CN106012053A - Electro-spinning micro-nanofiber device and method for preparing micro-nanofiber - Google Patents
Electro-spinning micro-nanofiber device and method for preparing micro-nanofiber Download PDFInfo
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- CN106012053A CN106012053A CN201610646216.4A CN201610646216A CN106012053A CN 106012053 A CN106012053 A CN 106012053A CN 201610646216 A CN201610646216 A CN 201610646216A CN 106012053 A CN106012053 A CN 106012053A
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- nanometer fiber
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- stock solution
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
Abstract
The invention provides an electro-spinning micro-nanofiber device and a method for preparing a micro-nanofiber and belongs to the field of biological materials and tissue engineering. The electro-spinning micro-nanofiber device comprises a high-voltage power supply, receiving devices, a porous spinning jet and a rotary motor, wherein the porous spinning jet is of a hollow cylindrical structure, and the hollow part is an electro-spinning stock solution storage groove capable of accommodating an electro-spinning stock solution; a plurality of spray orifices are formed in the surface of the porous spinning jet; one pole of the high-voltage power supply is connected with the receiving devices, and the other pole of the high-voltage power supply is connected with the porous spinning jet; the rotary motor drives the porous spinning jet to rotate. By virtue of the porous device, the yield can be improved, and micro-nanofibers with uniform directivity are obtained. Meanwhile, the required application voltage can be greatly reduced, and the method for adjustment and control of the more uniform spinning directivity through a single step is also provided.
Description
Technical field
The invention belongs to the preparation field of micro/nano material, be related specifically to a kind of electrostatic spinning micro nanometer fiber device
And the method preparing micro nanometer fiber.
Background technology
Fiber membrane that micro/nano-fibre has been prepared to owing to having high-specific surface area and be widely used in medicine and carry
Body, biological support, organizational project and Application in Chemical Engineering.In tissue repair is applied, the fiber prepared by micro/nano-fibre heap props up
Frame, may be used for simulating human body cell epimatrix structure, it is provided that the attached work of cell, the micro-growing environment bred, break up, to impaired group
Knit or the reparation of organ, regeneration play an important role.
Electrostatic spinning technique is a kind of can effectively production and one of mode preparing micro nanometer fiber, its Main Function machine
Reason is through flowing through an electrospinning stock solution at needle tubing tip, by applying a high electric field, utilizes the electrostatic of charged particle to arrange
Scold effect, when the effect of electric field force is more than the surface tension of solution, the unordered of spurting can be formed on the cone that needle tubing is most advanced and sophisticated
Micro nanometer fiber, these fibers can be collected at fiber owing to the draw of electric field force is directed and is deposited on collection device
Flight course in, high volatile solvent can volatilize, and can collect the micro nanometer fiber of solidification on collection device.Due to former
Liquid is pulled by electric field and extends, and last finished diameter is typically at micro/nano level.Micro nanometer fiber can shape during collecting
Becoming the fenestral fabric that is stacked with, the biological structure such as this structure and natural extracellular matrix is closely similar, so nanometer
The research of fiber is widely used in biological support.
Traditional electrostatic spinning preparation facilities, is limited to the characteristics such as single needle, and fiber preparation efficiency is relatively low, and at electrostatic spinning
During industrialization, the low-yield of electrospinning fibre and randomness have had influence on the feasible of electrospinning large-scale production and manufacture
Property.Therefore, in electrostatic spinning prepares micro nanometer fiber field, there have been many scientific research personnel that electrostatic spinning apparatus is carried out
Many optimizations and improvement, to improving the productivity of electrostatic spinning.(Theron, S.A., et al., the Multiple such as Theron
jets in electrospinning: experiment and modeling. Polymer, 2005. 46(9): p.
