetic direction oriented alignment of 100～600nm.

Claims (6)

1. the preparation method of a directional magnetic electro spinning nano fiber, concrete preparation process is as follows:
A. respectively with FeCl 2.4H 2O, FeCl 3.6H 2O is dissolved in the FeCl that the distilled water compound concentration is 0.1～2molL 2Solution and concentration are the FeCl of 0.1～2molL 3Solution; Install additional in the reactor of strong magnet, in band stirring and bottom FeCl 3Solution and FeCl 2Solution is according to mol ratio Fe 3+: Fe 2+=1～2: 1 mixed evenly is mixed with mixed liquor, feeds nitrogen to remove the oxygen in the mixed solution; The control reacting liquid temperature to mixed solution and dripping ammoniacal liquor, is 6.5～7 until the pH of solution value at 50～90 ℃, behind reaction 15～30min, continues slow dropping ammonia in solution, is 9～10 until the pH value, continues to stop reaction behind the reaction 30min; Take out supernatant liquid,, be neutral,, obtain Fe the product freeze drying until washing lotion with distilled water cyclic washing product 3O 4Nano particle;
B. with the Fe of drying 3O 4Nanoparticulate dispersed is prepared mass percent in the aqueous solution be 5～30% Fe 3O 4Suspension adds the quality percentage composition and is 0.1～1% surfactant again in solution, use ultrasonic dispersing; Surfactant is a kind of in dodecyl sodium sulfate, lauryl sodium sulfate, Tween 80, ammonium oleate, the alkyl quaternary ammonium salts;
C. get above-mentioned Fe 3O 4Suspension joins in the electrospinning silk Polymer Solution and disposes spinning solution, Fe 3O 4With high molecular mass ratio be 5～40: 100, and carry out the supersonic oscillations of 1～12h; But electrospinning silk Polymer Solution is a kind of in all spinning macromolecular materials;
D. above-mentioned spinning solution is added storage tank, under pump pressure or gravity effect, spinning solution is sprayed from shower nozzle, because the repulsive interaction of Polymer Solution surface charge, drop stretches and is the taylor cone shape, under effect of electric field, be drawn into fiber, repeatedly splitting took place in fiber before reaching dash receiver, on the dash receiver in band magnetic field, collect diameter at the tunica fibrosa of 100～600nm along the magnetic direction oriented alignment.
2. the preparation method of directional magnetic electro spinning nano fiber according to claim 1 is characterized in that in the described mixed liquor of steps A Fe 3+With Fe 2+Mol ratio be 1.5～1.75: 1; The described electrospinning silk of step B Polymer Solution is a kind of in polyvinyl alcohol, Merlon, poly butyric ester, shitosan, gelatin, the polyoxyethylene.
3. a directional magnetic electro spinning nano fiber that adopts the described method preparation of claim 1 is characterized in that containing nanometer Fe in fiber 3O 4Magnetic-particle, distribution of fiber diameters are 100～600nm, and fiber is along the magnetic direction oriented alignment.
4. one kind prepares the used electrospinning silk equipment of the described directional magnetic electro spinning nano fiber of claim 3, comprising a high direct voltage electrostatic generator, a storage tank, connect a syringe pump on the storage tank, the storage tank bottom connects one group of metal shower nozzle, shower nozzle links to each other with HV generator is anodal, and a metal dash receiver that links to each other with negative pole or ground connection is provided with a magnetic field on the metal dash receiver.
5. electrospinning silk equipment according to claim 4 is characterized in that being provided with two N utmost points that face and S utmost point magnet on the metal dash receiver, two magnet distance is 10～30cm, and the magnet surface magnetic intensity is 200～2000 Gausses.
6. electrospinning silk equipment according to claim 4 is characterized in that placing conductive coil on the metal dash receiver, and distance is 5～10cm between conductive coil, and the magnetic field intensity that conductive coil produces is 200～2000 Gausses.
CNB2006100895144A 2006-06-30 2006-06-30 Directional magnetic electrical spinning Nano fibers, preparation method and equipment needed Expired - Fee Related CN100432307C (en)

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