CN100577897C - Multi-fluid composite electrostatic spinning device - Google Patents
Multi-fluid composite electrostatic spinning device Download PDFInfo
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- CN100577897C CN100577897C CN200710062722A CN200710062722A CN100577897C CN 100577897 C CN100577897 C CN 100577897C CN 200710062722 A CN200710062722 A CN 200710062722A CN 200710062722 A CN200710062722 A CN 200710062722A CN 100577897 C CN100577897 C CN 100577897C
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Abstract
The invention relates to a multi-fluid composite electrostatic spinning plant belonging to the electrostatic spinning plant field. A multi-fluid composite electric spinning nozzle is arranged on a base and comprises an outer nozzle and a plurality of inner nozzles embedded in the outer nozzle; wherein the inner nozzles and the outer nozzle are respectively connected with the positive high voltage or negative high voltage from one output end of the a high voltage supply through independent wires connecting with the nozzles; a fiber collector is arranged in front of the multi-fluid composite electric spinning nozzle and is connected the ground wire of the other end of the high voltage supply; the inner nozzles embedded in the outer nozzles are radically and evenly distributed; the inner nozzles and the outer nozzles are non-contact and the inner nozzles are non-contact neither. Spinning solution is injected from the inner nozzles and the outer nozzle respectively through a liquid pump at a continuous and controllable speed forming a composite fluid. Under the influence of the electric field produced by the high voltage supply, porous micro/ nanometer tubes or multiple components composite fiber with a plurality of inner channels after pulling and solidification are formed finally from the composite fluid.
Description
Technical field
The invention belongs to the electrostatic spinning apparatus field, particularly make little, nanotube or have that the compound nucleocapsid structure of multicomponent is little, the multi-fluid composite electrostatic spinning device of nano-fiber material with a plurality of inner passages,
Background technology
Since the discovery of the CNT nineties in 20th century, little, the nanometer composite fiber material that has little, the nano material of tubular structure and have a nucleocapsid structure is at efficient catalytic, adsorbing separation, high sensor, little, receive fluid device, various fields such as medicament slow release all have wide application prospect.Electrostatic spinning is a kind of simple effective method (Reneker, D.H. that is used to prepare the one-dimensional material of little, nanoscale; Chun, I.Nanotechnology 1996,7,216～223), it is that polymer solution or melt are placed the high-voltage electrostatic field, and charged polymer liquid drops under the effect of electric field Coulomb force and is stretched.When electric field force was enough big, the polymer drop overcame surface tension and forms the injection thread.Thread is solvent evaporation or curing in course of injection, finally drops on the receiving system, forms little, the nano fibrous membrane of nonwoven fabric shape.Compare traditional spinning process, electrostatic spinning has the advantage of a lot of uniquenesses, and is minimum as fibre diameter, and products therefrom is a nonwoven fabric construct, have very big specific area etc., but this traditional single fluid electrospinning only is applicable to the nano-fiber material of making one-component.In recent years, a kind of new coaxial electric spinning equipment is developed.This technology is based on two the capillary composition with different-diameter, and the capillary that thickness is different injects different polymer solutions respectively, obtains having complex fiber material (Loscertales, the I.G. of nucleocapsid structure through electrospinning; Barrero, A.; Guerrero, I.; Cortijo, R.; Marquez, M.;
-Calvo, A.M.Science 2002,295, and 1695～1698),, just can obtain little, the nanotube that constitute by cladding material if optionally remove the material of internal layer.But this coaxial electrospinning has in preparation that more complicated inside is little, the one dimension of nanostructured and function is little, be subjected to certain limitation aspect the nano-fiber material.
Summary of the invention
The object of the present invention is to provide a kind of preparation of simple and effective to have little, the nanotube of ultra-fine multi-channel structure or multicomponent is little, the multi-fluid composite electrostatic spinning device of nanometer composite fiber material.
The present invention is by a kind of spinning head that can produce the single composite fluid of particular design, produces under high voltage electrostatic field that continuous multichannel is little, nanotube or little, the nanofiber of the compound nucleocapsid structure of multicomponent.