2889-2899) utilize 9 syringe needles to be arranged in 3 × 3 and 9 × 1 arrays and carry out electrospinning experiment, find that this kind of Multi needle device can
Significantly improve electrostatic spinning yield.(Zhou, F.L., R.H. Gong, and P. Isaac, the Polymeric such as Zhou
nanofibers via flat spinneret electrospinning. Polymer Engineering & Science,
2009. 49 (12): p. 2475-2481.) utilize oval and circular distribution Multi needle planar arrangement to carry out electrospinning experiment,
Discovery which improves technology stability, and improves electrospinning yield to a certain extent.For electrostatic spinning basic research with
And device improves and all electrostatic spinning yield increase is had certain effect.But the yield for fear of single needle electrospinning is too low, most electrostatic
Device for spinning is required for promoting to realize yield by multiple injecting systems and EFI mouth, the complexity of device and each portion
Coordination between part all industrialization to electrostatic spinning define certain obstruction.
In existing electrostatic spinning batch preparation facilities, upwards (model builds pretty young woman etc., laboratory Nanowire to electric spinning equipment
The electrospinning device of dimension, 2013.) exposed area of solution is added by special pivoted member, it is possible to concurrently form many
Individual spinning electrode, is obviously improved for electrostatic spinning yield.But it is limited to the restriction without homogeneous bore, electrospinning fibre diameter
It is distributed relatively broad, a large amount of preparation methods of narrow diameter distribution electrospinning fibre is limited to the stock solution selected, must execute simultaneously
Add great electric field and overcome the gravity of upwards electrospinning., in electrostatic spinning application, spinning parameter is regulated and controled meanwhile, special
It not to spinning diameter, the regulation and control of directivity, be a key technology yet.At present spinning diameter, directivity control methods can
To realize by change voltage, spinning distance, solution concentration, injection flow and operating distance.But in industrialized production,
It is generally required to after fixing other parameters all, more a certain parameter is adjusted, in actual production, it is difficult to realize all ginsengs
The stable regulation and control of number, it is difficult to prepare the electrospinning fibre that diameter, directivity are unified in a large number, more limit the expansion of many application.
Summary of the invention
In order to solve problems of the prior art, it is an object of the invention to provide a kind of micro-nano fibre of electrostatic spinning
Dimension device and the method preparing micro nanometer fiber.The present invention provides a kind of and new prepares micro nanometer fiber scheme in a large number, and provides
Spinning directivity in situ regulates and controls immediately, it is achieved effectively control generate the morphosis of fiber and improve existing problem.In order to carry
High yield and obtain the micro nanometer fiber of uniform directivity, the application devises one group and is fixed on turning motor and can at the uniform velocity turn
Dynamic multi-holed jet electrode；And electrospinning stock solution is inserted in the accumulator tank of multi-holed jet, then by applying electric field in many
Between hole spinning head and collection device, and by the uniform rotating speed of applying in multi-holed jet electrode, electrospinning stock solution can be via centrifugal
Power and electric field force move towards collection device and produce nanofiber, can obtain high yield and directivity at collection device afterwards
Fiber.The program can obtain simultaneously electrospinning via Multiple-Aperture Device and improve productivity, simultaneously required for applying voltage can be big
Width is by low, and provides a kind of one step to obtain more uniformly spinning directivity regulation and control.
To achieve these goals, the technical solution used in the present invention is as follows:
Plant electrostatic spinning micro nanometer fiber device, including high voltage power supply, receive device, multi-holed jet, turning motor；Described
The cylindrical structure that multi-holed jet is hollow, hollow space is electrospinning stock solution accumulator tank, can accommodate electricity visit stock solution, porous spray
The surface of silk head is provided with multiple spray orifice, and a pole of high voltage power supply is connected on reception device, and another pole is connected on multi-holed jet, described
Turning motor drives the rotation of multi-holed jet.
The bottom of described multi-holed jet is provided with sheet metal, is connected with high voltage power supply.
It is further provided with syringe pump, provides electricity to visit stock solution to multi-holed jet.
The working speed of described turning motor is 30 RPM-15000 RPM.
Described injection diameter is 5 um-5 mm.
Described reception device 3 selects conductive metallic material, including: Fe, Al, Ni, Au, Ag, Cu, CuO, Al2O3、Zn、
Zn0、Fe3O4、Fe2O3。
The diameter of described spray orifice, distance and height, according to diameter and the choosing of build stack parameter of micro nanometer fiber material
Take and regulate.
The method that electrostatic spinning micro nanometer fiber device described in a kind of basis prepares micro nanometer fiber, including walking as follows
Rapid:
1) by electrospinning stock solution, in syringe pump injects multi-holed jet；
2) by turning motor, multi-holed jet is applied a rotating speed 30 RPM-15000 RPM；
3) between multi-holed jet and reception device, voltage 0.2 kV to 60 kV is applied；
4) electrospinning stock solution is under the electric field action power of operating on centrifugal force and high voltage power supply, forms electrostatic spinning at nozzle fine
Dimension, obtains prepared micro nanometer fiber in outside receiving on device.
Described electrospinning stock solution, uses two or more stock solution to mix, doping functional treatment medicine or nano material.
Described electrospun solution is selected from following material: polyethers, polyphenylene oxide, condensing model, polythiophene, polyaniline, polyamide, poly-
Acid imide, polyester, polyurethane, epoxy resin, polyolefin, polyalkenyl halides, polystyrene, poly-to styrene, polyoxyethylene, poly-
Aziridine, kayexalate, poly(ethylene oxide), poly-ethylene methacrylic acid methyl ester, poly terephthalic acid p-phenylenediamine, poly-vinegar
Acid ethylene, polyacetylene, polyglycolic acid, polyacrylic acid, polylactic acid, Poly(D,L-lactide-co-glycolide, polyvinylpyrrolidine
Ketone, Polyethylene Glycol, polyvinyl alcohol, poly methyl silsesquioxane, poly-epsilon-caprolactone, poly-butyrolactone, poly-valerolactone, polypyrrole, poly-
A-amino acid, methylcellulose, ethyl cellulose, sodium carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl
Ylmethyl cellulose, p-phthalic acid hydroxypropyl methyl cellulose, terephthaldehyde's acid cellulose, starch and derivant, fiber
Albumen, fibroin, chitin, chitosan, chondroitin sulfate；Collagen, gelatin, hydrogel, hyaluronic acid and its copolymer, spread out
Biology or mixture.
Compared with prior art, the method have the advantages that
(1) multi-holed jet has the cylindrical structure of hollow, and electrospinning stock solution accumulator tank micro-opening wide in top is beneficial to immediately provide electricity
Spinning stock solution, has ensured the convenience of operation and the preparation stability guaranteeing spinning；And the device structure of the present invention is reasonable, safety
Property high, easy and simple to handle.
(2) multi-holed jet has plural spinneret orifice, beneficially fiber and produces in a large number；And described revolution porous
Spinning head, can remain a constant speed gyration, not only reduces the high voltage electric field of electrostatic spinning, and overcomes spinning coulomb and repel each other
The impact that power electric discharge is uneven, significantly improves the efficiency of spinning and the quality of fiber；It addition, multi-holed jet have employed revolution from
Mental and physical efforts and high-tension electricity prepare fiber, can carry out mating preparation parameter regulation and control for different electrospinning stock solutions.
(3) present invention is capable of the high directivity fibre structure stacking of micro nanometer fiber；And described injection diameter,
Distance spins the nano-fiber material of different-diameter with being highly available for regulating such that it is able to obtain different silk fiber build stack,
Thus enrich the kind of micro nanometer fiber material greatly.
Accompanying drawing explanation
With embodiment, this practicality invention is further illustrated below in conjunction with the accompanying drawings:
Fig. 1 is the structural representation of electrostatic spinning micro nanometer fiber device, reference: 1. syringe pump, 2. high voltage power supply, 3. connect
Receiving apparatus, 4. multi-holed jet, 5. electricity visit stock solution, 6. turning motor, 7. sheet metal, 8. spray orifice；
Fig. 2 is the polyvinyl pyrrolidone fibers optical fiber picture that the present invention arrives.