Multi-fluid composite electrostatic spinning device of the present invention comprises multithread bluk recombination electrospinning spinning head, high voltage source, fiber collecting device, ground wire, Pressure gauge, valve, filter, overflow valve, solution feed pump, fluid reservoir, pedestal etc.;
The one multithread bluk recombination electrospinning spinning head that is installed on the pedestal is formed (the concrete number of inner nozzle is decided on actual needs) by a bigger outer nozzle and an a plurality of less inner nozzle of diameter that is embedded in the outer nozzle of diameter, inside and outside jet pipe respectively by be connected on the jet pipe independently the positive high voltage or the negative high voltage of the output of lead and high voltage source one end are connected separately, or inner nozzle is connected by the positive high voltage or the negative high voltage of lead with the output of high voltage source one end separately, or outer nozzle is connected by the positive high voltage or the negative high voltage of lead with the output of high voltage source one end; The place ahead at multithread body multithread bluk recombination electrospinning spinning head is equipped with a fiber collecting device, and the fiber collecting device is connected with the other end ground wire of high voltage source by lead;
The charging aperture of inside and outside jet pipe is connected with the discharging opening of separately filter by pipeline respectively, the charging aperture of filter separately is connected with separately solution feed flow delivery side of pump by pipeline, and the import of solution solution feed pump separately is equipped with a pipeline that is connected with separately fluid reservoir.
Spacing between described multithread bluk recombination electrospinning spinning head and the fiber collecting device is 5～50cm, and electric-field intensity is at 0.5～3.0kV/cm.
Described fiber collecting device is metal plate, the wire netting flat board of can be parallel mobile conduction, or the metal rotary drum of can be parallel mobile conduction.The fiber collecting device links to each other with ground wire to guarantee fiber collecting device zero potential by lead.
On described inside and outside jet pipe and the pipeline that separately filter is connected Pressure gauge is installed.
On described inside and outside jet pipe and the pipeline that separately filter is connected valve is installed.
On the filter of described inside and outside jet pipe and the pipeline that the solution solution feed pump is connected overflow valve is installed, and an exit of overflow valve is equipped with a pipeline that is connected with fluid reservoir.
Described solution feed pump can accurately be regulated fluid flow, and range of flow is 0.1～1000mL/h, and that the difference by flow can realize is little to multichannel, nanotube or multicomponent is little, the accurate control of the diameter of nanofiber or internal structure.
Do not contact mutually each other between each inner nozzle of described composition multithread bluk recombination electrospinning spinning head and the outer nozzle, guarantee that the ectonexine fluid did not contact mutually before flowing out spinning head; Do not contact mutually each other between described each inner nozzle.
The outer nozzle of described composition multithread bluk recombination electrospinning spinning head is located by the space washer that is installed on the pedestal in the position of nozzle one end with the inner nozzle that is embedded in the outer nozzle, and inner nozzle is radial uniform; There is sealing ring the junction of inner nozzle and outer nozzle.The position of the end that described inner nozzle is connected with the feed flow pipeline is to fix by the set screw on the pedestal, and is fixed on the pedestal by the conduit saddle piece, is connected with the feed flow pipeline by pipe joint.
Described outer nozzle and/or inner nozzle are made by conductive metallic material.
Described high voltage source is 0～100kV.
Multichannel little in preparation, compound little of nanotube or multicomponent, during nanofiber, in, outer liquid flows out from pipeline separately with suitable flow velocity and applies high-tension electricity, outer spinning liquid is coating a plurality of internal layer spinning solution bodies and is forming one superfine liquid stream by the multithread bluk recombination and spray from spinning head, under the electrostatic field that high voltage source produces, this compound fluid is subjected to the effect of statcoulomb power, liquid stream is constantly slenderizing and curing gradually in flying to the process of electrode (fiber collecting device), and last shape has the porous with a plurality of inner passages little, nanotube or multicomponent are compound little, nanofiber.