Detailed description of the invention
Below in conjunction with being embodied as example, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate this
Bright rather than limit the scope of the present invention.In addition, it is to be understood that after having read the content of instruction of the present invention, this area skill
The present invention can be made various changes or modifications by art personnel, and these equivalent form of values fall within the model of the application claims equally
Enclose.
Electrostatic spinning micro nanometer fiber device of the present invention specifically includes: a kind of swinging electrostatic spinning multi-holed jet, should
Spinning head 4 has four and is spaced 90 °, the spray orifice 8 of vertical height 5mm arrangement, and electrospinning stock solution 5 can flow out via these spouts,
Under electric field and revolution centrifugal action, the liquid flowing out spray orifice 8 can form micro nanometer fiber.Multi-holed jet has four
Individual spray orifice, it is possible to significantly improve the productivity of micro nanometer fiber.Fibrous material is prepared the selection of used liquid and can be arranged in pairs or groups not
The regulation and control of electrospinning fibre diameter, directivity, surface character and form are done with the selection controlling parameter.
The present invention solves its technology and be the technical scheme is that multi-holed jet 4 different electrospinning stock solution 5 of arranging in pairs or groups is entered by topic
Row electrostatic spinning, such as polyvinylpyrrolidone ethanol solution, by stock solution in syringe pump 1 injects spinning head 4, at spinning head and
Apply high voltage between collection device 3, meanwhile, use turning motor 6 that spinning head 4 provides a stable rotating speed so that spray webbing
Four spray orifices 7 can produce micro nanometer fiber, to receive solidification equipment 3 to collect prepared micro nanometer fiber simultaneously.
In said method, in solution, the mass fraction of polyvinylpyrrolidone is 15%-25%, and the feed rate of solution is
10-30ml/h, spinning head and the collection distance received between device are 4-9cm, and the rotating speed of slewing equipment is 40-90RPM.
In said method, multi-holed jet can be made up of with sheet metal 7 hollow metal cylinder；Use the cylinder of different-diameter
Shape wire netting is as receiving device 3.
Electrostatic spinning micro nanometer fiber device shown in Fig. 1 by syringe pump 1, high voltage power supply (HV generator) 2, connect
Receipts (solidification) device 3, multi-holed jet 4, turning motor 6, sheet metal 7 are constituted, and syringe is installed on syringe pump 1.Concrete behaviour
Make as follows: the polyvinylpyrrolidone ethanol solution that concentration is 20% is connected to dropping liquid pin by 5ml syringe cylinder by silica gel tube
Head, syringe cylinder with suitable speed to multi-holed jet 4 feeding polyvinylpyrrolidone ethanol solution, by the four of multi-holed jet
Individual spray orifice (aperture is 0.8mm, differential seat angle 90 °, vertical drop 5mm) sprays, and controls polyvinyl pyrrole by micro-injection pump
The feed liquor speed of alkanone ethanol solution is 20ml/h.Spinning head sheet metal 7 is connected with HV generator, and upper electrode is fixed on
At sheet metal 7, bottom electrode is fixed on reception device 3, when electrostatic force and when making a concerted effort more than solution surface tension of centrifugal force, molten
Liquid is stretched, and forms injection stream at spinning head spray orifice.Solvent volatilization in course of injection, collects solid the most on the reception device
The polyvinyl pyrrolidone fibers (Fig. 2) changed.
The polyvinyl pyrrolidone fibers prepared by said method, its average diameter, can be by regulation in 2～20 μm
The parameters such as spout 8 aperture, solution concentration, electrostatic spinning voltage, solution feed rate, slewing equipment rotating speed and collection distance are adjusted
The size of control fibre diameter.This electrostatic spinning multi-holed jet can obtain higher productivity, and obtained micro nanometer fiber is straight
Footpath uniformity is good, and directivity is good, is suitable for attachment and the production of cell.
Embodiment 1
Weigh 8g poly-epsilon-caprolactone, be dissolved in 20ml dichloromethane as in molten, magnetic agitation 60min at normal temperatures,
To water white electrospinning stock solution.
The electrospinning stock solution prepared is injected in 5ml syringe, by silica gel tube, syringe is connected injection needle, by height
The positive level of pressure electrostatic generator connects holes spinning head sheet metal, and region connects external reception device, and spinning head is fixed on revolution dress
Putting, speed of gyration is regulated to 70RPM, and syringe pump flow velocity is regulated to 20ml/h, receives device radius and selects 9cm, then simultaneously
Start slewing equipment and high voltage power supply, voltage is set to 15kv, many times of productivity can be collected fine with the electrospinning of directivity
Dimension.
Embodiment 2
Weigh the solution that PVP mass fraction is 15%, use water as solvent, be simultaneously introduced 0.1g Fe3O4With 0.5g tetracycline
Medicine, at normal temperatures magnetic agitation 60min, obtain water white electrospinning stock solution.
The electrospinning stock solution prepared is injected in 5ml syringe, by silica gel tube, syringe is connected injection needle, by height
The positive level of pressure electrostatic generator connects four hole spinning head bearings, and region connects external reception device, spinning head is fixed on slewing equipment
On, speed of gyration is regulated to 180RPM, and syringe pump flow velocity is regulated to 15ml/h, receives device radius and selects 5cm, opens the most simultaneously
Dynamic slewing equipment and high voltage power supply, be set to 12kv by voltage, can collect the electrospinning fibre of many times of productivity and directivity.
Embodiment 3
Weigh 5g polyvinylpyrrolidone, be dissolved in 25ml ethanol, be simultaneously introduced 0.1g Fe3O4, under room temperature, magnetic force stirs
Mix 60min, obtain the brown electrospinning stock solution of dispersed-powder distribution.
The electrospinning stock solution prepared is injected in 5ml syringe, by silica gel tube, syringe is connected injection needle, by height
The positive level of pressure electrostatic generator connects four hole spinning head bearings, and region connects external reception device, spinning head is fixed on slewing equipment
On, speed of gyration is regulated to 3000RPM, and syringe pump flow velocity is regulated to 30ml/h, receives device radius and selects 13cm, then simultaneously
Start slewing equipment and high voltage power supply, voltage is set to 18kv, many times of productivity can be collected fine with the electrospinning of directivity
Dimension.
Claims (10)
1. kind of electrostatic spinning micro nanometer fiber device, it is characterised in that include high voltage power supply (2), receive device (3), many
Hole spinning head (4), turning motor (6)；Described multi-holed jet (4) is the cylindrical structure of hollow, and hollow space is electricity
Spinning stock solution accumulator tank, can accommodate electricity and visit stock solution (5), and the surface of multi-holed jet (4) is provided with multiple spray orifice (8), high voltage power supply
(2) a pole is connected on reception device (3), and another pole is connected on multi-holed jet (4), and described turning motor (6) drives many
The rotation of hole spinning head (4).
Electrostatic spinning micro nanometer fiber device the most according to claim 1, it is characterised in that described multi-holed jet
(4) bottom is provided with sheet metal (7), is connected with high voltage power supply (2).
Electrostatic spinning micro nanometer fiber device the most according to claim 1, it is characterised in that be further provided with syringe pump
(1), electricity is provided to visit stock solution (5) to multi-holed jet (4).
Electrostatic spinning micro nanometer fiber device the most according to claim 1, it is characterised in that described turning motor (6)
Working speed be 30 RPM-15000 RPM.
Electrostatic spinning micro nanometer fiber device the most according to claim 1, it is characterised in that described spray orifice (8) diameter
It is 5 um-5 mm.
Electrostatic spinning micro nanometer fiber device the most according to claim 1, it is characterised in that described reception device (3)
Select conductive metallic material, including: Fe, Al, Ni, Au, Ag, Cu, CuO, Al2O3、Zn、Zn0、Fe3O4、Fe2O3。
Electrostatic spinning micro nanometer fiber device the most according to claim 1, it is characterised in that described spray orifice (8) straight
Footpath, distance and height, diameter and build stack parameter according to micro nanometer fiber material are chosen and are regulated.