The present invention can be used for preparing the superfine fibre with multi-channel structure, because prepared fibrous material has superfine diameter and multi-channel internal structure, thereby has a great specific area, and this device is very simple, is applicable to comprise that material system widely such as inorganic, organic, polymer, this multichannel fiber are very suitable for making that ultralight is thin, super warming fabric, ultrafast moisture absorption, fast dried fiber, the high efficiency filter nethike embrane, catalyst, and little, receive fluid line etc.; This technology also can prepare the multinuclear-shell composite structure functional fibre material with many internal compositions, such fibrous material has the not available new function of one-component, thereby can realize that with existing material be raw material, make new material with specific function.As the material with biocompatibility is shell fluid, internal layer can inject multiple medicine, can realize that multicomponent pharmaceutical transports simultaneously or be inside and outside layer raw material that preparation has unique catalysis, sensing, light, electricity, magnetic property so that the functional fibre material of multiple performance multinuclear-shell composite structure with the multicomponent inorganic matter.In addition, because the shell material can well be isolated from the outside inner layer material, thereby carry for the multicomponent pharmaceutical of realizing air or water sensitivity and to have unique effect.Device of the present invention is simple, and suitable material is extensive, and prepared product has very wide application prospect in various fields.
Multi-fluid composite electrostatic spinning device of the present invention can prepare that multichannel is little, nanotube or compound little, the nano-fiber material of multicomponent nucleocapsid structure.This has wide practical value in little, the various fields such as fluid device pipeline, multicomponent pharmaceutical conveying, the super warming fibrous material of bionical ultralight, efficient catalytic or filter membrane of receiving.
Below in conjunction with drawings and Examples in detail the present invention is described in detail.
Description of drawings
Fig. 1. the structural representation of apparatus of the present invention.
Fig. 2. the longitudinal section schematic diagram of multithread bluk recombination electrospinning spinning head of the present invention (this sentences four inner fluid spinning heads is example).
Fig. 3. the spinning head outlet schematic partial cross-sectional view (this sentences four inner fluid spinning heads is example) of multithread bluk recombination electrospinning spinning head of the present invention.
Reference numeral
1. multithread bluk recombination electrospinning spinning head 2. high voltage sourcies 3. fiber collecting devices 4. ground wires
5. Pressure gauge 6. valves 7. filters 8. overflow valves
9. solution feed pump 10. fluid reservoirs 11. pipe joints 12. dog screws
13. inner nozzle 14. conduit saddle pieces 15. pedestals 16. space washers
17. sealing ring 18. outer nozzle feed pipes 19. outer nozzles
The specific embodiment
See also Fig. 1～3.The one multithread bluk recombination electrospinning spinning head 1 that is installed on the pedestal 15 is made up of a large diameter outer nozzle 19 and 4 inner nozzles 13 that are embedded in the minor diameter in the outer nozzle, the inside and outside jet pipe that is prepared into by conducting metal respectively by be connected on the jet pipe independently lead and a power supply are that the positive high voltage or the negative high voltage of the high voltage source 2 one ends output of 0～100kV is connected separately; The metal plate fiber collecting device 3 of one can be parallel mobile conduction is installed at 5～50cm place, the place ahead of multithread bluk recombination electrospinning spinning head 1, and the electric-field intensity between multithread bluk recombination electrospinning spinning head and the fiber collecting device is at 0.5～3.0kV/cm; Fiber collecting device 3 is connected with the other end ground wire of high voltage source 2 by lead, to guarantee fiber collecting device zero potential.
The charging aperture of the inside and outside jet pipe pipeline by having valve 6 respectively is connected with the discharging opening of separately filter 7, and Pressure gauge 5 is installed on pipeline, (range of flow is that 0.1～1000mL/h) outlet is connected to the solution solution feed pump 9 of the pipeline of the charging aperture of filter 7 separately by having overflow valve 8 and separately control fluid flow, in the import of separately solution solution feed pump 9 pipeline that is connected with separately fluid reservoir 10 is installed, an exit of described overflow valve 8 is equipped with a pipeline that is connected with fluid reservoir 10 separately.
The outer nozzle 19 of described composition multithread bluk recombination electrospinning spinning head 1 be embedded in inner nozzle 13 in the outer nozzle 19 in the position of outer nozzle 19 nozzles one end by space washer 16 location that are installed on the pedestal 15, and inner nozzle 13 is embedded in and is radial uniform in the nozzle; Inner nozzle 13 has sealing ring 17 with the junction of outer nozzle 19.
The position of the end that described inner nozzle 13 is connected with the feed flow pipeline is fixing by the set screw on the pedestal 15 12, and is fixed on the pedestal 15 by conduit saddle piece 14, is connected with the feed flow pipeline by pipe joint 11.
Do not contact mutually each other between described each inner nozzle and the outer nozzle, guarantee that the ectonexine fluid did not contact mutually before flowing out spinning head.
Do not contact mutually each other between described each inner nozzle.
When compound little, the nanofiber of multichannel little, the nanotube of preparation or multicomponent, outer solution is by the outer solution solution feed pump 9 of outer solution fluid reservoir 10 processes, be delivered to the outer nozzle feed pipe 18 of multithread bluk recombination electrospinning spinning head 1 again via overflow valve 8 on the outer solution feed flow pipeline and filter 7, solution pressure and flow are by Pressure gauge 5 on the outer solution feed flow pipeline and valve 6 controls.
In like manner, the internal layer fluid through separately internal layer solution fluid reservoir 10 through separately internal layer solution solution feed pump 9, be delivered to the inner nozzle separately 13 of multithread bluk recombination electrospinning spinning head 1 again via overflow valve separately 8 on the internal layer solution feed flow pipeline separately and filter 7, solution pressure and flow are by Pressure gauge separately 5 on the internal layer solution feed flow pipeline separately and valve 6 controls separately (figure slightly).
The preparation of inorganic little, the nanotube of multichannel: the mixed solution for preparing inorganic matter colloidal sol and high polymer with sol-gel process is outer spinning solution, employing is the internal layer fluid with the immiscible oils of outer liquid, through device of the present invention, with the high-temperature calcination of product process, obtain having inorganic little, the nanotube of multi-channel structure then.
Four-way titanium dioxide TiO for example
2The preparation process of micron tube is: 2.0g polyvinylpyrrolidone (PVP) is dissolved in 10.0g absolute ethyl alcohol and the 2.0g glacial acetic acid, be stirred to dissolving fully, then this solution is placed ice-water bath to continue to stir and add 6.0g butyl titanate (or metatitanic acid isopropyl alcohol ester), continue to stir the titanium sol solution that formed stable uniform in 1 hour.This solution is delivered to outer nozzle by solution feed pump and conduit; With atoleine (or vegetable oil, machine oil etc.) is the internal layer fluid, is delivered to four inner nozzles by solution feed pump and conduit.Compound spinning head connects the high pressure positive electric field, metallic plate ground connection, and the distance of spinning head and metallic plate about voltage 20kV, about outer rate of flow of fluid 10mL/h, about inner laminar flow rate of flow of fluid 1mL/h, is carried out electrospinning about 20cm.Obtain one deck tunica fibrosa on metallic plate, this tunica fibrosa places Muffle furnace to be heated to 500 ℃, and 1 ℃/min of programming rate in 500 ℃ of insulations 1 hour, is chilled to room temperature then naturally.Obtain four-way titanium dioxide TiO
2Micron tube.
In like manner, if be outer spinning solution with the mixed solution of inorganic matter colloidal sol and high polymer, oils is internal layer liquid, through 2,3, and 4,5 ... the inner fluid device for spinning just can obtain 2,3,4,5 accordingly ... passage inorganic matter micro-nano mitron.
Multichannel is organic, the preparation of micro polymer, nanotube: with high polymeric solution is outer spinning solution, employing is the internal layer fluid with the immiscible oils of outer liquid, through as embodiment 1 device of the present invention, then product is deoiled through washing, obtain having little, the nanotube of multi-channel structure.
For example the hollow preparation process little, nanofiber of two passage acrylic fibers is: (PAN) is dissolved in 8.0g N with the 2.0g polyacrylonitrile, in the dinethylformamide (DMF), be stirred to the solution that dissolving fully forms stable uniform, this solution is delivered to outer nozzle by solution feed pump and conduit; With atoleine (or vegetable oil, machine oil etc.) is the internal layer fluid, is delivered to two inner nozzles by solution feed pump and conduit.Compound spinning head connects the high pressure positive electric field, metallic plate ground connection, and the distance of spinning head and metallic plate about voltage 30kV, about outer rate of flow of fluid 10mL/h, about inner laminar flow rate of flow of fluid 1mL/h, is carried out composite electrospun about 20cm.Obtain one deck tunica fibrosa on metallic plate, this tunica fibrosa is dried through petroleum ether, obtains hollow little, the nanofiber of two passage acrylic fibers.