8. the side preparing micro nanometer fiber according to the electrostatic spinning micro nanometer fiber device described in any one of claim 1-7
Method, it is characterised in that comprise the steps:
1) by electrospinning stock solution, in syringe pump injects multi-holed jet；
2) by turning motor, multi-holed jet is applied a rotating speed 30 RPM-15000 RPM；
3) between multi-holed jet and reception device, voltage 0.2 kV to 60 kV is applied；
4) electrospinning stock solution is under the electric field action power of operating on centrifugal force and high voltage power supply, forms electrostatic spinning at nozzle fine
Dimension, obtains prepared micro nanometer fiber in outside receiving on device.
Method the most according to claim 8, it is characterised in that described electrospinning stock solution, uses two or more stock solution to mix,
Doping functional treatment medicine or nano material.
Method the most according to claim 8, it is characterised in that described electrospun solution is selected from following material: polyethers, poly-
Phenylate, condensing model, polythiophene, polyaniline, polyamide, polyimides, polyester, polyurethane, epoxy resin, polyolefin, poly-halo
Alkene, polystyrene, poly-to styrene, polyoxyethylene, polymine, kayexalate, poly(ethylene oxide), poly-methyl
Hexenoic acid methyl ester, poly terephthalic acid p-phenylenediamine, polyvinyl acetate, polyacetylene, polyglycolic acid, polyacrylic acid, polylactic acid,
Poly(D,L-lactide-co-glycolide, polyvinylpyrrolidone, Polyethylene Glycol, polyvinyl alcohol, poly methyl silsesquioxane, poly-ε-
Caprolactone, poly-butyrolactone, poly-valerolactone, polypyrrole, poly-a-amino acid, methylcellulose, ethyl cellulose, carboxymethyl cellulose
Element sodium, hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, p-phthalic acid hydroxypropyl methyl cellulose, right
Cellulose phthalate element, starch and derivant, fibrin, fibroin, chitin, chitosan, chondroitin sulfate；Collagen,
Gelatin, hydrogel, hyaluronic acid and its copolymer, derivant or mixture.
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| CN201610646216.4A CN106012053A (en) | 2016-08-09 | 2016-08-09 | Electro-spinning micro-nanofiber device and method for preparing micro-nanofiber |
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| CN106591967A (en) * | 2016-12-20 | 2017-04-26 | 广东开放大学（广东理工职业学院） | Electrostatic spinning device with cylindrical surface in form of helical array and electrostatic spinning method |
| CN106782747A (en) * | 2017-01-09 | 2017-05-31 | 清华大学 | Silver nanoparticle fiber membrane and preparation method thereof and equipment and electronic device |
| CN106966047A (en) * | 2017-03-23 | 2017-07-21 | 浙江工业大学 | A kind of preparation method of edible nanofiber preservative film |
| CN107299400A (en) * | 2017-07-17 | 2017-10-27 | 浙江大学 | The preparation method of swinging directionality composite micro-nano rice fiber preparation facilities and composite micro-nano rice fiber |
| CN107456609A (en) * | 2017-07-17 | 2017-12-12 | 浙江大学 | The preparation method of directionality biology micro nanometer fiber support quick preparation device and micro nanometer fiber support |
| CN108085784A (en) * | 2017-12-29 | 2018-05-29 | 济南大学 | A kind of synthetic method and products obtained therefrom of NiO multistages micro nanometer fiber |
| CN110207600A (en) * | 2019-06-21 | 2019-09-06 | 广东工业大学 | A kind of spinning equipment, at silk detection device and at yarn examination method |
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| CN110207600A (en) * | 2019-06-21 | 2019-09-06 | 广东工业大学 | A kind of spinning equipment, at silk detection device and at yarn examination method |
| CN110644063A (en) * | 2019-10-08 | 2020-01-03 | 南通大学 | Electrostatic spinning rotary spinning device and use method thereof |
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