In like manner, if be outer spinning solution with required macromolecule such as polyolefin, polyamide, nylon, polyester etc., oils is internal layer liquid, through 2,3,4,5 ... inner fluid spinning system just can obtain 2 accordingly, 3,4,5 ... hollow little, the nanofiber of passage.
The preparation of inorganic little, the nanofiber of multicomponent nucleocapsid structure: with inorganic sol and macromolecule mixed solution is outer spinning solution, is the internal layer fluid according to actual conditions with required multicomponent functional material, through device of the present invention, obtain having the inorganic functional fibrous material of multinuclear-shell structure as embodiment 1.
Tin ash SnO for example
2, indium oxide In
2O
3, zinc oxide ZnO three kernels, titanium dioxide TiO
2The preparation process of shell composite structure nanofiber is: 2.0g polyvinylpyrrolidone (PVP) is dissolved in 10.0g absolute ethyl alcohol and the 1.0g glacial acetic acid, be stirred to dissolving fully, continue then to stir and add 6.0g butyl titanate (or metatitanic acid isopropyl alcohol ester), continue to stir the titanium sol solution that formed stable uniform in 1 hour.This solution is delivered to outer nozzle by solution feed pump and conduit; Similarly, with indium alkoxide In (OR)
3, tin alkoxide Sn (OR)
4, zinc acetate Zn (Ac)
2Polymer solution be the internal layer fluid, be delivered to three inner nozzles by solution feed pump and conduit.Compound spinning head connects the high pressure positive electric field, metallic plate ground connection, and the distance of spinning head and metallic plate about voltage 20kV, about outer rate of flow of fluid 10mL/h, about inner laminar flow rate of flow of fluid 1mL/h, is carried out composite electrospun about 20cm.Obtain one deck tunica fibrosa on metallic plate, this tunica fibrosa places Muffle furnace to be heated to 500 ℃, and 1 ℃/min of programming rate in 500 ℃ of insulations 1 hour, is chilled to room temperature then naturally.Obtain tin ash SnO
2, indium oxide In
2O
3, zinc oxide ZnO three kernels, titanium dioxide TiO
2The shell composite structure nanofiber.
In like manner, if be inside and outside layer spinning solution with required corresponding inorganic sol and mixed with polymers solution, through 2,3,4,5 ... inner fluid spinning system just can obtain 2,3,4,5 accordingly ... little, the nano-fiber material of nuclear-shell composite structure.
The multicomponent nuclear-structure polymer shell is little, the preparation of nanofiber: with high polymeric solution is outer spinning solution, is the internal layer fluid according to actual conditions with required multicomponent functional material, through device of the present invention, obtain having the functional fibre material of multinuclear-shell structure as embodiment 1.
For example, the preparation process of polyoxyethylene (the PEO)-bright B of Luo Dan, polyacrylic acid (PAA)-fluorescein isothiocynate two nuclear/shell composite fibres is, 1g polyvinylpyrrolidone (PVP) is dissolved in stirs 1h in the 9g absolute ethyl alcohol to form a homogeneous solution standby as outer spinning solution; The 4g polyoxyethylene is dissolved in the 6g water, adds the bright B of 0.01g Luo Dan then, stir, as an internal layer backed up for flow; The 4g polyacrylic acid is dissolved in the 6g water, adds the 0.01g fluorescein isothiocynate then, stir, as another internal layer backed up for flow.Above-mentioned PVP solution is delivered to outer nozzle by solution feed pump and conduit; With PEO, PAA is the internal layer fluid, and solution feed pump and conduit by separately are delivered to two inner nozzles respectively.Multithread body multithread bluk recombination electrospinning spinning head connects the high pressure positive electric field, metallic plate ground connection, and the distance of spinning head and metallic plate about voltage 15kV, about outer rate of flow of fluid 10mL/h, about inner laminar flow rate of flow of fluid 1mL/h, is carried out composite electrospun about 20cm.On metallic plate, obtain the micro nanometer fiber film that one deck has dual core-shell structure.
In like manner, if with solution such as required macromolecule such as polyolefin, polyamide, nylon, polyester is outer spinning solution, adopting different polymer solutions as the case may be is internal layer liquid, through 2,3,4,5 ... inner fluid spinning system just can obtain 2,3 accordingly, 4,5 ... compound little, the nano functional fibrous material of kernel-shell multicomponent.
Claims (8)
1. multi-fluid composite electrostatic spinning device, this device comprises multithread bluk recombination electrospinning spinning head, high voltage source, fiber collecting device, ground wire, Pressure gauge, valve, filter, overflow valve, solution feed pump, fluid reservoir, pedestal;
The one multithread bluk recombination electrospinning spinning head that is installed on the pedestal is made up of an outer nozzle and a plurality of inner nozzle that is embedded in the outer nozzle, inside and outside jet pipe respectively by be connected on the jet pipe independently the positive high voltage or the negative high voltage of the output of lead and high voltage source one end are connected separately, or inner nozzle is connected by the positive high voltage or the negative high voltage of lead with the output of high voltage source one end separately, or outer nozzle is connected by the positive high voltage or the negative high voltage of lead with the output of high voltage source one end; The place ahead at multithread bluk recombination electrospinning spinning head is equipped with a fiber collecting device, and the fiber collecting device is connected with the other end ground wire of high voltage source by lead;
The charging aperture of inside and outside jet pipe is connected with the discharging opening of separately filter by pipeline respectively, the charging aperture of filter separately is connected with separately solution feed flow delivery side of pump by pipeline, and the import of solution solution feed pump separately is equipped with a pipeline that is connected with separately fluid reservoir;
On the filter of described inside and outside jet pipe and the pipeline that the solution solution feed pump is connected overflow valve is installed, and an exit of overflow valve is equipped with a pipeline that is connected with fluid reservoir;
On described inside and outside jet pipe and the pipeline that separately filter is connected Pressure gauge is installed.
2. device according to claim 1 is characterized in that: the spacing between described multithread bluk recombination electrospinning spinning head and the fiber collecting device is 5～50cm, and electric-field intensity is at 0.5～3.0kV/cm.
3. device according to claim 1 and 2 is characterized in that: described fiber collecting device is the metal plate of can be parallel mobile conduction, or the metal rotary drum of can be parallel mobile conduction.
4. device according to claim 3 is characterized in that: described metal plate is the wire netting flat board.
5. device according to claim 1 is characterized in that: the scope that described solution feed pump is regulated fluid flow is 0.1～1000mL/h.
6. device according to claim 1 and 2 is characterized in that: do not contact mutually each other between each inner nozzle of described composition multithread bluk recombination electrospinning spinning head and the outer nozzle, guarantee that the ectonexine fluid did not contact mutually before flowing out spinning head; Do not contact mutually each other between described each inner nozzle.
7. device according to claim 1 and 2, it is characterized in that: the outer nozzle of described composition multithread bluk recombination electrospinning spinning head is located by the space washer that is installed on the pedestal in the position of nozzle one end with the inner nozzle that is embedded in the outer nozzle, and inner nozzle is radial uniform; The position of the end that described inner nozzle is connected with the feed flow pipeline is to fix by the set screw on the pedestal, and is fixed on the pedestal by the conduit saddle piece, is connected with the feed flow pipeline of solution by pipe joint.
8. device according to claim 6, it is characterized in that: the outer nozzle of described composition multithread bluk recombination electrospinning spinning head is located by the space washer that is installed on the pedestal in the position of nozzle one end with the inner nozzle that is embedded in the outer nozzle, and inner nozzle is radial uniform; The position of the end that described inner nozzle is connected with the feed flow pipeline is to fix by the set screw on the pedestal, and is fixed on the pedestal by the conduit saddle piece, is connected with the feed flow pipeline of solution by pipe joint.
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Cited By (1)
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|---|---|---|---|---|
| CN102051693A (en) * | 2011-01-20 | 2011-05-11 | 东华大学 | Split type composite electrostatic spinning device |
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